CN111704442A - Preparation method of tooth bracket for orthodontic treatment and tooth bracket prepared by preparation method - Google Patents
Preparation method of tooth bracket for orthodontic treatment and tooth bracket prepared by preparation method Download PDFInfo
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- CN111704442A CN111704442A CN202010575568.1A CN202010575568A CN111704442A CN 111704442 A CN111704442 A CN 111704442A CN 202010575568 A CN202010575568 A CN 202010575568A CN 111704442 A CN111704442 A CN 111704442A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000000843 powder Substances 0.000 claims abstract description 110
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 108
- 239000002131 composite material Substances 0.000 claims abstract description 88
- 238000005245 sintering Methods 0.000 claims abstract description 85
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 58
- 239000002002 slurry Substances 0.000 claims abstract description 53
- 239000011159 matrix material Substances 0.000 claims abstract description 46
- 238000002834 transmittance Methods 0.000 claims abstract description 38
- 239000011230 binding agent Substances 0.000 claims abstract description 36
- 238000005452 bending Methods 0.000 claims abstract description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000002156 mixing Methods 0.000 claims abstract description 11
- 238000000465 moulding Methods 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 74
- 230000008569 process Effects 0.000 claims description 62
- 238000000498 ball milling Methods 0.000 claims description 34
- 238000010438 heat treatment Methods 0.000 claims description 34
- 238000005238 degreasing Methods 0.000 claims description 33
- 238000001816 cooling Methods 0.000 claims description 30
- 238000002347 injection Methods 0.000 claims description 25
- 239000007924 injection Substances 0.000 claims description 25
- 238000009694 cold isostatic pressing Methods 0.000 claims description 21
- 238000001035 drying Methods 0.000 claims description 21
- 229910052681 coesite Inorganic materials 0.000 claims description 19
- 229910052906 cristobalite Inorganic materials 0.000 claims description 19
- 239000000377 silicon dioxide Substances 0.000 claims description 19
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 19
- 229910052682 stishovite Inorganic materials 0.000 claims description 19
- 229910052905 tridymite Inorganic materials 0.000 claims description 19
- 238000004321 preservation Methods 0.000 claims description 18
- 238000009766 low-temperature sintering Methods 0.000 claims description 16
- 238000004537 pulping Methods 0.000 claims description 14
- 239000000203 mixture Substances 0.000 claims description 12
- 239000002202 Polyethylene glycol Substances 0.000 claims description 7
- 229920002125 Sokalan® Polymers 0.000 claims description 7
- 235000021355 Stearic acid Nutrition 0.000 claims description 7
- 229910052593 corundum Inorganic materials 0.000 claims description 7
- 238000000227 grinding Methods 0.000 claims description 7
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 7
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 7
- 239000004584 polyacrylic acid Substances 0.000 claims description 7
- 229920001223 polyethylene glycol Polymers 0.000 claims description 7
- 230000001681 protective effect Effects 0.000 claims description 7
- 239000008117 stearic acid Substances 0.000 claims description 7
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 7
- 239000008188 pellet Substances 0.000 claims 1
- 239000000919 ceramic Substances 0.000 description 46
- 238000010998 test method Methods 0.000 description 27
- 239000002245 particle Substances 0.000 description 16
- 239000011148 porous material Substances 0.000 description 9
- 238000011895 specific detection Methods 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 8
- 239000012071 phase Substances 0.000 description 8
- 239000013078 crystal Substances 0.000 description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- 239000000654 additive Substances 0.000 description 4
- 230000000996 additive effect Effects 0.000 description 4
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 4
- 239000007791 liquid phase Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 229910001220 stainless steel Inorganic materials 0.000 description 4
- 239000010935 stainless steel Substances 0.000 description 4
- 239000012752 auxiliary agent Substances 0.000 description 2
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000005324 grain boundary diffusion Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 230000005012 migration Effects 0.000 description 2
- 238000013508 migration Methods 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- 230000009466 transformation Effects 0.000 description 2
- 230000000172 allergic effect Effects 0.000 description 1
- 208000010668 atopic eczema Diseases 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
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- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 210000003128 head Anatomy 0.000 description 1
- 238000001513 hot isostatic pressing Methods 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 238000009740 moulding (composite fabrication) Methods 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61C—DENTISTRY; APPARATUS OR METHODS FOR ORAL OR DENTAL HYGIENE
- A61C7/00—Orthodontics, i.e. obtaining or maintaining the desired position of teeth, e.g. by straightening, evening, regulating, separating, or by correcting malocclusions
- A61C7/12—Brackets; Arch wires; Combinations thereof; Accessories therefor
- A61C7/14—Brackets; Fixing brackets to teeth
- A61C7/16—Brackets; Fixing brackets to teeth specially adapted to be cemented to teeth
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
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- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
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- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
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Abstract
The invention provides a preparation method of a tooth bracket for orthodontic treatment and the prepared tooth bracket, wherein the preparation method comprises the following steps: mixing the composite matrix powder, the composite sintering aid, the binder and water to prepare slurry, and sequentially molding and sintering the slurry to obtain the tooth bracket; the composite matrix powder comprises alumina powder and zirconia powder. The tooth bracket with high bending strength, high hardness and high light transmittance is prepared by adopting the composite matrix powder and the composite sintering aid.
Description
Technical Field
The invention belongs to the technical field of rail transit, and relates to a tooth bracket preparation method for orthodontic and a tooth bracket prepared by the same.
Background
When teeth are fixedly corrected, various types of correcting force are provided by adopting an arch wire, so that the teeth of a patient are arranged orderly, and occlusion is improved. The orthodontic forces applied by the archwire to the teeth are typically transmitted through the brackets. Brackets are components that are cemented to the surface of the crown for receiving and securing an orthodontic archwire. The bracket not only determines the size and direction of the orthodontic force transmitted to the tooth, but also influences the aesthetic degree and comfort in the treatment process, so that the bracket is required to have high strength, hardness and biocompatibility, and is required to have small volume and aesthetic degree. The tooth bracket is one of important components of a fixed orthodontic technology, a plurality of tooth brackets are connected through an arch wire in the orthodontic process, the tooth bracket is pressed on the surface of a tooth in the mounting process, and the tooth bracket is generally adsorbed on the tooth through the lower surface of a base; the volume of tooth support groove itself is less, when it adsorbs when the tooth surface, when dismantling it through instruments such as conventional tweezers, its bottom surface closely adsorbs with the tooth, and the adsorption affinity is big, and general instrument need borrow power to base or support wing in the dismantlement process, and then pulls out, operates like this and causes the damage in tooth support groove very easily, influences its normal use, need spend very big strength moreover and can accomplish the dismantlement work. The bracket in the prior stage mainly comprises a stainless steel bracket and a ceramic bracket, the stainless steel bracket is widely used due to simple preparation process and low cost, but the color difference between stainless steel and teeth is large, the attractiveness is poor, and meanwhile, nickel in the stainless steel bracket can be separated out in the use process and cannot be used by a patient allergic to the nickel. In comparison, the ceramic bracket not only has the advantages of small volume, high strength, low friction coefficient and the like, but also is usually similar to the color and luster of teeth or transparent and has good aesthetic property, so the ceramic bracket is popular with patients. Ceramic brackets are an important direction in the development of current brackets.
Ceramic brackets can be classified into two types, white and transparent, which approximate teeth, according to the color of the bracket. The white ceramic bracket has color similar to that of teeth and good aesthetic degree, thereby being popular with patients. However, due to the large color difference between different patients 'teeth, it is impossible to customize brackets with similar color to the patient's teeth for different patients in consideration of the manufacturing cost. In contrast, transparent ceramic brackets are suitable for patients with different tooth colors, and therefore, the transparent ceramic brackets have a larger suitable group. The preparation of the transparent ceramic bracket usually requires that a ceramic single crystal is prepared first, for example, a transparent aluminum oxide bracket used at present is prepared by a Czochralski method, and then the aluminum oxide single crystal is cut, ground and polished to prepare the bracket.
CN1701764 discloses a method for manufacturing a transparent alumina ceramic bracket, which comprises the following steps: mixing and molding the superfine alumina powder with the purity of more than 99.9 percent; after degreasing, sintering in air at 1200-1500 ℃; and then hot isostatic pressing at 1100 to 1400 ℃.
Zirconia has higher strength, lower friction coefficient and better biocompatibility than alumina, so that the bracket with smaller volume and better performance can be prepared by adopting the zirconia. However, the difficulty of manufacturing single crystal zirconia is much higher than that of single crystal alumina due to the high melting point of zirconia and the phase transition at temperatures near the melting point (2370 ℃), thus limiting the application of transparent zirconia brackets.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a tooth bracket preparation method for orthodontic and the prepared tooth bracket.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the invention provides a method for preparing a tooth bracket for orthodontic treatment, which comprises the following steps:
and mixing the composite matrix powder, the composite sintering aid, the binder and water to prepare slurry, and sequentially molding and sintering the slurry to obtain the tooth bracket.
The composite matrix powder comprises alumina powder and zirconia powder.
According to the invention, alumina particles are filled in gaps of a network structure by utilizing the gelling property of alumina, so that the stacking density is improved, the green strength is increased, meanwhile, zirconia is added, a double electric layer formed by alumina gel is utilized, the zirconia is uniformly mixed in the alumina particles, a network support is filled, the alumina particles are tightly attached after being dried, the toughening mechanism of the zirconia is fully exerted, and the zirconia toughened alumina ceramic material is prepared. Because the thermal expansion coefficient of the zirconia is larger than that of the alumina, in the sintering and temperature rising process, zirconia particles continuously grow up and are connected with alumina particles in a staggered mode, and crystal grains continuously increase and fill gaps, so that the density is increased. In the sintering and cooling process, the alumina matrix can generate enough compressive stress on the zirconia to limit the transformation from tetragonal phase zirconia to monoclinic phase zirconia, and the tetragonal phase zirconia can effectively change the conduction direction of cracks in the fracture process, so that the brittleness of the ceramic is reduced, the bending strength of the ceramic is increased, and the material can be used for preparing the tooth bracket with the bending strength of more than or equal to 500 MPa.
As a preferred technical scheme of the present invention, the preparation method specifically comprises the following steps:
mixing composite matrix powder, a composite sintering aid, a binder and water, and then performing ball milling and pulping to obtain slurry;
(II) injecting the slurry into a bracket grinding tool to form a bracket green body, drying and degreasing the bracket green body in sequence, and placing the bracket green body in a sealed environment for cold isostatic pressing to obtain a formed bracket green body;
and (III) sequentially carrying out high-temperature sintering and low-temperature sintering on the formed bracket green blank in a vacuum environment, and carrying out furnace air cooling to obtain the tooth bracket.
As a preferable technical scheme of the invention, in the step (I), the composite matrix powder comprises alumina powder and zirconia powder.
Preferably, the mass ratio of the alumina powder to the zirconia powder is (4 to 5):1, and may be, for example, 4.0:1, 4.1:1, 4.2:1, 4.3:1, 4.4:1, 4.5:1, 4.6:1, 4.7:1, 4.8:1, 4.9:1 or 5.0:1, but not limited to the values listed, and other values not listed in the range of values are also applicable.
Preferably, the alumina powder has an average particle size of 0.1 to 0.5. mu.m, for example, 0.1. mu.m, 0.2. mu.m, 0.3. mu.m, 0.4. mu.m or 0.5. mu.m, but the average particle size is not limited to the above-mentioned values, and other values not shown in the above-mentioned range are also applicable.
Preferably, the zirconia powder has an average particle size of 0.1 to 0.5. mu.m, for example, 0.1. mu.m, 0.2. mu.m, 0.3. mu.m, 0.4. mu.m or 0.5. mu.m, but the average particle size is not limited to the above-mentioned values, and other values not listed in the above range are also applicable.
Preferably, the mass of the composite sintering aid is 0.1 to 0.5% of the mass of the composite base powder, and may be, for example, 0.1%, 0.2%, 0.3%, 0.4%, or 0.5%, but is not limited to the recited values, and other values not recited in the range of the values are also applicable.
Preferably, the composite sintering aid is MgO and SiO2A mixture of (a).
The invention adds proper amount of MgO and SiO2Composite sintering auxiliary agent makes a small amount of liquid phases appear in the sintering process on the one hand, utilizes it to form the liquid phase and reduce sintering temperature and restrain the grain growth in the sintering, therefore the high transparent ceramic bracket grain size that makes is less, and the crystalline grain is difficult for droing, on the other hand suppresses grain boundary migration and crystalline grain growth, makes the micropore have sufficient time to rely on the grain boundary diffusion and is got rid of, easily realizes densifying.
Preferably, the MgO and SiO2The mass ratio of (a) to (b) is 1 (2) to (5), and may be, for example, 1:2, 1:2.5, 1:3, 1:3.5, 1:4, 1:4.5 or 1:5, but is not limited to the above-mentioned values, and other values not shown in the above-mentioned range are also applicable.
Preferably, the mass of the binder is 1 to 5% of the mass of the composite base powder, and may be, for example, 1%, 2%, 3%, 4% or 5%, but is not limited to the recited values, and other values not recited in the above range are also applicable.
Preferably, the binder comprises one or a combination of at least two of polyethylene glycol, polyacrylic acid or stearic acid.
Preferably, the mass ratio of the total mass of the composite base powder, the composite sintering aid and the binder to the water is 1 (5-10), and may be, for example, 1:5, 1:5.5, 1:6, 1:6.5, 1:7, 1:7.5, 1:8, 1:8.5, 1:9, 1:9.5 or 1:10, but is not limited to the enumerated values, and other unrecited values within the numerical range are also applicable.
As a preferred technical scheme, in the step (I), the ball milling medium adopted in the ball milling pulping process is Al2O3And (4) a small ball.
Preferably, the slurry has a value of 1 (2-4) compared to the value of the milling medium, and may be, for example, 1:2, 1:2.5, 1:3, 1:3.5, 1:4, 1:4.5, or 1:5, but is not limited to the recited values, and other values not recited within the range are also applicable.
Preferably, the ball milling time is 12-24 h, for example, 12h, 13h, 14h, 15h, 16h, 17h, 18h, 19h, 20h, 21h, 22h, 23h or 24h, but not limited to the recited values, and other values not recited in the range of the values are also applicable.
In a preferred embodiment of the present invention, in the step (II), the slurry is injected at a temperature of 120 to 150 ℃ and may be, for example, 120 ℃, 122 ℃, 124 ℃, 126 ℃, 128 ℃, 130 ℃, 132 ℃, 134 ℃, 136 ℃, 138 ℃, 140 ℃, 142 ℃, 144 ℃, 146 ℃, 148 ℃ or 150 ℃, but the slurry is not limited to the above-mentioned values, and other values not shown in the above-mentioned range of values are also applicable.
Preferably, the injection pressure of the slurry is 70 to 130MPa, and may be, for example, 70MPa, 75MPa, 80MPa, 85MPa, 90MPa, 95MPa, 100MPa, 105MPa, 110MPa, 115MPa, 120MPa, 125MPa or 130MPa, but is not limited to the above-mentioned values, and other values not mentioned in the above-mentioned range are also applicable.
Preferably, the slurry is injected at a rate of 30 to 90g/s, for example 30g/s, 35g/s, 40g/s, 45g/s, 50g/s, 55g/s, 60g/s, 65g/s, 70g/s, 75g/s, 80g/s, 95g/s or 90g/s, but not limited to the recited values, and other values not recited in this range are equally applicable.
The injection stage of the slurry is from the time the screw advances the slurry to the time the slurry fills the cavity, where the pressure set on the slurry at the head of the screw (i.e., the injection pressure defined herein) and the rate at which the screw advances the slurry (i.e., the injection rate defined herein) are the key parameters for injection molding. During the injection phase, sufficient velocity and pressure must be established to ensure that the slurry fills the mold cavity. If the injection pressure is adjusted too low, the pressure of the mold cavity is insufficient, and the slurry cannot fill the mold cavity; on the contrary, if the adjustment is too high, the product will have undesirable phenomena such as edge overflow and mold expansion.
Preferably, the temperature of the bracket mold during the injection of the slurry is 40 to 60 ℃, and may be, for example, 40 ℃, 41 ℃, 42 ℃, 43 ℃, 44 ℃, 45 ℃, 46 ℃, 47 ℃, 48 ℃, 49 ℃, 50 ℃, 51 ℃, 52 ℃, 53 ℃, 54 ℃, 55 ℃, 56 ℃, 57 ℃, 58 ℃, 59 ℃ or 60 ℃, but is not limited to the values listed, and other values not listed in the range of the values are also applicable.
In a preferred embodiment of the present invention, in the step (II), the drying temperature is 40 to 60 ℃ and may be, for example, 40 ℃, 41 ℃, 42 ℃, 43 ℃, 44 ℃, 45 ℃, 46 ℃, 47 ℃, 48 ℃, 49 ℃, 50 ℃, 51 ℃, 52 ℃, 53 ℃, 54 ℃, 55 ℃, 56 ℃, 57 ℃, 58 ℃, 59 ℃ or 60 ℃, but is not limited to the recited values, and other values not recited in the numerical range are also applicable.
Preferably, the drying time is 24 to 48 hours, for example, 24 hours, 25 hours, 26 hours, 27 hours, 28 hours, 29 hours, 30 hours, 31 hours, 32 hours, 33 hours, 34 hours, 35 hours, 36 hours, 37 hours, 38 hours, 39 hours, 40 hours, 41 hours, 42 hours, 43 hours, 44 hours, 45 hours, 46 hours, 47 hours or 48 hours, but is not limited to the recited values, and other values not recited in the range of the values are also applicable.
Preferably, the degreasing process is thermal degreasing, and specifically comprises two stages;
preferably, the first stage of the degreasing process comprises: the temperature of the dried green bracket is raised to 400-500 ℃ under a protective atmosphere, and the temperature is maintained for a certain period of time, for example, 400 ℃, 410 ℃, 420 ℃, 430 ℃, 440 ℃, 450 ℃, 460 ℃, 470 ℃, 480 ℃, 490 ℃ or 500 ℃, but the values are not limited to the values listed, and other values not listed in the range of values are also applicable.
Preferably, in the first stage, the temperature rise rate is 1-3 ℃/min, for example, 1.0 ℃/min, 1.1 ℃/min, 1.2 ℃/min, 1.3 ℃/min, 1.4 ℃/min, 1.5 ℃/min, 1.6 ℃/min, 1.7 ℃/min, 1.8 ℃/min, 1.9 ℃/min, 2.0 ℃/min, 2.1 ℃/min, 2.2 ℃/min, 2.3 ℃/min, 2.4 ℃/min, 2.5 ℃/min, 2.6 ℃/min, 2.7 ℃/min, 2.8 ℃/min, 2.9 ℃/min, or 3.0 ℃/min, but not limited to the values listed, and other values not listed within the range of values are also applicable.
Preferably, in the first stage, the holding time is 1 to 4 hours, for example, 1.0 hour, 1.5 hours, 2.0 hours, 2.5 hours, 3.0 hours, 3.5 hours or 4.0 hours, but not limited to the recited values, and other values not recited in the range of the values are also applicable.
Preferably, the second stage of the degreasing process comprises: after the heat preservation in the first stage is finished, the raw bracket blank is further heated to 1100-1200 ℃, then is preserved for a while, and is finally cooled to room temperature along with the furnace, such as 1100 ℃, 1110 ℃, 1120 ℃, 1130 ℃, 1140 ℃, 1150 ℃, 1160 ℃, 1170 ℃, 1180 ℃, 1190 ℃ or 1200 ℃, but the temperature is not limited to the values listed, and other values not listed in the value range are also applicable.
Preferably, in the second stage, the temperature increase rate is 3-8 ℃/min, such as 3 ℃/min, 3.5 ℃/min, 4 ℃/min, 4.5 ℃/min, 5 ℃/min, 5.5 ℃/min, 6 ℃/min, 6.5 ℃/min, 7 ℃/min, 7.5 ℃/min, or 8 ℃/min, but is not limited to the values listed, and other values not listed in the range of values are also applicable.
Preferably, in the second stage, the holding time is 1 to 4 hours, for example, 1.0 hour, 1.5 hours, 2.0 hours, 2.5 hours, 3.0 hours, 3.5 hours or 4.0 hours, but not limited to the recited values, and other values not recited in the range of the values are also applicable.
Degreasing is a process of removing organic substances (mainly binder discharged in the present invention) in a molded body by heating or other physical methods and generating a small amount of sintering. Degreasing is the most difficult and important factor compared to batching, forming, sintering and post-processing of ceramic parts. Incorrect processing modes and parameters of the degreasing process cause inconsistent product shrinkage, resulting in deformation, cracking, stress and inclusions. Degreasing is also important for the subsequent sintering, and cracks and deformations occurring during degreasing cannot be compensated by sintering. The binder and the degreasing are linked, and the binder determines the degreasing means.
In a preferred embodiment of the present invention, in the step (II), the cold isostatic pressing is performed under a pressure of 30 to 50MPa, for example, 30MPa, 31MPa, 32MPa, 33MPa, 34MPa, 35MPa, 36MPa, 37MPa, 38MPa, 39MPa, 40MPa, 41MPa, 42MPa, 43MPa, 44MPa, 45MPa, 46MPa, 47MPa, 48MPa, 49MPa or 50MPa, but the pressure is not limited to the above-mentioned values, and other values not listed in the above-mentioned range are also applicable.
The dwell time of the cold isostatic pressing is 3-10 min, for example, 3min, 4min, 5min, 6min, 7min, 8min, 9min or 10min, but is not limited to the values listed, and other values not listed in the range of values are also applicable.
As a preferred embodiment of the present invention, in step (iii), the high temperature sintering process includes: the molded bracket green body is heated to 1300 to 1500 ℃ and then kept warm for a certain period of time, for example, 1300 ℃, 1310 ℃, 1320 ℃, 1330 ℃, 1340 ℃, 1350 ℃, 1360 ℃, 1370 ℃, 1380 ℃, 1390 ℃, 1400 ℃, 1410 ℃, 1420 ℃, 1430 ℃, 1440 ℃, 1450 ℃, 1460 ℃, 1470 ℃, 1480 ℃, 1490 ℃ or 1500 ℃, but is not limited to the values listed, and other values not listed in the range of values are also applicable.
Preferably, the temperature rise rate of the molded bracket green blank is 3-8 ℃/min, such as 3.0 ℃/min, 3.5 ℃/min, 4.0 ℃/min, 4.5 ℃/min, 5.0 ℃/min, 5.5 ℃/min, 6.0 ℃/min, 6.5 ℃/min, 7.0 ℃/min, 7.5 ℃/min, or 8.0 ℃/min, but not limited to the values listed, and other values not listed within the range of the values are also applicable, and further preferably, the temperature rise rate is 4-7 ℃/min.
Preferably, the holding time of the high temperature sintering process is 0.5 to 1.5 hours, for example, 0.5 hour, 0.6 hour, 0.7 hour, 0.8 hour, 0.9 hour, 1.0 hour, 1.1 hour, 1.2 hour, 1.3 hour, 1.4 hour or 1.5 hour, but not limited to the listed values, and other values in the range of the values are also applicable.
Preferably, the low-temperature sintering process comprises: after the heat preservation of the high-temperature sintering is finished, the temperature of the bracket green body is reduced to 1200-1300 ℃ and then the temperature is preserved for a period of time, for example, 1200 ℃, 1210 ℃, 1220 ℃, 1230 ℃, 1240 ℃, 1250 ℃, 1260 ℃, 1270 ℃, 1280 ℃, 1290 ℃ or 1300 ℃, but the temperature is not limited to the values listed, and other values not listed in the value range are also applicable.
Preferably, the cooling rate of the green bracket after high-temperature sintering is 3-8 ℃/min, such as 3.0 ℃/min, 3.5 ℃/min, 4.0 ℃/min, 4.5 ℃/min, 5.0 ℃/min, 5.5 ℃/min, 6.0 ℃/min, 6.5 ℃/min, 7.0 ℃/min, 7.5 ℃/min, or 8.0 ℃/min, but not limited to the values listed, and other values not listed within the range of values are also applicable, and further preferably, the cooling rate is 4-7 ℃/min.
Preferably, the holding time of the low-temperature sintering process is 2 to 6 hours, for example, 2.0 hours, 2.5 hours, 3.0 hours, 3.5 hours, 4.0 hours, 4.5 hours, 5.0 hours, 5.5 hours or 6.0 hours, but is not limited to the enumerated values, and other unrecited values in the numerical range are also applicable.
In a second aspect, the invention provides a dental bracket prepared by the preparation method of the first aspect, wherein the dental bracket comprises composite matrix powder, a composite sintering aid, a binder and water.
Wherein the composite matrix powder comprises alumina powder and zirconia powder.
In a preferred embodiment of the present invention, the bending strength of the dental bracket is 500MPa or more, and may be, for example, 500MPa, 510MPa, 520MPa, 530MPa, 540MPa, 550MPa, 560MPa, 570MPa, 580MPa, 590MPa or 600MPa, but the bending strength is not limited to the above-mentioned values, and other values not listed in the above-mentioned range are also applicable.
Preferably, the dental bracket has a hardness of 2000HV or more, for example 2000HV, 2100HV, 2200HV, 2300HV, 2400HV, 2500HV, 2600HV, 2700HV, 2800HV, 2900HV or 3000HV, but is not limited to the values listed, and other values not listed in this range are equally applicable.
Preferably, the total light transmission is > 90%, for example 90%, 91%, 92%, 93%, 94%, 95%, 96%, 97%, 98% or 99%, but is not limited to the recited values, and other values not recited within the range of values are equally applicable.
The system refers to an equipment system, or a production equipment.
Compared with the prior art, the invention has the beneficial effects that:
(1) according to the invention, alumina particles are filled in gaps of a network structure by utilizing the gelling property of alumina, so that the stacking density is improved, the green strength is increased, meanwhile, zirconia is added, a double electric layer formed by alumina gel is utilized, the zirconia is uniformly mixed in the alumina particles, a network support is filled, the alumina particles are tightly attached after being dried, the toughening mechanism of the zirconia is fully exerted, and the zirconia toughened alumina ceramic material is prepared. Because the thermal expansion coefficient of the zirconia is larger than that of the alumina, in the sintering and temperature rising process, zirconia particles continuously grow up and are connected with alumina particles in a staggered mode, and crystal grains continuously increase and fill gaps, so that the density is increased. In the sintering and cooling process, the alumina matrix can generate enough compressive stress on the zirconia to limit the transformation from tetragonal phase zirconia to monoclinic phase zirconia, and the tetragonal phase zirconia can effectively change the conduction direction of cracks in the fracture process, so that the brittleness of the ceramic is reduced, the bending strength of the ceramic is increased, and the material can be used for preparing the tooth bracket with the bending strength of more than or equal to 500 MPa.
(2) The invention adds proper amount of MgO and SiO2Composite sintering auxiliary agent makes a small amount of liquid phases appear in the sintering process on the one hand, utilizes it to form the liquid phase and reduce sintering temperature and restrain the grain growth in the sintering, therefore the high transparent ceramic bracket grain size that makes is less, and the crystalline grain is difficult for droing, on the other hand suppresses grain boundary migration and crystalline grain growth, makes the micropore have sufficient time to rely on the grain boundary diffusion and is got rid of, easily realizes densifying.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments.
Example 1
The embodiment provides a preparation method of a tooth bracket, which comprises the following steps:
(1) mixing the composite matrix powder, the composite sintering aid, the binder and water, and then performing ball milling and pulping to obtain slurry;
the composite matrix powder is a mixture of alumina powder and zirconia powder, wherein the mass ratio of the alumina powder to the zirconia powder is 4:1, the composite matrix powder is 100g in total, the average particle size of the alumina powder is 0.1 mu m, and the average particle size of the zirconia powder is 0.1 mu m;
the composite sintering aid is MgO and SiO2A mixture of (1), wherein MgO and SiO2The mass ratio of the composite sintering aid is 1:2, and the mass of the composite sintering aid is 0.1 percent of the mass of the composite matrix powder;
the binder comprises one or the combination of at least two of polyethylene glycol, polyacrylic acid or stearic acid, and the mass of the binder is 1 percent of that of the composite matrix powder;
the mass ratio of the total mass of the composite matrix powder, the composite sintering aid and the binder to the water is 1: 5;
the ball milling medium adopted in the ball milling pulping process is Al2O3The mass ratio of the slurry to the ball milling medium is 1:2, and the ball milling time is12h；
(2) After being injected into the bracket grinding tool, the slurry forms a bracket green body, wherein the injection temperature of the slurry is 120 ℃, the injection pressure is 70MPa, and the injection speed is 30 g/s; in the process of injecting the slurry, the temperature of the bracket mould is 40 ℃;
sequentially drying and degreasing the bracket green body, wherein the drying temperature is 40 ℃, and the drying time is 48 hours; the degreasing process is thermal degreasing, and specifically comprises two stages, wherein the first stage comprises: under the protective atmosphere, heating the dried bracket green body to 400 ℃ at the heating rate of 1 ℃/min, and then preserving heat for 4 h; the second stage comprises: after the first stage of heat preservation is finished, continuously heating the bracket green blank to 1100 ℃ at the heating rate of 3 ℃/min, preserving heat for 4 hours again, and finally cooling to room temperature along with the furnace;
after demolding, placing the degreased bracket green blank in a sealed environment for cold isostatic pressing to obtain a formed bracket green blank, wherein the pressure of the cold isostatic pressing is 30MPa, and the pressure maintaining time of the cold isostatic pressing is 10 min;
(3) the formed bracket green body is sequentially subjected to high-temperature sintering and low-temperature sintering in a vacuum environment, wherein the high-temperature sintering process comprises the following steps: heating the formed bracket green blank to 1300 ℃ at the heating rate of 3 ℃/min, and then preserving heat for 1.5 h; the low-temperature sintering process comprises the following steps: after the heat preservation of the high-temperature sintering is finished, cooling the bracket green blank to 1200 ℃ at a cooling rate of 3 ℃/min, and preserving heat for 6 h; finally, the tooth bracket finished product is obtained by furnace air cooling.
The prepared finished product of the tooth bracket is flat and compact in surface, free of cracks and free of pores which are obviously visible to naked eyes, the bending strength of the tooth bracket is tested according to a fine ceramic bending strength test method provided by GB/T6569-2006, the hardness of the tooth bracket is tested according to a fine ceramic room temperature hardness test method provided by GB/T16534-2009, the total light transmittance of the tooth bracket is detected according to a light transmittance fine ceramic transmittance test method provided by JC/T2020-2010, and the specific detection result is as follows: the flexural strength was 512MPa, the hardness was 2250HV, and the total light transmittance was 91%.
Example 2
The embodiment provides a preparation method of a tooth bracket, which comprises the following steps:
(1) mixing the composite matrix powder, the composite sintering aid, the binder and water, and then performing ball milling and pulping to obtain slurry;
the composite matrix powder is a mixture of alumina powder and zirconia powder, wherein the mass ratio of the alumina powder to the zirconia powder is 4.2:1, the average grain diameter of the alumina powder is 0.2 mu m, and the average grain diameter of the zirconia powder is 0.2 mu m;
the composite sintering aid is MgO and SiO2A mixture of (1), wherein MgO and SiO2The mass ratio of (1: 3) and the mass of the composite sintering additive is 0.2% of the mass of the composite matrix powder;
the binder comprises one or the combination of at least two of polyethylene glycol, polyacrylic acid or stearic acid, and the mass of the binder is 2% of that of the composite matrix powder;
the mass ratio of the total mass of the composite matrix powder, the composite sintering aid and the binder to the water is 1: 6;
the ball milling medium adopted in the ball milling pulping process is Al2O3The mass ratio of the slurry to the ball milling medium is 1:2.5, and the ball milling time is 15 hours;
(2) after being injected into the bracket grinding tool, the slurry forms a bracket green body, wherein the injection temperature of the slurry is 128 ℃, and the injection pressure is 85 MPa; the injection speed is 45 g/s; in the process of injecting the slurry, the temperature of the bracket mould is 45 ℃;
sequentially drying and degreasing the bracket green body, wherein the drying temperature is 45 ℃, and the drying time is 42 h; the degreasing process is thermal degreasing, and specifically comprises two stages, wherein the first stage comprises: under the protective atmosphere, heating the dried bracket green body to 420 ℃ at the heating rate of 1.5 ℃/min, and then preserving heat for 3 h; the second stage comprises: after the first stage of heat preservation is finished, continuously heating the bracket green blank to 1125 ℃ at the heating rate of 4 ℃/min, preserving heat for 3h again, and finally cooling to room temperature along with the furnace;
after demolding, placing the degreased bracket green blank in a sealed environment for cold isostatic pressing to obtain a molded bracket green blank, wherein the pressure of the cold isostatic pressing is 35MPa, and the pressure maintaining time of the cold isostatic pressing is 9 min;
(3) the formed bracket green body is sequentially subjected to high-temperature sintering and low-temperature sintering in a vacuum environment, wherein the high-temperature sintering process comprises the following steps: heating the formed bracket green blank to 1350 ℃ at the heating rate of 4 ℃/min, and then preserving heat for 1.3 h; the low-temperature sintering process comprises the following steps: after the heat preservation of the high-temperature sintering is finished, cooling the bracket green blank to 1230 ℃ at a cooling rate of 4 ℃/min, and preserving the heat for 5 hours; finally, the tooth bracket finished product is obtained by furnace air cooling.
The prepared finished product of the tooth bracket is flat and compact in surface, free of cracks and free of pores which are obviously visible to naked eyes, the bending strength of the tooth bracket is tested according to a fine ceramic bending strength test method provided by GB/T6569-2006, the hardness of the tooth bracket is tested according to a fine ceramic room temperature hardness test method provided by GB/T16534-2009, the total light transmittance of the tooth bracket is detected according to a light transmittance fine ceramic transmittance test method provided by JC/T2020-2010, and the specific detection result is as follows: the flexural strength was 520MPa, the hardness was 2360HV, and the total light transmittance was 93%.
Example 3
The embodiment provides a preparation method of a tooth bracket, which comprises the following steps:
(1) mixing the composite matrix powder, the composite sintering aid, the binder and water, and then performing ball milling and pulping to obtain slurry;
the composite matrix powder is a mixture of alumina powder and zirconia powder, wherein the mass ratio of the alumina powder to the zirconia powder is 4.5:1, the average grain diameter of the alumina powder is 0.3 mu m, and the average grain diameter of the zirconia powder is 0.3 mu m;
the composite sintering aid is MgO and SiO2A mixture of (1), wherein MgO and SiO2The mass ratio of (1: 3) and the mass of the composite sintering additive is 0.3% of the mass of the composite matrix powder;
the binder comprises one or the combination of at least two of polyethylene glycol, polyacrylic acid or stearic acid, and the mass of the binder is 3% of that of the composite matrix powder;
the mass ratio of the total mass of the composite matrix powder, the composite sintering aid and the binder to the water is 1: 8;
the ball milling medium adopted in the ball milling pulping process is Al2O3The mass ratio of the slurry to the ball milling medium is 1:3, and the ball milling time is 18 h;
(2) after being injected into the bracket grinding tool, the slurry forms a bracket green body, wherein the injection temperature of the slurry is 135 ℃, and the injection pressure is 100 MPa; the injection speed is 60 g/s; in the process of injecting the slurry, the temperature of the bracket mould is 50 ℃;
sequentially drying and degreasing the bracket green body, wherein the drying temperature is 50 ℃, and the drying time is 36 h; the degreasing process is thermal degreasing, and specifically comprises two stages, wherein the first stage comprises: under the protective atmosphere, heating the dried bracket green body to 450 ℃ at the heating rate of 2 ℃/min, and then preserving heat for 3 h; the second stage comprises: after the first stage of heat preservation is finished, continuously heating the bracket green blank to 1150 ℃ at the heating rate of 5 ℃/min, preserving heat for 3h again, and finally cooling to room temperature along with the furnace;
demoulding the degreased bracket green blank, and then placing the degreased bracket green blank in a sealed environment for cold isostatic pressing to obtain a formed bracket green blank, wherein the pressure of the cold isostatic pressing is 40MPa, and the pressure maintaining time of the cold isostatic pressing is 7 min;
(3) the formed bracket green body is sequentially subjected to high-temperature sintering and low-temperature sintering in a vacuum environment, wherein the high-temperature sintering process comprises the following steps: heating the formed bracket green blank to 1400 ℃ at the heating rate of 5 ℃/min, and then preserving heat for 1 h; the low-temperature sintering process comprises the following steps: after the heat preservation of the high-temperature sintering is finished, cooling the bracket green blank to 1250 ℃ at the cooling rate of 5 ℃/min, and preserving the heat for 4 h; finally, the tooth bracket finished product is obtained by furnace air cooling.
The prepared finished product of the tooth bracket is flat and compact in surface, free of cracks and free of pores which are obviously visible to naked eyes, the bending strength of the tooth bracket is tested according to a fine ceramic bending strength test method provided by GB/T6569-2006, the hardness of the tooth bracket is tested according to a fine ceramic room temperature hardness test method provided by GB/T16534-2009, the total light transmittance of the tooth bracket is detected according to a light transmittance fine ceramic transmittance test method provided by JC/T2020-2010, and the specific detection result is as follows: the flexural strength was 540MPa, the hardness was 2400HV, and the total light transmittance was 95%.
Example 4
The embodiment provides a preparation method of a tooth bracket, which comprises the following steps:
(1) mixing the composite matrix powder, the composite sintering aid, the binder and water, and then performing ball milling and pulping to obtain slurry;
the composite matrix powder is a mixture of alumina powder and zirconia powder, wherein the mass ratio of the alumina powder to the zirconia powder is 4.7:1, the average grain diameter of the alumina powder is 0.4 mu m, and the average grain diameter of the zirconia powder is 0.4 mu m;
the composite sintering aid is MgO and SiO2A mixture of (1), wherein MgO and SiO2The mass ratio of (1: 4) and the mass of the composite sintering additive is 0.4% of the mass of the composite matrix powder;
the binder comprises one or the combination of at least two of polyethylene glycol, polyacrylic acid or stearic acid, and the mass of the binder is 4% of that of the composite matrix powder;
the mass ratio of the total mass of the composite matrix powder, the composite sintering aid and the binder to the water is 1: 9;
the ball milling medium adopted in the ball milling pulping process is Al2O3The mass ratio of the slurry to the ball milling medium is 1:3.5, and the ball milling time is 21 h;
(2) after being injected into the bracket grinding tool, the slurry forms a bracket green body, wherein the injection temperature of the slurry is 142 ℃, and the injection pressure is 115 MPa; the injection speed is 75 g/s; in the process of injecting the slurry, the temperature of the bracket mould is 55 ℃;
sequentially drying and degreasing the bracket green body, wherein the drying temperature is 55 ℃, and the drying time is 30 h; the degreasing process is thermal degreasing, and specifically comprises two stages, wherein the first stage comprises: under the protective atmosphere, heating the dried bracket green body to 470 ℃ at the heating rate of 2.5 ℃/min, and then preserving heat for 2 h; the second stage comprises: after the first stage of heat preservation is finished, continuously heating the bracket green blank to 1175 ℃ at the heating rate of 6 ℃/min, preserving heat for 2 hours again, and finally cooling to room temperature along with the furnace;
demoulding the degreased bracket green blank, and then placing the degreased bracket green blank in a sealed environment for cold isostatic pressing to obtain a formed bracket green blank, wherein the pressure of the cold isostatic pressing is 45MPa, and the pressure maintaining time of the cold isostatic pressing is 5 min;
(3) the formed bracket green body is sequentially subjected to high-temperature sintering and low-temperature sintering in a vacuum environment, wherein the high-temperature sintering process comprises the following steps: heating the formed bracket green blank to 1450 ℃ at the heating rate of 6 ℃/min, and then preserving heat for 0.7 h; the low-temperature sintering process comprises the following steps: after the heat preservation of the high-temperature sintering is finished, cooling the bracket green blank to 1270 ℃ at the cooling rate of 6 ℃/min, and preserving the heat for 3 h; finally, the tooth bracket finished product is obtained by furnace air cooling.
The prepared finished product of the tooth bracket is flat and compact in surface, free of cracks and free of pores which are obviously visible to naked eyes, the bending strength of the tooth bracket is tested according to a fine ceramic bending strength test method provided by GB/T6569-2006, the hardness of the tooth bracket is tested according to a fine ceramic room temperature hardness test method provided by GB/T16534-2009, the total light transmittance of the tooth bracket is detected according to a light transmittance fine ceramic transmittance test method provided by JC/T2020-2010, and the specific detection result is as follows: the flexural strength was 530MPa, the hardness was 2280HV, and the total light transmittance was 93%.
Example 5
The embodiment provides a preparation method of a tooth bracket, which comprises the following steps:
(1) mixing the composite matrix powder, the composite sintering aid, the binder and water, and then performing ball milling and pulping to obtain slurry;
the composite matrix powder is a mixture of alumina powder and zirconia powder, wherein the mass ratio of the alumina powder to the zirconia powder is 5:1, the average grain diameter of the alumina powder is 0.5 mu m, and the average grain diameter of the zirconia powder is 0.5 mu m;
the composite sintering aid is MgO and SiO2A mixture of (1), wherein MgO and SiO2The mass ratio of (1: 5) and the mass of the composite sintering additive is 0.5 percent of the mass of the composite matrix powder;
the binder comprises one or the combination of at least two of polyethylene glycol, polyacrylic acid or stearic acid, and the mass of the binder is 5% of that of the composite matrix powder;
the mass ratio of the total mass of the composite matrix powder, the composite sintering aid and the binder to the water is 1: 10;
the ball milling medium adopted in the ball milling pulping process is Al2O3The mass ratio of the slurry to the ball milling medium is 1:4, and the ball milling time is 24 hours;
(2) after being injected into the bracket grinding tool, the slurry forms a bracket green body, wherein the injection temperature of the slurry is 150 ℃, and the injection pressure is 130 MPa; the injection speed is 90 g/s; in the process of injecting the slurry, the temperature of the bracket mould is 60 ℃;
sequentially drying and degreasing the bracket green body, wherein the drying temperature is 60 ℃, and the drying time is 24 hours; the degreasing process is thermal degreasing, and specifically comprises two stages, wherein the first stage comprises: under the protective atmosphere, heating the dried bracket green body to 500 ℃ at the heating rate of 3 ℃/min, and then preserving heat for 1 h; the second stage comprises: after the first stage of heat preservation is finished, continuously heating the bracket green blank to 1200 ℃ at the heating rate of 8 ℃/min, preserving heat for 1h again, and finally cooling to room temperature along with the furnace;
after demolding, placing the degreased bracket green blank in a sealed environment for cold isostatic pressing to obtain a molded bracket green blank, wherein the pressure of the cold isostatic pressing is 50MPa, and the pressure maintaining time of the cold isostatic pressing is 3 min;
(3) the formed bracket green body is sequentially subjected to high-temperature sintering and low-temperature sintering in a vacuum environment, wherein the high-temperature sintering process comprises the following steps: heating the formed bracket green blank to 1500 ℃ at the heating rate of 8 ℃/min, and then preserving heat for 0.5 h; the low-temperature sintering process comprises the following steps: after the heat preservation of the high-temperature sintering is finished, cooling the bracket green blank to 1300 ℃ at a cooling rate of 8 ℃/min, and preserving heat for 2 h; finally, the tooth bracket finished product is obtained by furnace air cooling.
The prepared finished product of the tooth bracket is flat and compact in surface, free of cracks and free of pores which are obviously visible to naked eyes, the bending strength of the tooth bracket is tested according to a fine ceramic bending strength test method provided by GB/T6569-2006, the hardness of the tooth bracket is tested according to a fine ceramic room temperature hardness test method provided by GB/T16534-2009, the total light transmittance of the tooth bracket is detected according to a light transmittance fine ceramic transmittance test method provided by JC/T2020-2010, and the specific detection result is as follows: the flexural strength was 506MPa, the hardness was 2100HV, and the total light transmittance was 90%.
Comparative example 1
This comparative example provides a method of preparing a dental bracket, which differs from example 3 in that:
the ceramic powder used for the tooth bracket is single alumina powder without zirconia powder, the input amount of the alumina powder is the same as that of the composite matrix powder in the embodiment 3, and the other component contents, the process parameters and the like are the same as those in the embodiment 3.
The prepared finished product of the tooth bracket has uneven surface and pores visible to naked eyes, the bending strength of the tooth bracket is tested according to a fine ceramic bending strength test method provided by GB/T6569-2006, the hardness of the tooth bracket is tested according to a fine ceramic room temperature hardness test method provided by GB/T16534-2009, the total light transmittance of the tooth bracket is detected according to a light transmittance fine ceramic transmittance test method provided by JC/T2020-2010, and the specific detection result is as follows: the flexural strength was 385MPa, the hardness was 1820HV, and the total light transmittance was 85%.
Comparative example 2
This comparative example provides a method of preparing a dental bracket, which differs from example 3 in that:
the ceramic powder used for the tooth bracket is single zirconia powder without alumina powder, the input amount of the zirconia powder is the same as that of the composite base powder in the embodiment 3, and the other component contents, the process parameters and the like are the same as those in the embodiment 3.
The prepared finished product of the tooth bracket has uneven surface and pores visible to naked eyes, the bending strength of the tooth bracket is tested according to a fine ceramic bending strength test method provided by GB/T6569-2006, the hardness of the tooth bracket is tested according to a fine ceramic room temperature hardness test method provided by GB/T16534-2009, the total light transmittance of the tooth bracket is detected according to a light transmittance fine ceramic transmittance test method provided by JC/T2020-2010, and the specific detection result is as follows: the flexural strength was 369MPa, the hardness was 1750HV, and the total light transmittance was 84%.
Comparative example 3
This comparative example provides a method of preparing a dental bracket, which differs from example 3 in that:
the sintering aid used for the tooth bracket is only MgO and does not contain SiO2The amount of MgO added was the same as that of the composite sintering aid in example 3, and the other component contents and process parameters were the same as those in example 3.
The prepared finished product of the tooth bracket has uneven surface and pores visible to naked eyes, the bending strength of the tooth bracket is tested according to a fine ceramic bending strength test method provided by GB/T6569-2006, the hardness of the tooth bracket is tested according to a fine ceramic room temperature hardness test method provided by GB/T16534-2009, the total light transmittance of the tooth bracket is detected according to a light transmittance fine ceramic transmittance test method provided by JC/T2020-2010, and the specific detection result is as follows: the bending strength of the finished product of the tooth bracket is 367MPa, the hardness is 1680HV, and the total light transmittance is 83%.
Comparative example 4
This comparative example provides a method of preparing a dental bracket, which differs from example 3 in that:
the sintering aid used for the tooth bracket is only SiO2Does not contain MgO, SiO2The input amount of the sintering aid is the same as that of the composite sintering aid in the embodiment 3, and the contents of other components, process parameters and the like are the same as those of the embodiment 3.
The prepared finished product of the tooth bracket has uneven surface and pores visible to naked eyes, the bending strength of the tooth bracket is tested according to a fine ceramic bending strength test method provided by GB/T6569-2006, the hardness of the tooth bracket is tested according to a fine ceramic room temperature hardness test method provided by GB/T16534-2009, the total light transmittance of the tooth bracket is detected according to a light transmittance fine ceramic transmittance test method provided by JC/T2020-2010, and the specific detection result is as follows: the flexural strength was 363MPa, the hardness was 1720HV, and the total light transmittance was 85%.
The applicant declares that the above description is only a specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and it should be understood by those skilled in the art that any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are within the scope and disclosure of the present invention.
Claims (10)
1. A method for preparing a tooth bracket for orthodontic treatment is characterized by comprising the following steps:
mixing the composite matrix powder, the composite sintering aid, the binder and water to prepare slurry, and sequentially molding and sintering the slurry to obtain the tooth bracket;
the composite matrix powder comprises alumina powder and zirconia powder.
2. The preparation method according to claim 1, wherein the preparation method specifically comprises the following steps:
mixing composite matrix powder, a composite sintering aid, a binder and water, and then performing ball milling and pulping to obtain slurry;
(II) injecting the slurry into a bracket grinding tool to form a bracket green body, drying and degreasing the bracket green body in sequence, and placing the bracket green body in a sealed environment for cold isostatic pressing to obtain a formed bracket green body;
and (III) sequentially carrying out high-temperature sintering and low-temperature sintering on the formed bracket green blank in a vacuum environment, and carrying out furnace air cooling to obtain the tooth bracket.
3. The method according to claim 2, wherein in the step (I), the composite base powder comprises alumina powder and zirconia powder;
preferably, the mass ratio of the alumina powder to the zirconia powder is (4-5): 1;
preferably, the average grain diameter of the alumina powder is 0.1-0.5 μm;
preferably, the average grain diameter of the zirconia powder is 0.1-0.5 μm;
preferably, the mass of the composite sintering aid is 0.1-0.5% of that of the composite matrix powder;
preferably, the composite sintering aid is MgO and SiO2A mixture of (a);
preferably, the MgO and SiO2The mass ratio of (1) to (2-5);
preferably, the mass of the binder is 1-5% of that of the composite matrix powder;
preferably, the binder comprises one or a combination of at least two of polyethylene glycol, polyacrylic acid or stearic acid;
preferably, the mass ratio of the total mass of the composite matrix powder, the composite sintering aid and the binder to the water is 1 (5-10).
4. The preparation method according to claim 2 or 3, characterized in that, in the step (I), the ball milling medium adopted in the ball milling pulping process is Al2O3A pellet;
preferably, the value of the slurry is 1 (2-4) compared with that of the ball milling medium;
preferably, the ball milling time is 12-24 h.
5. The method according to any one of claims 2 to 4, wherein in the step (II), the injection temperature of the slurry is 120 to 150 ℃;
preferably, the injection pressure of the slurry is 70-130 MPa;
preferably, the injection speed of the slurry is 30-90 g/s;
preferably, the temperature of the bracket mould is 40-60 ℃ in the process of injecting the slurry.
6. The method according to any one of claims 2 to 5, wherein in the step (II), the drying temperature is 40 to 60 ℃;
preferably, the drying time is 24-48 h;
preferably, the degreasing process is thermal degreasing, and specifically comprises two stages;
preferably, the first stage of the degreasing process comprises: heating the dried bracket green body to 400-500 ℃ in a protective atmosphere, and then preserving heat for a period of time;
preferably, in the first stage, the temperature rise rate is 1-3 ℃/min;
preferably, in the first stage, the heat preservation time is 1-4 h;
preferably, the second stage of the degreasing process comprises: after the heat preservation in the first stage is finished, continuously heating the bracket green blank to 1100-1200 ℃, preserving heat for a period of time again, and finally cooling to room temperature along with the furnace;
preferably, in the second stage, the temperature rise rate is 3-8 ℃/min;
preferably, in the second stage, the heat preservation time is 1-4 h.
7. The process according to any one of claims 2 to 6, wherein in the step (II), the cold isostatic pressing is carried out at a pressure of 30 to 50 MPa;
and the pressure maintaining time of the cold isostatic pressing is 3-10 min.
8. The method according to any one of claims 2 to 7, wherein in the step (III), the high-temperature sintering process comprises: heating the formed bracket green blank to 1300-1500 ℃, and then preserving heat for a period of time;
preferably, the temperature rise rate of the formed bracket green blank is 3-8 ℃/min, and further preferably, the temperature rise rate is 4-7 ℃/min;
preferably, the heat preservation time in the high-temperature sintering process is 0.5-1.5 h;
preferably, the low-temperature sintering process comprises: after the heat preservation of the high-temperature sintering is finished, cooling the bracket green blank to 1200-1300 ℃ and preserving the heat for a period of time;
preferably, the cooling rate of the bracket green blank after high-temperature sintering is 3-8 ℃/min, and further preferably, the cooling rate is 4-7 ℃/min;
preferably, the heat preservation time in the low-temperature sintering process is 2-6 h.
9. A dental bracket prepared by the preparation method of any one of claims 1 to 8, wherein the dental bracket comprises composite matrix powder, composite sintering aid, binder and water;
wherein the composite matrix powder comprises alumina powder and zirconia powder.
10. The dental bracket of claim 9, wherein the bending strength of the dental bracket is 500MPa or more;
preferably, the hardness of the tooth bracket is more than or equal to 2000 HV;
preferably, the total light transmittance is more than or equal to 90 percent.
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| CN115650706A (en) * | 2022-10-31 | 2023-01-31 | 熵瓷功能材料(江苏)有限公司 | Preparation method of high-entropy ceramic color bracket |
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