CN112759415A - Preparation process of porous ceramic - Google Patents
Preparation process of porous ceramic Download PDFInfo
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- CN112759415A CN112759415A CN202011645347.3A CN202011645347A CN112759415A CN 112759415 A CN112759415 A CN 112759415A CN 202011645347 A CN202011645347 A CN 202011645347A CN 112759415 A CN112759415 A CN 112759415A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000000463 material Substances 0.000 claims abstract description 71
- 239000002002 slurry Substances 0.000 claims abstract description 50
- 239000011148 porous material Substances 0.000 claims abstract description 23
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- 229910000505 Al2TiO5 Inorganic materials 0.000 description 11
- AABBHSMFGKYLKE-SNAWJCMRSA-N propan-2-yl (e)-but-2-enoate Chemical group C\C=C\C(=O)OC(C)C AABBHSMFGKYLKE-SNAWJCMRSA-N 0.000 description 11
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- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 3
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- C04B38/0615—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by burning-out added substances by burning natural expanding materials or by sublimating or melting out added substances the burned-out substance being a monolitic element having approximately the same dimensions as the final article, e.g. a porous polyurethane sheet or a prepreg obtained by bonding together resin particles
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- C04B35/46—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 titanium oxides or titanates
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Abstract
A preparation process of porous ceramic relates to the technical field of ceramic. The preparation process of the porous ceramic comprises the following steps: the method comprises the steps of printing a three-dimensional model material with three-dimensional communicating holes by adopting resin in a 3D mode, coating ceramic slurry containing an adhesive on the surface of a framework of the three-dimensional model material, drying and curing, then carrying out heat treatment to enable the adhesive to be pyrolyzed and degreased and enable the three-dimensional model material to be decomposed to obtain a ceramic blank, and sintering and forming the ceramic blank. The preparation process can prepare the porous ceramic with better pore connectivity.
Description
Technical Field
The application relates to the technical field of ceramics, in particular to a preparation process of porous ceramics.
Background
The porous ceramic with holes is widely applied to the fields of metal smelting, catalyst carriers, heat insulation materials, porous medium burners and the like. The applicant researches and discovers that the holes of the porous ceramic are generally formed by a pore-forming agent or obtained by injecting ceramic slurry into a mold for sintering and molding, however, the holes formed by the pore-forming agent are generally closed-cell structures and are difficult to achieve good three-dimensional communication; the holes obtained by injecting the ceramic slurry into a mold for sintering are generally straight-hole type holes, and the porous ceramics prepared by the two methods are not suitable for the use environment requiring high airflow flux.
Disclosure of Invention
The application provides a preparation process of porous ceramic, which can prepare porous ceramic with better pore connectivity.
The embodiment of the application is realized as follows:
the embodiment of the application provides a preparation process of porous ceramic, which comprises the following steps:
the method comprises the steps of printing a three-dimensional model material with three-dimensional communicating holes by adopting resin in a 3D mode, coating ceramic slurry containing an adhesive on the surface of a framework of the three-dimensional model material, drying and curing, then carrying out heat treatment to enable the adhesive to be pyrolyzed and degreased and enable the three-dimensional model material to be decomposed to obtain a ceramic blank, and sintering and forming the ceramic blank.
The preparation process of the porous ceramic has the beneficial effects that:
the three-dimensional model material with the three-dimensional intercommunicating pores can be printed by a 3D printing technology, the three-dimensional model material has the three-dimensional intercommunicating pores, after ceramic slurry is coated on the surface of a framework of the three-dimensional model material, the pores of the three-dimensional model material still remain, the ceramic slurry is solidified on the surface of the framework of the three-dimensional model material after drying and curing, after heat treatment, the adhesive is pyrolyzed and degreased, the three-dimensional model material made of resin is decomposed, only a ceramic blank remains, the ceramic blank is sintered and formed into porous ceramic, the porous ceramic retains the pores of the three-dimensional model material, has the pores with high three-dimensional intercommunicating height, and can be suitable for use environments requiring high airflow.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings that are required to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present application and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained from the drawings without inventive effort.
FIG. 1 is a porous ceramic according to an embodiment of the present disclosure;
FIG. 2 is a three-dimensional model of a three-dimensional modeling material according to an embodiment of the present application;
FIG. 3 is an SEM photograph of a porous ceramic of example 1 of the present application;
fig. 4 is an XRD pattern of the porous ceramic of example 1 of the present application.
Detailed Description
Embodiments of the present application will be described in detail below with reference to examples, but those skilled in the art will appreciate that the following examples are only illustrative of the present application and should not be construed as limiting the scope of the present application. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The following is a detailed description of the process for preparing the porous ceramic according to the embodiments of the present application:
the embodiment of the application provides a preparation process of porous ceramic, which comprises the following steps:
the method comprises the steps of printing a three-dimensional model material with three-dimensional communicating holes by adopting resin in a 3D mode, coating ceramic slurry containing an adhesive on the surface of a framework of the three-dimensional model material, drying and curing, then carrying out heat treatment to enable the adhesive to be pyrolyzed and degreased and enable the three-dimensional model material to be decomposed to obtain a ceramic blank, and sintering and forming the ceramic blank.
The three-dimensional model material with three-dimensional intercommunicating pores can be printed by a 3D printing technology, the three-dimensional model material has three-dimensional intercommunicating pores, after ceramic slurry is coated on the surface of a framework of the three-dimensional model material, the pores of the three-dimensional model material still remain, the slurry is solidified on the surface of the framework of the three-dimensional model material after drying and curing, after heat treatment, the adhesive is pyrolyzed and degreased, the three-dimensional model material is decomposed, only a ceramic blank remains, the ceramic blank is sintered and formed into porous ceramic (refer to figure 1), the porous ceramic retains the pores of the three-dimensional model material, has the highly three-dimensional intercommunicating pores, and can be suitable for use environments requiring high airflow flux, such as a porous medium burner, a high-temperature. It is understood that the three-dimensional communication holes refer to that the holes of the three-dimensional model material communicate not only in one direction, for example, the three-dimensional communication holes may communicate in both the thickness direction and the length direction of the three-dimensional model material.
Illustratively, the step of 3D printing out a three-dimensional model material having three-dimensional communication holes using a resin includes:
a three-dimensional model of a three-dimensional model material (see fig. 2) is designed, converted into a USP format, input into a 3D printer, and then printed out by the 3D printer using resin. Alternatively, UTR9000E photosensitive resin may be used as the resin.
3D prints and can print layer by layer, through repeated stack layer by layer, can print out the material that the structure is complicated. The pore structure, pore shape and pore size of the three-dimensional model material printed by 3D are controllable. Illustratively, the pore size of the three-dimensional model material varies in a gradient manner along a predetermined direction, for example, the three-dimensional model material comprises at least three layers of pore structures arranged along the thickness direction, the pore diameter of each layer of pore structure is the same, and the pore size of each layer of pore structure gradually increases or decreases along the thickness direction of the three-dimensional model material. Optionally, the shape of the holes of the three-dimensional model material is a polygon or a circle.
In one possible embodiment, the step of coating the skeleton surface of the three-dimensional model material with the ceramic slurry comprises:
and immersing the three-dimensional model material into the ceramic slurry to obtain a ceramic precursor, taking out the ceramic precursor, and removing the ceramic slurry in the three-dimensional communicating hole under the action of an external force.
The diameter of the hole of the three-dimensional model material is 0.1-10 mm. It should be noted that the three-dimensional model material with the diameter of the hole is suitable for being immersed in the ceramic slurry to enable the surface of the framework of the three-dimensional model material to be wrapped with the ceramic slurry, and the hole is not suitable for being filled with the ceramic slurry by injecting the slurry into the hole due to the small diameter of the hole. Optionally, the three-dimensional modeling material has a hole diameter of any one of 0.1mm, 1mm, 2mm, 4mm, 5mm, 7mm, 8mm, and 10mm or a range between any two.
In addition, the ceramic slurry in the three-dimensional communicating holes can be removed under the action of external force, so that the holes of the three-dimensional model material are reserved, and the hole connectivity of the porous ceramic can be better ensured.
Further, the means for removing the ceramic slurry in the three-dimensional communication holes by the external force includes at least one of a centrifugal treatment, a purge treatment, and a vibration treatment of the ceramic precursor.
Redundant slurry can be thrown away through centrifugal treatment, the slurry in the holes of the three-dimensional model material can be vibrated out through a vibration mode, and the redundant slurry in the holes of the ceramic precursor can be blown out through a blowing mode, so that the holes of the three-dimensional model material are well reserved.
Illustratively, the purging process can adopt compressed gas purging, and the pressure of the compressed gas is 0.3-0.6 MPa. Wherein the compressed gas is optionally compressed air or compressed inert gas. The pressure of 0.3-0.6 MPa is proper, so that redundant slurry in the holes of the ceramic precursor can be blown out, and the influence on the strength of the formed porous ceramic caused by the fact that the slurry wrapped on the surface of the framework of the three-dimensional model material is blown away due to overlarge pressure can be avoided.
When the ceramic precursor is treated by two or three of the centrifugal treatment, the purging treatment and the vibration treatment, the order of the steps of the centrifugal treatment, the purging treatment and the vibration treatment is not limited, and can be selected according to actual conditions. In addition, the steps of slurry dipping, ceramic precursor treatment under the action of external force, drying and curing can be repeated until the slurry hanging of the three-dimensional model material reaches the target volume fraction or the target mass fraction. The determination method of the target volume fraction and the target mass fraction comprises the following steps: multiplying the length, the width and the height of the three-dimensional model material to obtain a first volume, multiplying the first volume by the density of the ceramic particles in the adopted ceramic slurry to obtain a first weight, dividing the weight of the hanging slurry by the density of the adopted ceramic particles to obtain a second volume, and dividing the second volume by the first volume to obtain a target volume fraction; dividing the weight of the hanging pulp by the first weight to be a target mass fraction.
Optionally, the temperature for drying and curing is 50-150 ℃. In the temperature range of 50-150 ℃, the ceramic slurry can be solidified on the surface of the framework of the three-dimensional model material, and meanwhile, the three-dimensional model material is not decomposed, so that a ceramic body with a stable structure can be obtained. Illustratively, the temperature of the dry curing is any one of 50 ℃, 70 ℃, 90 ℃, 100 ℃, 110 ℃, 130 ℃ and 150 ℃ or a range between any two.
In one possible embodiment, the ceramic slurry includes alumina, titanium dioxide, a dispersant, a binder, a stabilizer, and a solvent for dissolving the binder.
The porous ceramic prepared by the ceramic slurry is aluminum titanate porous ceramic, wherein the adhesive can be dissolved in a solvent, the dispersing agent can promote the stabilizing agent, the aluminum oxide and the titanium dioxide to be uniformly dispersed in the dissolved adhesive, and the adhesive can bond the aluminum oxide, the titanium dioxide and the stabilizing agent together. The aluminum oxide and the titanium dioxide can react to generate the aluminum titanate, and the stabilizer can stabilize the crystalline phase of the aluminum titanate, so that the aluminum titanate porous ceramic has higher thermal shock resistance. In the present embodiment, the kind of the ceramic slurry is not particularly limited.
Illustratively, the stabilizer includes at least one of magnesium oxide, magnesite, magnesium carbonate, silica, ferric oxide, cerium oxide, lanthanum oxide, and yttrium oxide. Illustratively, the titanium dioxide includes at least one of anatase type, rutile type, and amorphous titanium dioxide.
Illustratively, the binder is selected from at least one of phenolic resin, epoxy resin, polyacrylic acid resin, and polyvinyl butyral. Alternatively, the solvent comprises ethanol and butanone. Ethanol can well dissolve the adhesives, and butanone and ethanol can be matched to achieve the effects of solubilization and dispersion. Illustratively, the volume ratio of ethanol to butanone is 1-4: 1 is, for example, 1:1, 2:1, 3:1 or 4: 1.
Optionally, the weight ratio of alumina, titania to stabilizer is 50-70: 30-50: 1-10. The weight ratio of the total weight of the aluminum oxide, the titanium dioxide and the stabilizer to the weight of the adhesive, the weight of the dispersant and the weight of the solvent is 100: 18-50: 0.1-10: 30-50. The ceramic slurry obtained by mixing the components in the proportion has proper viscosity and is easier to wrap on the surface of the framework of the three-dimensional model material.
Illustratively, the particle size of the alumina is required to be 0.5-5 μm D50, the particle size of the titanium dioxide is required to be 0.1-5 μm D50, and the particle size of the stabilizer is required to be 0.5-2 μm D50. The ceramic slurry comprising the alumina, the titanium dioxide and the stabilizer in the particle size range does not collapse due to large shrinkage caused by too fine particle size during sintering. In addition, D50-0.5 to 5 μm means the proportion of alumina having a particle size in the range of 0.5 to 5 μm.
Further, in one possible embodiment, the pyrolysis temperature is 800-.
Optionally, the pyrolysis process is performed in an inert atmosphere or in a vacuum environment, which can increase the strength of the ceramic body, in which case the ceramic body can be further processed after pyrolysis and then sintered for forming.
The process for preparing the porous ceramic of the present application will be described in further detail with reference to examples.
Example 1
The embodiment provides a preparation process of porous ceramic, which comprises the following steps:
designing a three-dimensional model of the three-dimensional model material, converting the three-dimensional model into USP format, inputting the USP format into a 3D printer, and printing the three-dimensional model material by using resin through the 3D printer, wherein the size of the three-dimensional model material is 140mmx290mmx25mm, and the shape of a hole is a square with the side length of 2 mm.
Immersing the printed three-dimensional model material into aluminum titanate ceramic slurry, taking out, centrifuging and throwing off redundant slurry, uniformly blowing the slurry on the surface of the three-dimensional model material by using 0.3MPa compressed air, and then drying the slurry in a forced air drying oven for 30min at the temperature of 100 ℃; the steps of slurrying, centrifuging, purging and drying are repeated until the volume fraction of the three-dimensional modeling material reaches 20%. Wherein the aluminum titanate ceramic slurry is prepared by calcining alpha-Al2O33kg of (D50 ═ 2 μm), 2kg of anatase titanium dioxide (D50 ═ 0.3 μm), 300g of magnesium carbonate powder (D50 ═ 0.5 μm), 350g of silica powder (D50 ═ 1 μm), 10g of ferric oxide (analytically pure), 16g of lanthanum oxide (analytically pure), 1.2kg of phenolic resin, 20g of polyvinyl butyral, 15g of castor oil, 5g of glycerol trioleate, 1600g of ethanol and 400g of butanone, and the mixture was subjected to ball milling for 5 hours.
Putting the three-dimensional model material subjected to slurry coating into a vacuum degreasing furnace, performing pyrolysis for 15 hours at 900 ℃, and introducing high-purity nitrogen for protection; and (3) after pyrolysis, keeping the temperature of 1600 ℃ for 5 hours in a high-temperature electric furnace with air atmosphere for sintering to obtain the aluminum titanate porous ceramic.
Example 2
The embodiment provides a preparation process of porous ceramic, which comprises the following steps:
designing a three-dimensional model of the three-dimensional model material, converting the three-dimensional model into USP format, inputting the USP format into a 3D printer, and printing the three-dimensional model material by using resin through the 3D printer, wherein the size of the three-dimensional model material is 140mmx100mmx25mm, and the shape of a hole is a square with the side length of 1.5 mm.
Immersing the printed three-dimensional model material into aluminum titanate ceramic slurry, taking out, centrifuging, throwing off redundant slurry, uniformly blowing the slurry on the surface of the three-dimensional model material by using 0.6MPa compressed air, and then drying the slurry in a blast drying oven for 30min at the temperature of 120 ℃; the steps of slurry dipping, centrifugation, purging and drying are repeated until the volume fraction of the three-dimensional model material reaches 30%. Wherein the aluminum titanate ceramic slurry is prepared by calcining alpha-Al2O33.2kg (D50 ═ 1 μm), 1.8kg of anatase titanium dioxide (D50 ═ 0.3 μm), 100g of magnesium oxide (analytical grade), 12g of ferric oxide (analytical grade), 20g of lanthanum oxide (analytical grade), 1kg of phenolic resin, 25g of polyvinyl butyral, 20g of Tween 20, 1400g of ethanol and 600g of butanone, and the mixture was ball-milled for 5 hours.
Putting the three-dimensional model material subjected to slurry coating into a vacuum degreasing furnace, performing pyrolysis for 20 hours at 800 ℃, and introducing high-purity nitrogen for protection; and after pyrolysis, the mixture is sintered in a high-temperature electric furnace with air atmosphere at the temperature of 1550 ℃ for 5 hours to obtain the aluminum titanate porous ceramic.
Example 3
This example provides a process for preparing a porous ceramic, which is substantially the same as that of example 1 except that the pyrolysis process of example 3 is performed in an air atmosphere.
Test example 1
The porosity of the porous ceramics obtained in examples 1 and 2 was measured by the drainage method, and the results are shown in table 1.
TABLE 1 porosity of porous ceramics
| Example 1 | Example 2 | |
| Porosity of the material | 85％ | 81％ |
As can be seen from the results of table 1, the porous ceramics obtained in examples 1 and 2 of the present application have a high porosity, which indicates that the porous ceramics having a porosity of more than 80% can be obtained by the process for preparing the porous ceramics of the examples of the present application.
Test example 2
The porous ceramics obtained in example 1 and example 2 were subjected to a water-cooling thermal shock test, which included the following steps: heating a muffle furnace to 1400 ℃, putting the porous ceramic into the furnace, keeping the temperature for 5min, clamping the porous ceramic, putting the porous ceramic into water, taking the porous ceramic out of the water, drying the porous ceramic, observing whether the porous ceramic cracks or not by using a magnifying glass, and continuing the circulating water-cooling thermal shock process if the porous ceramic does not crack.
And (3) testing results: the porous ceramics of example 1 and example 2 have no cracking after 10 times of water-cooling thermal shock, which shows that the porous ceramics of example 1 and example 2 of the present application have good thermal shock resistance.
Test example 3
The porous ceramic obtained in example 1 was observed under an electron scanning microscope to obtain an SEM image as shown in FIG. 3, and the porous ceramic obtained in example 1 was subjected to an XRD test to obtain a result as shown in FIG. 4, wherein AT in FIG. 4 represents an aluminum titanate crystal phase.
Test example 4
The ceramic green bodies and porous ceramics obtained in example 1, the porous ceramics obtained in example 3, and the ceramic green bodies obtained in example 4 were tested for their compressive strength, and the results are shown in table 2.
TABLE 2 compressive strength of ceramic green bodies and porous ceramics
As can be seen from the results in Table 2, the pyrolysis process in example 3 was carried out in an air atmosphere, and the compressive strength of the resulting ceramic body was much lower than that of the ceramic body in example 1.
The foregoing is illustrative of the present application and is not to be construed as limiting thereof, as numerous modifications and variations will be apparent to those skilled in the art. Any modification, equivalent replacement, improvement and the like made within the spirit and principle of the present application shall be included in the protection scope of the present application.
Claims (10)
1. A process for preparing a porous ceramic, comprising:
the method comprises the steps of printing a three-dimensional model material with three-dimensional communicating holes by using resin in a 3D mode, coating ceramic slurry containing an adhesive on the surface of a framework of the three-dimensional model material, drying and curing, then carrying out heat treatment to enable the adhesive to be pyrolyzed and degreased and enable the three-dimensional model material to be decomposed to obtain a ceramic blank, and sintering and forming the ceramic blank.
2. The process for preparing a porous ceramic according to claim 1, wherein the step of coating the skeleton surface of the three-dimensional model material with the ceramic slurry comprises:
and immersing the three-dimensional model material into ceramic slurry to obtain a ceramic precursor, taking out the ceramic precursor, and removing the ceramic slurry in the three-dimensional communicating hole under the action of external force.
3. The process for preparing a porous ceramic according to claim 2, wherein the means for removing the ceramic slurry in the three-dimensional communication holes by an external force comprises at least one of a centrifugal treatment, a purge treatment and a vibration treatment of the ceramic precursor.
4. The preparation process of the porous ceramic according to claim 3, wherein the purging process adopts compressed gas for purging, and the pressure of the compressed gas is 0.3-0.6 MPa.
5. The process for preparing a porous ceramic according to any one of claims 1 to 4, wherein the diameter of the pores of the three-dimensional model material is 0.1 to 10 mm.
6. The process for preparing porous ceramic according to any one of claims 1 to 4, wherein the size of the pores of the three-dimensional model material is changed in a gradient manner along a predetermined direction.
7. The process for preparing a porous ceramic according to any one of claims 1 to 4, wherein the temperature for drying and curing is 50 to 150 ℃.
8. The process for preparing porous ceramic according to any one of claims 1 to 4, wherein the pyrolysis is performed in an inert atmosphere or a vacuum environment.
9. The process for preparing a porous ceramic according to any one of claims 1 to 4, wherein the ceramic slurry comprises alumina, titanium dioxide, the binder, a stabilizer, a dispersant and a solvent for dissolving the binder.
10. The process for preparing porous ceramics according to claim 9, wherein the particle size of the alumina is required to be 0.5 to 5 μm when D50 is cut, the particle size of the titanium dioxide is required to be 0.1 to 5 μm when D50 is cut, and the particle size of the stabilizer is required to be 0.5 to 2 μm when D50 is cut.
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