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CN109400011A - A kind of nanometer heat insulation material material and its mixed method, nanometer heat insulation material and preparation method thereof - Google Patents

A kind of nanometer heat insulation material material and its mixed method, nanometer heat insulation material and preparation method thereof Download PDF

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Publication number
CN109400011A
CN109400011A CN201811409159.3A CN201811409159A CN109400011A CN 109400011 A CN109400011 A CN 109400011A CN 201811409159 A CN201811409159 A CN 201811409159A CN 109400011 A CN109400011 A CN 109400011A
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heat insulation
insulation material
nanometer heat
powder
nano
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CN109400011B (en
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张凡
安煊熜
李文静
杨洁颖
赵英民
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Aerospace Research Institute of Materials and Processing Technology
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Aerospace Research Institute of Materials and Processing Technology
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    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B26/00Compositions of mortars, concrete or artificial stone, containing only organic binders, e.g. polymer or resin concrete
    • C04B26/02Macromolecular compounds
    • C04B26/28Polysaccharides or derivatives thereof
    • C04B26/285Cellulose or derivatives thereof
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2201/00Mortars, concrete or artificial stone characterised by specific physical values
    • C04B2201/20Mortars, concrete or artificial stone characterised by specific physical values for the density
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2201/00Mortars, concrete or artificial stone characterised by specific physical values
    • C04B2201/30Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values
    • C04B2201/32Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values for the thermal conductivity, e.g. K-factors
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2201/00Mortars, concrete or artificial stone characterised by specific physical values
    • C04B2201/50Mortars, concrete or artificial stone characterised by specific physical values for the mechanical strength

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Thermal Insulation (AREA)

Abstract

The present invention relates to a kind of nanometer heat insulation material material and its mixed method, nanometer heat insulation materials and preparation method thereof.Mixed method are as follows: ceramic fibre is uniformly dispersed with water, is then dried, pre-dispersed ceramic fibre is obtained;Nano-powder, pre-dispersed ceramic fibre and dispersion aids selected from the group being made of neopelex, methylcellulose, carboxymethyl cellulose, hydroxyethyl cellulose and polyethylene glycol oxide are subjected to mechanical fusion, obtain nanometer heat insulation material material.The nanometer heat insulation material the preparation method comprises the following steps: by being uniformly mixed by weight percentage for 85~100% material and 0~15% additive, obtain mixture;Mixture is molded, nanometer heat insulation material is made.Mixed method in the present invention realizes the uniform mixing of material under the premise of not destroying the microstructure of fiber morphology and nano-powder;The present invention can be made that density is small, thermal coefficient is low, the nanometer heat insulation material of excellent in mechanical performance.

Description

A kind of nanometer heat insulation material material and its mixed method, nanometer heat insulation material and its Preparation method
Technical field
The invention belongs to functional composite material technical field more particularly to a kind of nanometer heat insulation material material and its mixing Method, nanometer heat insulation material and preparation method thereof.
Background technique
High-temperature fibre, nano-powder are the main raw material(s) for preparing high-performance nano heat-barrier material, the main work of fiber With being mechanics enhancing, the main function of nano-powder is to inhibit heat transmitting, is used to prepare after two kinds of raw material are evenly dispersed efficiently Nanometer heat insulation material, therefore powder fiber pre-processes the performance that mixed quality directly affects efficient nano heat-barrier material.
In order to guarantee that powder fiber preferably pre-processes mixing, it is necessary to scattered fiber and powder.Disperse from fiber Angle sees mainly there is physical dispersion and function additive dispersion, but inorfil brittleness is big, and diameter is small, surface area is big, Yi Cheng Beam, fiber dispersion can be poor, and current main powder fiber dispersing method has: 1, ultrasonic disperse belongs to wet dispersion, and leads to It crosses the material that wet dispersion obtains and needs first to remove solvent in nanometer heat insulation material in subsequent prepare, and the removal process meeting of solvent The density of material is caused to increase, the thermal coefficient of material increases, and high performance nanometer heat insulation material can not be made;2, mechanical stirring Dispersion causes the movement of liquid stream strong turbulence to cause particle agglomeration size degradation, fiber beam spreading solution, to accelerate by strong mechanical stirring Dispersion, also belongs to wet dispersion;3, kneader, is mainly used in high viscosity, the mixing of high-elastic plastic material, dispersion, and stemness is low The dispersion effect of binder fiber is bad;4, conventional mechanical disperses, and easily causes fibrous fracture, weakens reinforcing effect, limits fiber Mechanics enhances the performance of performance, is unfavorable for improving the comprehensive performance of nanometer heat insulation material.
Therefore need to provide a kind of pretreatment mixed method of nano-powder fiber, to prepare high-performance nano heat-barrier material It lays the foundation.
Summary of the invention
In order to solve one or more technical problem existing in the prior art, the present invention provides a kind of nano heat-insulatings Material material and its mixed method, nanometer heat insulation material and preparation method thereof.Mixed method in the present invention is not destroying fibre Under the premise of the microstructure for tieing up pattern and nano-powder, the uniform mixing of material is realized;The method of the present invention can be made close Spend that small, thermal coefficient is low, the high-performance nano heat-barrier material of excellent in mechanical performance.
To achieve the goals above, the present invention provides a kind of preparation method of nanometer heat insulation material, institute in first aspect The method of stating includes the following steps:
(1) ceramic fibre is uniformly dispersed with water, obtains slurry, then dry the slurry, obtain pre-dispersed pottery Porcelain fiber;
(2) by nano-powder, pre-dispersed ceramic fibre and selected from by neopelex, methylcellulose, carboxylic The dispersion aids of the group of methylcellulose, hydroxyethyl cellulose and polyethylene glycol oxide composition carries out mechanical fusion, and it is equal to obtain mixing Even nanometer heat insulation material material.
Preferably, the nanometer heat insulation material material by by weight percentage for 55~85% nano-powder, 14 ~40% pre-dispersed ceramic fibre and 0.5~5% dispersion aids composition;And/or in step (1), the ceramics are fine The dosage of dimension is 0.5~1wt% of the dosage of the water.
Preferably, the revolving speed of the mechanical fusion is 300~1600r/min, time of the mechanical fusion is 1~ 3600min。
Preferably, the nano-powder is selected from by silica nano-powder, nanometer alumina powder, zirconia nano-powder The group of body, nano-sized SiC powder and Nano-silicon Nitride Powder composition;And/or the ceramic fibre is selected from by quartz fibre, height The group of silica fiber, glass fibre, mullite fiber, basalt cotton fiber, alumina fibre and Zirconium oxide fibre composition.
Preferably, the partial size of the nano-powder is 0.1~1000nm;And/or the diameter of the ceramic fibre be 0.1~ 50um, the length of the ceramic fibre are 0.1~50mm.
The present invention provides the nano heat-insulating material that mixed method of the present invention described in first aspect obtains in second aspect Material uses material.
The present invention provides the nano heat-insulating material that mixed method of the present invention described in first aspect obtains in the third aspect The method that material prepares nanometer heat insulation material with material, described method includes following steps:
(a) it will be mixed by weight percentage for 85~100% nanometer heat insulation material material and 0~15% additive It closes uniformly, obtains mixture;
(b) mixture in step (a) is molded, nanometer heat insulation material is made.
Preferably, the method also includes carrying out pressure maintaining for nanometer heat insulation material obtained in step (b).
Preferably, the pressure of the molding is 0.5~20MPa, and the speed of the molding is 0.1~50mm/s;The guarantor The pressure of pressure is identical as the pressure of the molding, and the time of the pressure maintaining is 0.5~60min;And/or the additive be selected from by The group of silicon carbide, silicon nitride, titanium dioxide and carbon dust composition.
The present invention provides the nano heat-insulating material that mixed method of the present invention described in first aspect obtains in fourth aspect Nanometer heat insulation material made from the method for material material or the present invention described in the third aspect.
The present invention at least have compared with prior art it is following the utility model has the advantages that
(1) present invention first carries out ceramic fibre pre-dispersed, then by nano-powder, pre-dispersed ceramic fibre and helps Dispersing agent carries out mechanical fusion, wherein pre-dispersed ceramic fibre is conducive to improve the effect of mechanical fusion, nano-powder and pre- The ceramic fibre of dispersion is able to carry out stable fusion, and dispersion aids is added and similarly effectively promotes the mixing point of material Effect is dissipated, the present invention can leniently be dispersed fiber by the way of mechanical fusion, not destroy fiber morphology and nano-powder Microstructure under the premise of, realize the uniform mixing of material, solve material present in existing dispersion mixing process mixing not Uniformly, be easy to lead to problems such as in mixed process fibrous fracture, nano-powder it is destructurized.
(2) mixed method of the invention is not necessarily to add the dispersion solvent of liquid, belongs to dry mixed, is suitable for preparation density Low, the high-performance nanos heat-barrier material such as thermal coefficient is low, and it is easy the composition and ratio of accurate control material, it is final to realize to height The preparation of performance nanometer heat insulation material.
(3) mixed method in the present invention can be used for uniformly mixing nano-powder and ceramic fibre, to prepare high-performance Nanometer heat insulation material is laid a good foundation;In addition, the mixed method in the present invention can also be used for other micrometer/nanometer scale complexs The mixing of system has universality.
(4) method that nanometer heat insulation material is prepared in the present invention, using nanometer heat insulation material material of the present invention For raw material, so that nanometer heat insulation material produced by the present invention has, density is small, thermal coefficient is low, mechanical strength is high, comprehensive performance The advantages that excellent, the method that the present invention prepares nanometer heat insulation material is simple and fast, low to equipment and environmental requirement, be it is a kind of it is low at This nanometer heat insulation material preparation method;The method parameter easy-regulating for preparing nanometer heat insulation material of the invention, can be according to work Skill needs are adjusted.
Detailed description of the invention
Attached drawing of the present invention only provides for the purpose of illustration, and the size in figure is not necessarily consistent with actual product.
Fig. 1 is not same order of the ceramic fibre in a specific embodiment of mixed method of the present invention in pre-dispersing operation The pictorial diagram of section.In figure: the pictorial diagram of the ceramic fibre before (a) indicating pre-dispersed;(b) indicate mixed comprising ceramic fibre and water Close the pictorial diagram of object;(c) the part pictorial diagram of the finely dispersed slurry comprising ceramic fibre and water is indicated;(d) ceramics are indicated Fiber filters out the pictorial diagram after water;(e) pictorial diagram of pre-dispersed ceramic fibre is indicated.
Fig. 2 is the pictorial diagram of the nano-powder in a specific embodiment of mixed method of the present invention.
Fig. 3 is the pictorial diagram for the pre-dispersed ceramic fibre for including in Fig. 1.
Fig. 4 is the pictorial diagram of the nanometer heat insulation material material in a specific embodiment of mixed method of the present invention.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, right below in conjunction with the embodiment in the present invention Technical solution of the present invention is clearly and completely described, it is clear that described embodiment is that a part of the invention is implemented Example, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art are not making creativeness Every other embodiment obtained, shall fall within the protection scope of the present invention under the premise of labour.
The present invention provides a kind of mixed method of nanometer heat insulation material material in first aspect, and the method includes such as Lower step:
(1) ceramic fibre is uniformly dispersed with water, obtains slurry, then dry the slurry, obtain pre-dispersed pottery Porcelain fiber;In the present invention, such as wet ceramic fibre can be uniformly dispersed under blender effect, obtains slurry, then It filters out dispersing agent (water) to dry the slurry, obtains the ceramic fibre of pre-dispersed (pretreatment);The present invention is to the blender The revolving speed of (high speed disperser) and the time being dispersed with stirring are not particularly limited, and the revolving speed of the blender for example can be 500~1000r/min (such as 500,600,700,800,900 or 1000r/min), the time being dispersed with stirring for example can be 1 ~20min (such as 1,2,3,4,5,6,7,8,9,10,11,12,13,14,15,16,17,18,19 or 20min);In the present invention In, the temperature of the drying for example can be 80~120 DEG C, and the time of the drying for example can be 24~36h;
(2) by nano-powder, pre-dispersed ceramic fibre and selected from by neopelex, methylcellulose, carboxylic The dispersion aids of the group of methylcellulose, hydroxyethyl cellulose and polyethylene glycol oxide (PEO) composition carries out mechanical fusion, is mixed Close uniform nanometer heat insulation material material.It in the present invention, such as can be by described in the progress of existing mechanical fusion equipment Mechanical fusion;In the present invention, for example, the nano-powder, pre-dispersed ceramic fibre and dispersion aids are put into machinery In fusion device, the powder substance first in the rotation container (revolving sleeve) of mechanical fusion equipment is acted on by centrifugal force, simultaneously Under pressure head auxiliary, safely dispersed towards squeezing on the chamber wall of rotation container, the powder substance being extruded is from revolving sleeve Hole at be discharged, then brought by circulating blade to the extruding dispersion for above revolving sleeve, repeating front, in this way, nano-powder Fusion can be stablized under certain revolving speed and time effect with pre-dispersed ceramic fibre, it is final to realize nano-powder and ceramics Fiber it is evenly dispersed.
The present invention first carries out ceramic fibre pre-dispersed, then by nano-powder, pre-dispersed ceramic fibre and helps point Powder carries out mechanical fusion, wherein first by the way that ceramic fibre is become puffy, puffy to ceramic fibre progress is pre-dispersed Ceramic fibre can effectively improve the effect of mechanical fusion, realize that the efficient mixing of nano-powder and ceramic fibre disperses, with Ceramic fibre is directly subjected to dispersed phase ratio by stirring action, without strict control dispersion revolving speed and time, revolving speed is not present The too low or time, the too short fiber that will lead to was unable to fully disperse, and revolving speed is too high or the time is too long, can make fibrous fracture, to drop The problem of low reinforcing effect;Nano-powder and pre-dispersed ceramic fibre in the present invention are able to carry out stable fusion, and add Enter dispersion aids and similarly effectively promote the mixing dispersion effect of material, the present invention being capable of temperature by the way of mechanical fusion The uniform mixing of material is realized under the premise of not destroying the microstructure of fiber morphology and nano-powder with ground dispersion fiber, is solved Material present in existing dispersion mixing process of having determined mixing is uneven, avoids and is easy to lead in simple and mechanical mixing dispersion process The problems such as causing fiber cut-off, nano-powder destructurized.
Mixed method of the invention is not necessarily to add the dispersion solvent of liquid, belongs to dry mixed, low suitable for preparation density, The low equal high-performance nanos heat-barrier material of thermal coefficient, and it is easy the composition and ratio of accurate control material, it is final to realize to high property The preparation of energy nanometer heat insulation material.
According to some preferred embodiments, the nanometer heat insulation material material by by weight percentage be 55~ The nano-powder of 85% (such as 55%, 60%, 65%, 70%, 75%, 80% or 85%), 14~40% (such as 14%, 16%, 18%, 20%, 22%, 25%, 28%, 30%, 32%, 35%, 38% or pre-dispersed ceramic fibre 40%) and 0.5~5% (such as 0.5%, 0.8%, 1%, 1.5%, 2%, 2.5%, 3%, 3.5%, 4%, 4.5% or 5%) helps point Powder composition.In the present invention, the dispersion aids that the especially dosage of each component under this proportion is 0.5~5%, can more have Effect ground guarantees the mixed uniformity of nano-powder and ceramic fibre, and the nanometer heat insulation material material under this proportion It is more advantageous to the efficient nano heat-barrier material of obtained excellent combination property.
According to some preferred embodiments, in step (1), the dosage of the ceramic fibre is the dosage of the water 0.5~1wt% (such as 0.5wt%, 0.55wt%, 0.6wt%, 0.65wt%, 0.7wt%, 0.75wt%, 0.8wt%, 0.85wt%, 0.9wt%, 0.95wt% or 1wt%).In the present invention, excellent when carrying out pre-dispersed to the ceramic fibre The mass ratio for being selected as the ceramic fibre and the water is (0.5~1): 100, it can better ensure that ceramic fibre is pre-dispersed Effect, to better assure that the uniformity of subsequent nano-powder and ceramic fibre mixing dispersion.
According to some preferred embodiments, the revolving speed of the mechanical fusion be 300~1600r/min (such as 300, 400,500,600,700,800,900,1000,1100,1200,1300,1400,1500 or 1600r/min), preferably 1000 The time of~1500r/min (1000,1100,1200,1300,1400 or 1500r/min) described mechanical fusion be 1~ 3600min (such as 1,5,10,20,30,60,80,120,160,200,240,280,320,360,400,500,600,700, 800,900,1000,1200,1600,2000,2400,3000 or 3600min), preferably 30~180min (such as 30,60, 120,150 or 180min).
According to some preferred embodiments, the nano-powder is selected from by silica nano-powder (such as silicon monoxide Nano-powder or silicon dioxide nano powder), nanometer alumina powder, nm-class powder of zirconium oxide, nano-sized SiC powder and nitrogen The group of SiClx nano-powder composition;And/or the ceramic fibre is selected from by quartz fibre, high silica fiber, glass fibre, Mo Lai The group of mineral wool, basalt cotton fiber, alumina fibre and Zirconium oxide fibre composition.
According to some preferred embodiments, the partial size of the nano-powder is 0.1~1000nm, preferably 5~ 100nm;And/or the diameter of the ceramic fibre is 0.1~50um, the length of the ceramic fibre is 0.1~50mm.
The present invention provides the nano heat-insulating that the mixed method as the present invention described in first aspect obtains in second aspect Material material.The density for the nanometer heat insulation material material that the present invention obtains is 0.03~0.09g/cm3, room temperature thermal conductivity 0.014~0.035W/mK of rate.
The present invention provides the nano heat-insulating that the mixed method as the present invention described in first aspect obtains in the third aspect The method that material prepares nanometer heat insulation material with material, described method includes following steps:
(a) will by weight percentage for 85~100% (such as 85%, 88%, 90%, 92%, 95%, 98% or 100%) nanometer heat insulation material material and 0~15% (such as 0%, 1%, 2%, 5%, 8%, 10%, 12% or 15%) Additive (such as with the additive for inhibiting thermal radiation function) be uniformly mixed (such as by mechanical dispersion or mechanical fusion Mode is uniformly mixed), obtain mixture;It certainly in the present invention, can also be fine by the nano-powder, pre-dispersed ceramics Dimension, the additive and selected from by neopelex, methylcellulose, carboxymethyl cellulose, hydroxyethyl cellulose and The dispersion aids of the group of polyethylene glycol oxide (PEO) composition carries out the mechanical fusion together, obtains the mixture.
(b) mixture in step (a) is molded (compression molding or compression moulding), nanometer heat insulation material is made; For example, in the present invention, the mixture in step (a) is layed in mold, mixture to be molded is stirred by scraper plate, is made Laying it is uniform after carry out the compression molding again, advantageously ensure that the quality and performance of nanometer heat insulation material;In the present invention In, the molding can for example be carried out using press or the equipment for being capable of providing equivalent pressure.
The method that nanometer heat insulation material is prepared in the present invention uses nanometer heat insulation material material of the present invention for original Expect, each component in the nanometer heat insulation material material can give full play to respective effect, so that nanometer produced by the present invention Heat-barrier material has many advantages, such as that density is small, thermal coefficient is low, mechanical strength is high, excellent combination property, the present invention prepare nanometer every The method of hot material is simple and fast, low to equipment and environmental requirement, is a kind of nanometer heat insulation material preparation method of low cost;This The method parameter easy-regulating for preparing nanometer heat insulation material of invention, can be adjusted according to process requirement.
According to some preferred embodiments, in step (b), the mixture in step (a) is subjected to gradient molding, system Obtain the nanometer heat insulation material;The gradient-norm briquetting includes following sub-step:
S1: the mixture in step (a) is divided into more parts of materials;Such as the mixture can be divided into 3~10 parts of objects Material;
S2: a material in the more parts of materials is laid with (stone) in being molded in mold, obtains nano heat-insulating First layered material of material;
S3: step S2 is repeated on the basis of obtained first layered material to carry out next layer of the nanometer heat insulation material The preparation of material is so constantly repeated up to and reaches predetermined layered material number or predetermined thickness, the nanometer heat insulation material is thus made.
In the present invention, for the mixture is divided into 5 parts of materials, i.e., the described mixture is by first part of material, Two parts of materials, third part material, the 4th part of material and the 5th part of material composition, correspondingly, first part of material carries out after being laid with Molding obtains the first layered material, and second part of material is molded to obtain the second layered material after being laid with, and third part material carries out mould after being laid with Pressure obtains third layered material, and the 4th part of material is molded to obtain the 4th layered material after being laid with, and the 5th part of material is molded after being laid with Obtain layer 5 material;It illustrates, in the present invention, term " first ", " second ", " third ", " the 4th ", " the 5th " etc. It is used for descriptive purposes only and cannot be understood as indicating or suggesting relative importance;For the ordinary skill in the art, Visual concrete condition understands the concrete meaning of above-mentioned term in the present invention.
In the present invention, it is preferred to prepare nanometer heat insulation material using the method for gradient molding (gradually be molded), by by Step suppresses fluffy nanometer heat insulation material material, is further continued for stone after each step compacting, carries out the compacting of next step, gradually press To the material thickness of design, the nanometer heat insulation material of required thickness is prepared.The method of the present invention due to be gradually thin layer compacting, and And matched between each component it is suitable so that the gas in fiber powder hole is easy to be discharged, powder fiber can effective force, this Inventive method, which can effectively solve directly to be molded fluffy nanometer heat insulation material, to be also easy to produce internal flaw with material and works as larger thickness Molding pressure cannot be transmitted effectively downwards and cause to easily cause intralayer defects by fluffy nanometer heat insulation material material in material Problem can effectively improve the structural intergrity of nanometer heat insulation material, be further ensured that the mechanical property of the nanometer heat insulation material Energy.
According to some preferred embodiments, in step s3, next layered material of the nanometer heat insulation material is being carried out Before preparation, pressure maintaining first is carried out to a upper layered material for the nanometer heat insulation material.In the present invention, it is preferred to be molded in each step Pressure maintaining is carried out after (compacting) and carries out pressure maintaining after each process of molding, can be released effectively residual stress, further really It protects nanometer heat insulation material interlayer flawless to generate, guarantees that the nanometer heat insulation material that performance is stable, has excellent performance is made.Certainly, exist In the present invention, when being molded by the way of gradient molding to the mixture, mould can also carried out to every part of material Without pressure maintaining after pressure, pressure maintaining is carried out after the molding of all materials to be done again, plays the role of discharging stress, being finally completed property The preparation for the nanometer heat insulation material can stablize, haveing excellent performance.In the present invention, institute more preferably is carried out after the compacting of each step Pressure maintaining is stated, can so guarantee that the effect of residual stress release is more preferable, the inside of nanometer heat insulation material can preferably be avoided to lack Fall into the generation with intralayer defects.
According to some preferred embodiments, in step s3, next layered material of the nanometer heat insulation material is being carried out Before preparation, loose processing (roughening treatment) first is carried out to the surface layer of a upper layered material for the nanometer heat insulation material;In this hair In bright, such as can be by small tooling target piece by the surface layer material target pine of a upper layered material, so that upper one layer of nanometer heat insulation material Expect that surface layer (surface) is loose.In the present invention, it is preferred to so may be used to carry out the preparation of next layered material after loose again to thin layer surface To be effectively improved the interface of upper a layered material and next layered material, interlayer matching is improved, in this way, obtained receive can be further ensured that Rice heat-barrier material is generated without Interlaminar Crack, further increases the mechanical property of nanometer heat insulation material.
According to some preferred embodiments, in step s3, next layered material of the nanometer heat insulation material is being carried out Before preparation, the loose processing step of pressure holding step and surface layer is successively first carried out to a upper layered material for the nanometer heat insulation material.
According to some preferred embodiments, in step sl, the mixture is divided into and accounts for the total of the mixture The identical more parts of materials of the weight percent of weight.In the present invention, it is preferred to for using the gradient molding of the weight blanking such as this Molding mode is effectively protected it is possible to prevente effectively from unevenly easily causing the non-uniform problem of material each section due to stone The homogeneity for having demonstrate,proved nanometer heat insulation material each section density enables to its thickness direction density variation within 5%, to have Conducive to the quality and performance for guaranteeing nanometer heat insulation material.
According to some preferred embodiments, the method also includes in step (b), by nanometer heat insulation material obtained The step of carrying out pressure maintaining can so play the role of discharging stress, be finally completed the nano heat-insulating that performance is stable, has excellent performance The preparation of material can reduce the internal flaw of nanometer heat insulation material and the generation of intralayer defects.
According to some preferred embodiments, the pressure of the molding be 0.5~20MPa (such as 0.5,1,2,3,4,5, 6,7,8,9,10,11,12,13,14,15,16,17,18,19 or 20MPa), the speed of the molding is 0.1~50mm/s (example Such as 0.1,5,10,15,20,25,30,35,40,45 or 50mm/s), preferably 2~10mm/s (such as 2,3,4,5,6,7,8,9 Or 10mm);The pressure of the pressure maintaining is identical as the pressure of the molding, time of the pressure maintaining be 0.5~60min (such as 0.5,5,8,10,12,15,18,20,22,25,28,30,32,35,38,40,42,45,48,50,52,55,58 or 60min), Preferably 0.5~20min (such as 0.5,1,2,3,4,5,6,7,8,9,10,11,12,13,14,15,16,17,18,19 or 20min).In the present invention, it is carried out by parameters such as the times of the speed of pressure, molding to the molding and pressure maintaining excellent Change, it is ensured that the less nanometer heat insulation material with the less excellent in mechanical performance of intralayer defects of internal flaw is made.
According to some preferred embodiments, the additive is selected from by silicon carbide (carborundum powder), silicon nitride (silicon nitride Powder), titanium dioxide (titanium dioxide powder) and carbon dust composition group.
The present invention provides the nano heat-insulating that the mixed method as the present invention described in first aspect obtains in fourth aspect Nanometer heat insulation material made from method described in material material or third aspect present invention.Nano heat-insulating material produced by the present invention Material has many advantages, such as that density is small, thermal coefficient is low, mechanical strength is high, excellent combination property;Nanometer heat insulation material energy of the invention Be enough in High Mach number aircraft prevents heat-insulated, can also apply in fields such as civilian kiln ladles.
According to some preferred embodiments, the density of the nanometer heat insulation material is 0.10~1.0g/cm3, room temperature leads Hot coefficient is 0.014W/mK~0.045W/mK, and thickness direction tensile strength is 0.3~0.9MPa, and thickness direction compression is strong Degree is 0.5~1.6MPa.In the present invention, nanometer heat insulation material is also denoted as high-performance nano heat-barrier material.
Hereafter the present invention will be further detailed by way of example, but protection scope of the present invention is unlimited In these embodiments.
Embodiment 1
1. quartz fibre is uniformly dispersed with water, slurry is obtained, wherein the mass ratio of quartz fibre and water is 0.5:100; Then finely dispersed slurry is filtered out into tooling dispersing agent, mold quartz fibre and dried, obtain pre-dispersed quartz Fiber.
2. according to silica nanometer powder: pre-dispersed quartz fibre: methylcellulose=500:100:6 (mass ratio) Ratio preparating mixture, for use.
3. mixture is put into mechanical fusion equipment, the revolving speed of mechanical fusion is 1200r/min, the time of mechanical fusion For 60min.
4. taking out uniformly mixed material, nanometer heat insulation material material is obtained, is numbered, for use.
5. according to nanometer heat insulation material material: the ratio preparating mixture of silicon carbide=900:90 (mass ratio) simultaneously uses Mechanical fusion equipment is uniformly mixed, and obtains mixture, and the revolving speed of mechanical fusion is 1200r/min, and the time of mechanical fusion is 20min。
6. being laid with mixture in a mold using scraper plate, mold is put into press after molding, and in molding pressure 3MPa, mould Pressure speed is molded under conditions of being 5mm/s, then carries out pressure maintaining, dwell pressure 3MPa, dwell time 20min, system Obtain nanometer heat insulation material.
The density of the nanometer heat insulation material that the present embodiment obtains material is 0.04g/cm3, room temperature thermal conductivity 0.014W/ m·K;The density of nanometer heat insulation material made from the present embodiment is 0.203g/cm3, room temperature thermal conductivity 0.014W/mK, thickness Direction tensile strength 0.56MPa, thickness direction compressive strength are 0.89MPa.
Embodiment 2
1. alumina fibre is uniformly dispersed with water, slurry is obtained, wherein the mass ratio of alumina fibre and water is 0.5: 100;Then finely dispersed slurry is filtered out into tooling dispersing agent, mold alumina fibre and dried, obtained pre-dispersed Alumina fibre.
2. according to silica nanometer powder: pre-dispersed alumina fibre: methylcellulose=500:120:12 (quality Than) ratio preparating mixture, for use.
3. mixture is put into mechanical fusion equipment, the revolving speed of mechanical fusion is 1000r/min, the time of mechanical fusion For 60min.
4. taking out uniformly mixed material, nanometer heat insulation material material is obtained, is numbered, for use.
5. according to nanometer heat insulation material material: the ratio preparating mixture of silicon carbide=900:90 (mass ratio) simultaneously uses Mechanical fusion equipment is uniformly mixed, and obtains mixture, and the revolving speed of mechanical fusion is 1200r/min, and the time of mechanical fusion is 20min。
6. being laid with mixture in a mold using scraper plate, mold is put into press after molding, and in molding pressure 3MPa, mould Pressure speed is molded under conditions of being 5mm/s, then carries out pressure maintaining, dwell pressure 3MPa, dwell time 20min, system Obtain nanometer heat insulation material.
The density of the nanometer heat insulation material that the present embodiment obtains material is 0.06g/cm3, room temperature thermal conductivity 0.028W/ m·K;The density of nanometer heat insulation material made from the present embodiment is 0.282g/cm3, room temperature thermal conductivity 0.028W/mK, thickness Direction tensile strength 0.65MPa, thickness direction compressive strength are 1.03MPa.
Embodiment 3
1. quartz fibre is uniformly dispersed with water, slurry is obtained, wherein the mass ratio of quartz fibre and water is 0.5:100; Then finely dispersed slurry is filtered out into tooling dispersing agent, mold quartz fibre and dried, obtain pre-dispersed quartz Fiber.
2. according to alumina nano powder: pre-dispersed quartz fibre: the ratio of methylcellulose=500:100:6 (mass ratio) Example preparating mixture, for use.
3. mixture is put into mechanical fusion equipment, the revolving speed of mechanical fusion is 1200r/min, the time of mechanical fusion For 60min.
4. taking out uniformly mixed material, nanometer heat insulation material material is obtained, is numbered, for use.
5. according to nanometer heat insulation material material: the ratio preparating mixture of silicon carbide=900:90 (mass ratio) simultaneously uses Mechanical fusion equipment is uniformly mixed, and obtains mixture, and the revolving speed of mechanical fusion is 1200r/min, and the time of mechanical fusion is 20min。
6. being laid with mixture in a mold using scraper plate, mold is put into press after molding, and in molding pressure 3MPa, mould Pressure speed is molded under conditions of being 5mm/s, then carries out pressure maintaining, dwell pressure 3MPa, dwell time 20min, system Obtain nanometer heat insulation material.
The density of the nanometer heat insulation material that the present embodiment obtains material is 0.08g/cm3, room temperature thermal conductivity 0.035W/ m·K;The density of nanometer heat insulation material made from the present embodiment is 0.32g/cm3, room temperature thermal conductivity 0.035W/mK, thickness side To tensile strength 0.76MPa, thickness direction compressive strength is 1.21MPa.
Embodiment 4
Embodiment 4 is substantially the same manner as Example 1, the difference is that:
In 2., according to silica nanometer powder: pre-dispersed quartz fibre: methylcellulose=500:100:30 (matter Measure ratio) ratio preparating mixture, for use.
The performance indicator such as table 1 for the nanometer heat insulation material material and nanometer heat insulation material obtained that the present embodiment obtains It is shown.
Embodiment 5
Embodiment 5 is substantially the same manner as Example 1, the difference is that:
In 2., according to silica nanometer powder: pre-dispersed quartz fibre: methylcellulose=500:100:40 (matter Measure ratio) ratio preparating mixture, for use.
The performance indicator such as table 1 for the nanometer heat insulation material material and nanometer heat insulation material obtained that the present embodiment obtains It is shown.
Embodiment 6
Embodiment 6 is substantially the same manner as Example 1, the difference is that:
In 2., according to silica nanometer powder: pre-dispersed quartz fibre: methylcellulose=500:100:2 (quality Than) ratio preparating mixture, for use.
The performance indicator such as table 1 for the nanometer heat insulation material material and nanometer heat insulation material obtained that the present embodiment obtains It is shown.
Embodiment 7
Embodiment 7 is substantially the same manner as Example 1, the difference is that:
In 2., according to silica nanometer powder: pre-dispersed quartz fibre: neopelex=500:100: The ratio preparating mixture of 6 (mass ratioes), for use.
The performance indicator such as table 1 for the nanometer heat insulation material material and nanometer heat insulation material obtained that the present embodiment obtains It is shown.
Embodiment 8
Embodiment 8 is substantially the same manner as Example 1, the difference is that:
In 2., according to silica nanometer powder: pre-dispersed quartz fibre: polyethylene glycol oxide=500:100:6 (quality Than) ratio preparating mixture, for use.
The performance indicator such as table 1 for the nanometer heat insulation material material and nanometer heat insulation material obtained that the present embodiment obtains It is shown.
Embodiment 9
Embodiment 9 is substantially the same manner as Example 1, the difference is that:
In 1., quartz fibre is uniformly dispersed with water, obtains slurry, wherein the mass ratio of quartz fibre and water is 1: 100;Then finely dispersed slurry is filtered out into tooling dispersing agent, mold quartz fibre and dried, obtained pre-dispersed Quartz fibre.
The performance indicator such as table 1 for the nanometer heat insulation material material and nanometer heat insulation material obtained that the present embodiment obtains It is shown.
Embodiment 10
Embodiment 10 is substantially the same manner as Example 1, the difference is that:
In 1., quartz fibre is uniformly dispersed with water, obtains slurry, wherein the mass ratio of quartz fibre and water is 1.2: 100;Then finely dispersed slurry is filtered out into tooling dispersing agent, mold quartz fibre and dried, obtained pre-dispersed Quartz fibre.
The performance indicator such as table 1 for the nanometer heat insulation material material and nanometer heat insulation material obtained that the present embodiment obtains It is shown.
Embodiment 11
Embodiment 11 is substantially the same manner as Example 1, the difference is that: step is 5. and 6. different, and further includes step ⑦。
In 5., according to nanometer heat insulation material material: the ratio preparating mixture of silicon carbide=900:90 (mass ratio) It is uniformly mixed using mechanical fusion equipment, obtains mixture, the revolving speed of mechanical fusion is 1200r/min, the time of mechanical fusion For 20min;The identical five parts of materials of the weight percent that the mixture is divided into the total weight for accounting for the mixture, it is described Five parts of materials by be by weight percentage 20% first part of material, 20% second part of material, 20% third part material, 20% the 4th part of material and 20% the 5th part of material composition.
In 6., it is laid with first part of material in a mold using scraper plate, mold is put into press after molding, and press in molding Power 3MPa, molding speed are molded under conditions of being 5mm/s, then carry out pressure maintaining, dwell pressure 3MPa, the dwell time is 5min obtains the first layered material.
7. repeating step the first layered material of gained on the basis of 6. to carry out next layered material of the nanometer heat insulation material Preparation, is so constantly repeated up to and reaches predetermined layered material number or predetermined thickness;In the next layer for carrying out the nanometer heat insulation material Before the preparation of material, pressure releasing die sinking first carries out loose processing to the surface layer of a upper layered material for the nanometer heat insulation material;Mold is let out After pressure, the nanometer heat insulation material suppressed is taken out in demoulding.
The performance indicator such as table 1 for the nanometer heat insulation material material and nanometer heat insulation material obtained that the present embodiment obtains It is shown.
Embodiment 12
Embodiment 12 is substantially the same manner as Example 11, the difference is that: 6. and 7. in, every part of material is molded Afterwards without pressure maintaining, after the molding of all mixtures to be done, uniformly progress pressure maintaining, dwell pressure 3MPa, dwell time are Nanometer heat insulation material is made in 20min.
The performance indicator such as table 1 for the nanometer heat insulation material material and nanometer heat insulation material obtained that the present embodiment obtains It is shown.
Embodiment 13
Embodiment 13 is substantially the same manner as Example 11, the difference is that:
In 7., before carrying out the preparation of next layered material of the nanometer heat insulation material, not to the nano heat-insulating material The surface layer of a upper layered material for material carries out loose processing.
The performance indicator such as table 1 for the nanometer heat insulation material material and nanometer heat insulation material obtained that the present embodiment obtains It is shown.
Embodiment 14
Embodiment 14 is substantially the same manner as Example 11, the difference is that:
In 5., the mixture is divided into three parts of materials, three parts of materials are by being by weight percentage 50% First part of material, 30% second part of material and 20% third part material.
The mode that above-mentioned three parts of materials successively decrease by weight percentage is successively subjected to 6. and 7. step.
The performance indicator such as table 1 for the nanometer heat insulation material material and nanometer heat insulation material obtained that the present embodiment obtains It is shown.
Comparative example 1
1. taking fumed silica 70wt%, silicon carbide 25wt%, the superfine E-glass fibre glass fibre that length is 5mm Superfine E-glass fibre glass fibre is added in high speed disperser and carries out pre-dispersed, speed of agitator 600r/min by 5wt%, and the time is Machinery is added in the superfine E-glass fibre glass fibre, fumed silica powder body material and silicon carbide of pre-dispersed mistake by 1min together In fusion device, with 1200r/min revolving speed mixing 30min.
2. utilizing steaming and cultivating equipment, the material of mixing and water vapour are come into full contact with into 30min at 80 DEG C, at steaming and cultivating equipment In the material merging mold managed, with hydraulic press with the final pressure compression moulding of the rate of pressurization of 1N/s and 2MPa.
It is dried 3. finally molding block materials are put into drying box, can be prepared by height through 110 DEG C of heat treatment 6h The super composite heat-insulated material of performance nano grade silica particles base.
The performance of composite heat-insulated material made from uniformly mixed material and this comparative example in this comparative example is carried out Test, the results are shown in Table 1.
Comparative example 2
Comparative example 2 is substantially the same manner as Example 1, the difference is that:
In 1., quartz fibre is added in high speed disperser and carries out pre-dispersed, speed of agitator 600r/min, the time is 1min is uniformly dispersed, and obtains pre-dispersed quartz fibre.
In 2., according to silica nanometer powder: the ratio of pre-dispersed quartz fibre=500:100 (mass ratio) is prepared Mixture, for use.
The performance indicator such as table 1 for the nanometer heat insulation material material and nanometer heat insulation material obtained that this comparative example obtains It is shown.
Comparative example 3
Comparative example 3 is substantially the same manner as Example 1, the difference is that:
In 2., according to silica nanometer powder: the ratio of pre-dispersed quartz fibre=500:100 (mass ratio) is prepared Mixture, for use.
The performance indicator such as table 1 for the nanometer heat insulation material material and nanometer heat insulation material obtained that this comparative example obtains It is shown.
Comparative example 4
Comparative example 4 is substantially the same manner as Example 1, the difference is that:
In 1., quartz fibre is added in high speed disperser and carries out pre-dispersed, speed of agitator 600r/min, the time is 1min is uniformly dispersed, and obtains pre-dispersed quartz fibre.
The performance indicator such as table 1 for the nanometer heat insulation material material and nanometer heat insulation material obtained that this comparative example obtains It is shown.
Finally, it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations;Although Present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that: it still may be used To modify the technical solutions described in the foregoing embodiments or equivalent replacement of some of the technical features; And these are modified or replaceed, technical solution of various embodiments of the present invention that it does not separate the essence of the corresponding technical solution spirit and Range.

Claims (10)

1. a kind of mixed method of nanometer heat insulation material material, which is characterized in that described method includes following steps:
(1) ceramic fibre is uniformly dispersed with water, obtains slurry, then dry the slurry, it is fine to obtain pre-dispersed ceramics Dimension;
(2) by nano-powder, pre-dispersed ceramic fibre and selected from by neopelex, methylcellulose, carboxymethyl The dispersion aids of the group of cellulose, hydroxyethyl cellulose and polyethylene glycol oxide composition carries out mechanical fusion, obtains uniformly mixed Nanometer heat insulation material material.
2. mixed method according to claim 1, it is characterised in that:
The nanometer heat insulation material material by be by weight percentage 55~85% nano-powder, pre- point of 14~40% Scattered ceramic fibre and 0.5~5% dispersion aids composition;And/or
In step (1), the dosage of the ceramic fibre is 0.5~1wt% of the dosage of the water.
3. mixed method according to claim 1, it is characterised in that:
The revolving speed of the mechanical fusion is 300~1600r/min, and the time of the mechanical fusion is 1~3600min.
4. mixed method according to any one of claims 1 to 3, it is characterised in that:
The nano-powder is selected from by silica nano-powder, nanometer alumina powder, nm-class powder of zirconium oxide, nanometer silicon carbide The group of powder and Nano-silicon Nitride Powder composition;And/or
The ceramic fibre is selected from by quartz fibre, high silica fiber, glass fibre, mullite fiber, basalt cotton fiber, oxygen Change the group of aluminum fiber and Zirconium oxide fibre composition.
5. mixed method according to any one of claims 1 to 3, it is characterised in that:
The partial size of the nano-powder is 0.1~1000nm;And/or
The diameter of the ceramic fibre is 0.1~50um, and the length of the ceramic fibre is 0.1~50mm.
6. the nanometer heat insulation material material obtained by mixed method described in any one of claim 1 to 5.
7. preparing nano heat-insulating with material by the nanometer heat insulation material that mixed method described in any one of claim 1 to 5 obtains The method of material, described method includes following steps:
(a) it will be mixed by weight percentage for 85~100% nanometer heat insulation material material and 0~15% additive equal It is even, obtain mixture;
(b) mixture in step (a) is molded, nanometer heat insulation material is made.
8. the method according to the description of claim 7 is characterized in that being received the method also includes in step (b) by obtained The step of rice heat-barrier material carries out pressure maintaining.
9. method according to claim 7 or 8, it is characterised in that:
The pressure of the molding is 0.5~20MPa, and the speed of the molding is 0.1~50mm/s;
The pressure of the pressure maintaining is identical as the pressure of the molding, and the time of the pressure maintaining is 0.5~60min;And/or
The additive is selected from the group being made of silicon carbide, silicon nitride, titanium dioxide and carbon dust.
10. nanometer heat insulation material material or claim that the mixed method as described in any one of claims 1 to 5 obtains Nanometer heat insulation material made from method described in any one of 7 to 9.
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CN113895103A (en) * 2021-10-09 2022-01-07 航天特种材料及工艺技术研究所 High-toughness nano heat-insulating material and preparation method thereof
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