CN116986910A - Method for preparing aluminum nitride ceramic by using adhesive injection molding technology - Google Patents
Method for preparing aluminum nitride ceramic by using adhesive injection molding technology Download PDFInfo
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- CN116986910A CN116986910A CN202311012509.3A CN202311012509A CN116986910A CN 116986910 A CN116986910 A CN 116986910A CN 202311012509 A CN202311012509 A CN 202311012509A CN 116986910 A CN116986910 A CN 116986910A
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- Prior art keywords
- aluminum nitride
- blank
- injection molding
- powder
- adhesive injection
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- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 title claims abstract description 99
- 239000000919 ceramic Substances 0.000 title claims abstract description 69
- 239000000853 adhesive Substances 0.000 title claims abstract description 51
- 230000001070 adhesive effect Effects 0.000 title claims abstract description 51
- 238000000034 method Methods 0.000 title claims abstract description 39
- 238000001746 injection moulding Methods 0.000 title claims abstract description 25
- 238000005516 engineering process Methods 0.000 title claims abstract description 23
- 239000000843 powder Substances 0.000 claims abstract description 85
- 238000005245 sintering Methods 0.000 claims abstract description 42
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 claims abstract description 20
- 238000007639 printing Methods 0.000 claims abstract description 20
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 14
- 238000001513 hot isostatic pressing Methods 0.000 claims abstract description 13
- 229910021645 metal ion Inorganic materials 0.000 claims abstract description 10
- 230000002209 hydrophobic effect Effects 0.000 claims abstract description 7
- 238000004519 manufacturing process Methods 0.000 claims abstract description 6
- 238000002347 injection Methods 0.000 claims abstract description 3
- 239000007924 injection Substances 0.000 claims abstract description 3
- 239000003292 glue Substances 0.000 claims description 48
- 238000007599 discharging Methods 0.000 claims description 39
- 239000012298 atmosphere Substances 0.000 claims description 22
- 239000000243 solution Substances 0.000 claims description 21
- 238000001035 drying Methods 0.000 claims description 19
- 238000010438 heat treatment Methods 0.000 claims description 19
- 229910052751 metal Inorganic materials 0.000 claims description 17
- 239000002184 metal Substances 0.000 claims description 17
- 239000002243 precursor Substances 0.000 claims description 16
- 238000001816 cooling Methods 0.000 claims description 14
- 239000002904 solvent Substances 0.000 claims description 14
- 238000000498 ball milling Methods 0.000 claims description 12
- 238000007873 sieving Methods 0.000 claims description 11
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 10
- 239000002245 particle Substances 0.000 claims description 9
- 208000028659 discharge Diseases 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 6
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 6
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- 230000001681 protective effect Effects 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 5
- 238000009826 distribution Methods 0.000 claims description 5
- 235000021355 Stearic acid Nutrition 0.000 claims description 3
- 230000009471 action Effects 0.000 claims description 3
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 3
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 3
- 239000008117 stearic acid Substances 0.000 claims description 3
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 2
- 239000011230 binding agent Substances 0.000 claims 2
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 claims 1
- 238000002360 preparation method Methods 0.000 abstract description 13
- 238000005507 spraying Methods 0.000 abstract description 11
- 230000008569 process Effects 0.000 abstract description 10
- 230000008595 infiltration Effects 0.000 abstract description 9
- 238000001764 infiltration Methods 0.000 abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 9
- 230000007062 hydrolysis Effects 0.000 abstract description 5
- 238000006460 hydrolysis reaction Methods 0.000 abstract description 5
- 238000006243 chemical reaction Methods 0.000 abstract description 3
- 239000000654 additive Substances 0.000 abstract description 2
- 230000000996 additive effect Effects 0.000 abstract description 2
- 238000005238 degreasing Methods 0.000 abstract description 2
- 230000035939 shock Effects 0.000 abstract description 2
- 230000009286 beneficial effect Effects 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 14
- 239000002002 slurry Substances 0.000 description 8
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 7
- 229910017083 AlN Inorganic materials 0.000 description 6
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 description 6
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 230000004048 modification Effects 0.000 description 6
- 238000012986 modification Methods 0.000 description 6
- VZJJZMXEQNFTLL-UHFFFAOYSA-N chloro hypochlorite;zirconium;octahydrate Chemical compound O.O.O.O.O.O.O.O.[Zr].ClOCl VZJJZMXEQNFTLL-UHFFFAOYSA-N 0.000 description 5
- 239000004890 Hydrophobing Agent Substances 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- 235000019441 ethanol Nutrition 0.000 description 4
- 239000010410 layer Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 238000010146 3D printing Methods 0.000 description 2
- NGDQQLAVJWUYSF-UHFFFAOYSA-N 4-methyl-2-phenyl-1,3-thiazole-5-sulfonyl chloride Chemical compound S1C(S(Cl)(=O)=O)=C(C)N=C1C1=CC=CC=C1 NGDQQLAVJWUYSF-UHFFFAOYSA-N 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 230000008707 rearrangement Effects 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 238000009718 spray deposition Methods 0.000 description 2
- -1 zirconium ions Chemical class 0.000 description 2
- 229910018509 Al—N Inorganic materials 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 229910052602 gypsum Inorganic materials 0.000 description 1
- 239000010440 gypsum Substances 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910001425 magnesium ion Inorganic materials 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000005022 packaging material Substances 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000004834 spray adhesive Substances 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- 229910052984 zinc sulfide Inorganic materials 0.000 description 1
- 229910052726 zirconium Inorganic materials 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
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
- C04B35/581—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on aluminium nitride
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y10/00—Processes of additive manufacturing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y70/00—Materials specially adapted for additive manufacturing
- B33Y70/10—Composites of different types of material, e.g. mixtures of ceramics and polymers or mixtures of metals and biomaterials
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Abstract
The invention discloses a method for preparing aluminum nitride ceramics by using an adhesive injection molding technology, and relates to the technical field of adhesive injection additive manufacturing. The preparation method of the invention adopts submicron aluminum nitride powder for preparation, and sequentially uses polyvinyl butyral and a hydrophobic agent to modify the powder, thereby solving the problem of hydrolysis of the adhesive caused by the reaction of the aluminum nitride powder and the water-based adhesive, and successfully printing an aluminum nitride ceramic blank by using the adhesive spraying technology. In addition, the invention adopts an infiltration process to infiltrate the blank into metal ions after degreasing the blank so as to improve the density of the blank and successfully introduce the second phase, thereby being beneficial to preparing AlN ceramics with high density, fine grains and uniform microstructure and improving the mechanical property and the thermal shock resistance of the AlN ceramics. The method of the invention further comprises the step of carrying out hot isostatic pressing treatment on the sintered body obtained by sintering, thereby further improving the strength and hardness of the aluminum nitride ceramic and finally obtaining the aluminum nitride ceramic with high performance.
Description
Technical Field
The invention relates to the technical field of adhesive spray additive manufacturing, in particular to a method for preparing aluminum nitride ceramics by using an adhesive spray forming technology.
Background
The aluminium nitride crystal is made of AIN 4 The covalent bond compound with tetrahedron as structural unit has wurtzite structure, belongs to hexagonal system, and is the only stable compound in binary Al-N system, and has theoretical density of about 3.26g/cm 3 。
The aluminum nitride ceramic has excellent mechanical property (the hardness is 12GPa at normal temperature, the bending strength can reach 400 MPa), chemical property (high temperature resistance and corrosion resistance, no need to consider oxidation at normal temperature), heat conductivity (the theoretical value of heat conductivity is about 320 W.m) -1 ·K -1 ) Extremely high insulation (volume resistivity > 1012 Ω & m), extremely low dielectric constant (about 8 at 1 MHz) and dielectric loss, non-toxicity and silicon-matched coefficient of thermal expansion (293-773 k, 4.8X10) -6 K -1 ) And the like, are considered as heat dissipation materials and packaging materials for new generation of ideal large-scale integrated circuits, semiconductor module circuits and high-power devices.
The adhesive spraying technology (BJ) is also called Three-dimensional printing (Three-Dimensional Printing,3 DP), and the principle is that the nozzle is controlled to automatically spray adhesive above the powder plane paved on the two-dimensional plane to selectively bond the powder particles together to form a single layer, then the z-axis is controlled to sink, then the material is paved again, the adhesive is sprayed again, and the process is repeatedly circulated, so that the Three-dimensional blank body can be obtained. The application range of the adhesive spraying technology is wider, the material selection is wide (gypsum powder, starch, sand, ceramic powder, metal powder, composite material powder, graphene and the like), the processing speed is high, the equipment has lower manufacturing cost and running cost, the production process is not limited by factors such as the shape and structure of the part, and the manufacturing of various parts with complex shapes can be completed. However, the green body formed by the method has poor precision and rough surface, and the prepared part has low density and low performance.
However, there is no prior art about the preparation of aluminum nitride ceramics by injection molding of adhesives.
Disclosure of Invention
The invention aims to solve the technical problem of how to prepare aluminum nitride ceramics by adopting an adhesive injection molding technology.
In order to solve the problems, the invention provides the following technical scheme:
in a first aspect, the present invention provides a method for preparing aluminum nitride ceramics by using an adhesive injection molding technology, comprising the following steps:
s1, mixing 85-90 parts of aluminum nitride powder and 1-5 parts of polyvinyl butyral uniformly at 80-100 ℃ under the action of a solvent according to parts by weight, and then filtering, washing and drying to obtain modified aluminum nitride powder;
s2, ball-milling and uniformly mixing the modified aluminum nitride powder, 1-5 parts of the hydrophobizing agent and 1-10 parts of the sintering aid, drying, and sieving with a 150-200 mesh sieve to obtain printing powder;
s3, feeding the powder obtained in the step S2 into adhesive injection molding equipment, and performing adhesive injection molding to obtain a blank;
s4, solidifying the blank body and performing vacuum glue discharge or atmosphere protection glue discharge-air glue discharge two-step glue discharge treatment;
s5, completely immersing the gel-discharged blank body in a metal precursor solution for 2-4 hours at room temperature, immersing in an ammonia solution for 5-15 minutes, taking out, and drying for 12-48 hours;
and S6, placing the green body dried in the S5 in an atmosphere sintering furnace for sintering to obtain a sintered body, and performing hot isostatic pressing treatment on the sintered body to obtain the aluminum nitride ceramic.
The solvent in step S1 may be one or more selected from n-butanol, absolute ethanol, and isopropanol. Under the action of a solvent, the aluminum nitride powder and the polyvinyl butyral are fully and uniformly mixed by being assisted by water bath heating, so that the modified aluminum nitride powder is obtained. In the step S2, when the raw materials are ball-milled, solvent auxiliary can be added, a planetary ball mill is adopted to ball mill for 10 to 12 hours at the rotating speed of 200 to 300rpm, and after the ball milling is finished, the solvent is removed by drying.
Before printing, the invention firstly modifies the aluminum nitride powder by polyvinyl butyral in the step S1, and then adds a hydrophobic agent to carry out hydrophobic modification on all the powder in the step S2, so that the saturation of the powder to glue during printing can be effectively reduced, the problem of adhesive hydrolysis caused by the reaction of the aluminum nitride powder and a water-based adhesive is solved, and the reduction of the performance of the aluminum nitride ceramic obtained after sintering caused by the adhesive hydrolysis before sintering is prevented.
In the step S1, the grain diameter of the aluminum nitride powder is submicron, and the grain diameter distribution is 0.2-1 mu m.
The aluminum nitride powder particle size selected in the invention is submicron, which is because: firstly, compared with nano-scale aluminum nitride fine powder, submicron-scale powder has better fluidity, can ensure the powder paving quality in the printing process, and avoids a series of quality problems such as cracks, air holes, burrs and the like caused by uneven powder paving; secondly, the particle size of the raw material powder is kept large enough, and enough gaps are reserved among the particles to enable the adhesive to enter, so that printing is facilitated; finally, on the premise of ensuring successful printing, compared with aluminum nitride powder with larger particle size, the submicron aluminum nitride powder selected by the invention has the advantages that the ceramic piece obtained after sintering is more compact, and the good performance of the ceramic piece can be ensured.
The further technical scheme is that the hydrophobic agent is one or more of phosphoric acid, silane coupling agents KH550, DP270 and stearic acid.
The sintering aid is yttrium oxide.
The further technical proposal is that the metal ion in the metal precursor solution is Zr 4+ ，Y 3+ ，Mg 2+ At least one of them.
The metal precursor solution is prepared by dissolving at least one of zirconium oxychloride octahydrate, yttrium nitrate and magnesium nitrate in absolute ethyl alcohol.
The further technical proposal is that the concentration of metal ions in the metal precursor solution is 0.1 to 0.3mol/L.
The method is characterized in that the blank body is degreased and then infiltrated with metal ions by adopting an infiltration process, so that the density of the blank body is improved, a second phase is successfully introduced into the blank body, rearrangement, dissolution-precipitation and grain growth of aluminum nitride ceramic particles are promoted by infiltration of the metal ions, the preparation of AlN ceramic with high density, fine grains and uniform microstructure is facilitated, and the mechanical property and the thermal shock resistance of the AlN ceramic are improved.
In the further technical scheme, in the step S3, the thickness of the adhesive jet printing layer is 100-150 mu m.
The technical scheme is that the vacuum glue discharging method comprises the following specific operations: placing the blank in a vacuum glue discharging furnace with the pressure of-0.1 MPa, heating to 600-1200 ℃ at the speed of 5-10 ℃/min, preserving the temperature for 4-8 hours, and then cooling the blank to the room temperature along with the furnace;
the specific operation of the atmosphere protection glue discharging is as follows: placing the blank in Ar and/or N 2 And heating the blank to 600-1200 ℃ at a speed of 5-10 ℃/min in a protected glue discharging furnace, preserving heat for 4-8h, and cooling the blank to room temperature along with the furnace.
The technical scheme is that the concrete operation of the air glue discharging is as follows: placing the blank body in a glue discharging furnace in air atmosphere, heating to 800-1000 ℃ at the speed of 5-10 ℃/min, preserving heat for 2-8h, and then cooling the blank body to room temperature along with the furnace.
The further technical scheme is that in the step S6, sintering conditions are as follows: at N 2 The flow is 0.3-0.8L/min, and the temperature is kept for 6-12 h at 1700-1900 ℃; specific operation of the HIP is, in N 2 Or Ar protective atmosphere, carrying out hot isostatic pressing treatment on the sintered body for 1-2 h at 1350-1500 ℃ and 100-180 MPa.
After the green body is sintered, the green body is naturally cooled to room temperature to obtain a sintered body, and then the sintered body is sinteredThe body was subjected to hot isostatic pressing. The temperature of the hot isostatic pressing treatment is 200-400 ℃ lower than the sintering temperature, so that abnormal growth of crystal grains in the sintered body can be prevented, and the compactness, strength and hardness of the ceramic sintered body can be improved. For a ceramic sample containing zirconium ions, yttrium ions and magnesium ions in the infiltrated metal precursor solution, by XRD phase analysis, the sample contains AlN, YAP, YAG, YAM, a small amount of MgO and a small amount of ZrO 2 。
In a second aspect, the present invention provides an aluminum nitride ceramic prepared by the preparation method of the first aspect.
Compared with the prior art, the invention has the following technical effects:
the method for preparing the aluminum nitride ceramic by the adhesive spray forming technology provided by the invention adopts submicron aluminum nitride powder for preparation, and sequentially adopts polyvinyl butyral and a hydrophobic agent for modifying the powder, so that the problem of adhesive hydrolysis caused by the reaction of the aluminum nitride powder and a water-based adhesive is solved, and an aluminum nitride ceramic blank is successfully printed by using the adhesive spray technology.
Further, the invention adopts an infiltration process to infiltrate the green body into metal ions after degreasing the green body so as to improve the density of the green body and successfully introduce a second phase, promote rearrangement, dissolution-precipitation and grain growth of particles, and facilitate preparation of AlN ceramics with high density, fine grains and uniform microstructure and improve the mechanical property of the AlN ceramics.
Finally, in the preparation method, the sintered body obtained by sintering is subjected to hot isostatic pressing, so that the strength and hardness of the aluminum nitride ceramic are further improved, and finally the aluminum nitride ceramic with high performance, which can be prepared by adopting an adhesive injection molding technology, is obtained.
Detailed Description
The technical solutions in the embodiments will be clearly and completely described below. It will be apparent that the embodiments described below are only some, but not all, embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
It should be understood that the terms "comprises" and "comprising," when used in this specification and the appended claims, specify the presence of stated features, integers, steps, operations, but do not preclude the presence or addition of one or more other features, integers, steps, operations, and/or groups thereof.
It is also to be understood that the terminology used in the description of the embodiments of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of embodiments of the invention. As used in the specification of the embodiments of the invention and the appended claims, the singular forms "a," "an," and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise.
Example 1
The embodiment provides a method for preparing aluminum nitride ceramics by using an adhesive injection molding technology, which comprises the following specific steps:
respectively weighing 900g of aluminum nitride powder, 20g of polyvinyl butyral, 40g of yttrium oxide (sintering aid) and 40g of phosphoric acid (hydrophobizing agent); the grain diameter of the aluminum nitride powder is submicron, and the grain diameter distribution is 0.2-1 mu m.
(1) Powder modification:
firstly heating aluminum nitride powder, polyvinyl butyral and a solvent in a water bath, stirring for 60min, fully and uniformly mixing the aluminum nitride powder and the polyvinyl butyral, and then filtering, washing and drying the powder to obtain the modified aluminum nitride powder.
(2) Ball milling and sieving:
ball-milling the modified aluminum nitride powder, the sintering aid, the hydrophobing agent and the solvent on a planetary ball mill for 12 hours at the rotating speed of 300rpm to obtain ceramic slurry, putting the ceramic slurry into an oven for drying, and then sieving with a 100-mesh screen to obtain the printing powder.
(3) And (3) forming:
the powder is sent into adhesive spraying equipment, and the adhesive spraying printing and forming are carried out to obtain a green body, wherein the thickness of the green body is 150 mu m.
(4) And (3) glue discharging:
and further solidifying the blank body and performing two-step glue discharging treatment of vacuum glue discharging and air glue discharging.
Specifically, firstly placing the blank in a negative pressure glue discharging furnace (the vacuum degree is more than or equal to 0.09 MPa), heating to 800 ℃ at the speed of 5 ℃/min, preserving heat for 8 hours, and cooling to room temperature along with the furnace;
and then placing the blank body in a glue discharging furnace in an air atmosphere, heating to 800 ℃ at a speed of 10 ℃/min, preserving heat for 6 hours, and then cooling the blank body to room temperature along with the furnace.
(5) Infiltration:
and (3) completely immersing the gel-removed green body in a metal precursor solution for 4 hours at room temperature, immersing the green body in an ammonia solution for 10 minutes, taking out, and drying in an oven for 24 hours.
The metal precursor solution of this example was an ethanol solution of zirconium oxychloride octahydrate, and the mass concentration of the substance was 0.3mol/L.
(6) Sintering:
sintering the dried blank in an atmosphere sintering furnace at 1850 ℃ and N 2 The flow rate is 0.5L/min, the temperature is kept for 6 hours, and then the mixture is cooled to room temperature along with a furnace, so as to obtain a sintered body. Sintered body is N 2 And (3) carrying out hot isostatic pressing treatment for 2 hours at the temperature of 1600 ℃ and the pressure of 180MPa in a protective atmosphere to obtain the aluminum nitride ceramic.
The aluminum nitride ceramic prepared by the method of this example had a relative density of 65%, a Vickers hardness of 14.3GPa, and a thermal conductivity of 130W/(mK).
Example 2
The embodiment provides a method for preparing aluminum nitride ceramics by using an adhesive injection molding technology, which comprises the following specific steps:
separately, 850g of aluminum nitride powder, 40g of polyvinyl butyral, 70g of yttrium oxide (sintering aid) and 40g of phosphoric acid (hydrophobizing agent) were weighed.
(1) Powder modification:
firstly heating aluminum nitride powder, polyvinyl butyral and a solvent in a water bath, stirring for 60min, fully and uniformly mixing the aluminum nitride powder and the polyvinyl butyral, and then filtering, washing and drying the powder to obtain the modified aluminum nitride powder.
(2) Ball milling and sieving:
ball-milling the modified aluminum nitride powder, the sintering aid, the hydrophobing agent and the solvent on a planetary ball mill for 10 hours at the rotating speed of 300rpm to obtain ceramic slurry, putting the ceramic slurry into an oven for drying, and then sieving with a 150-mesh screen to obtain the printing powder.
(3) And (3) forming:
the powder is sent into adhesive spraying equipment, and the adhesive spraying printing and forming are carried out to obtain a green body, wherein the thickness of the green body is 150 mu m.
(4) And (3) glue discharging:
and further solidifying the blank body and performing two-step glue discharging treatment of vacuum glue discharging and air glue discharging.
Specifically, firstly placing the blank in a negative pressure glue discharging furnace (the vacuum degree is more than or equal to 0.09 MPa), heating to 1000 ℃ at the speed of 10 ℃/min, preserving heat for 4 hours, and cooling to room temperature along with the furnace;
and then placing the blank body in a glue discharging furnace in an air atmosphere, heating to 800 ℃ at a speed of 10 ℃/min, preserving heat for 6 hours, and then cooling the blank body to room temperature along with the furnace.
(5) Infiltration:
and (3) completely immersing the gel-removed green body in a metal precursor solution for 4 hours at room temperature, immersing the green body in an ammonia solution for 10 minutes, taking out, and drying in an oven for 24 hours.
The metal precursor solution of this example was an ethanol solution of zirconium oxychloride octahydrate, and the mass concentration of the substance was 0.3mol/L.
(6) Sintering:
sintering the dried blank in an atmosphere sintering furnace at 1850 ℃ and N 2 The flow rate is 0.5L/min, the temperature is kept for 6 hours, and then the mixture is cooled to room temperature along with a furnace, so as to obtain a sintered body. Sintered body is N 2 And (3) carrying out hot isostatic pressing treatment for 2 hours at the temperature of 1500 ℃ and the pressure of 180MPa in a protective atmosphere to obtain the aluminum nitride ceramic.
The aluminum nitride ceramic prepared by the method of this example had a relative density of 63%, a Vickers hardness of 12.7GPa, and a thermal conductivity of 135W/(mK).
Example 3
The embodiment provides a method for preparing aluminum nitride ceramics by using an adhesive injection molding technology, which comprises the following specific steps:
respectively weighing 900g of aluminum nitride powder, 20g of polyvinyl butyral, 40g of yttrium oxide (sintering aid) and 40g of KH550 (hydrophobizing agent); the grain diameter of the aluminum nitride powder is submicron, and the grain diameter distribution is 0.2-1 mu m.
(1) Powder modification:
firstly heating aluminum nitride powder, polyvinyl butyral and a solvent in a water bath, stirring for 60min, fully and uniformly mixing the aluminum nitride powder and the polyvinyl butyral, and then filtering, washing and drying the powder to obtain the modified aluminum nitride powder.
(2) Ball milling and sieving:
ball-milling the modified aluminum nitride powder, the sintering aid, the hydrophobing agent and the solvent on a planetary ball mill for 12 hours at the rotating speed of 300rpm to obtain ceramic slurry, putting the ceramic slurry into an oven for drying, and then sieving with a 100-mesh screen to obtain the printing powder.
(3) And (3) forming:
the powder is sent into adhesive spraying equipment, and the adhesive spraying printing and forming are carried out to obtain a green body, wherein the thickness of the green body is 120 mu m.
(4) And (3) glue discharging:
and further solidifying the blank body and performing two-step glue discharging treatment of vacuum glue discharging and air glue discharging.
Specifically, firstly placing the blank in a negative pressure glue discharging furnace (the vacuum degree is more than or equal to 0.09 MPa), heating to 800 ℃ at the speed of 5 ℃/min, preserving heat for 8 hours, and cooling to room temperature along with the furnace;
and then placing the blank body in a glue discharging furnace in an air atmosphere, heating to 800 ℃ at a speed of 10 ℃/min, preserving heat for 6 hours, and then cooling the blank body to room temperature along with the furnace.
(5) Infiltration:
and (3) completely immersing the gel-removed green body in a metal precursor solution for 4 hours at room temperature, immersing the green body in an ammonia solution for 10 minutes, taking out, and drying in an oven for 24 hours.
The metal precursor solution of this example was an ethanol solution of zirconium oxychloride octahydrate and magnesium nitrate, and the mass concentration of the metal ion was 0.3mol/L.
(6) Sintering:
sintering the dried blank in an atmosphere sintering furnace at 1850 ℃ and N 2 The flow rate is 0.5L/min, the temperature is kept for 6 hours, and then the mixture is cooled to room temperature along with a furnace, so as to obtain a sintered body. Sintered body is N 2 And (3) carrying out hot isostatic pressing treatment for 2 hours at the temperature of 1600 ℃ and the pressure of 180MPa in a protective atmosphere to obtain the aluminum nitride ceramic.
The aluminum nitride ceramic prepared by the method of this example had a relative density of 66.7%, a Vickers hardness of 15.2GPa, and a thermal conductivity of 128W/(mK).
Example 4
The embodiment provides a method for preparing aluminum nitride ceramics by using an adhesive injection molding technology, which comprises the following specific steps:
respectively weighing 900g of aluminum nitride powder, 20g of polyvinyl butyral, 40g of yttrium oxide (sintering aid) and 40g of stearic acid (hydrophobizing agent); the grain diameter of the aluminum nitride powder is submicron, and the grain diameter distribution is 0.2-1 mu m.
(1) Powder modification:
firstly heating aluminum nitride powder, polyvinyl butyral and a solvent in a water bath, stirring for 60min, fully and uniformly mixing the aluminum nitride powder and the polyvinyl butyral, and then filtering, washing and drying the powder to obtain the modified aluminum nitride powder.
(2) Ball milling and sieving:
ball-milling the modified aluminum nitride powder, the sintering aid, the hydrophobing agent and the solvent on a planetary ball mill for 12 hours at the rotating speed of 300rpm to obtain ceramic slurry, putting the ceramic slurry into an oven for drying, and then sieving with a 100-mesh screen to obtain the printing powder.
(3) And (3) forming:
the powder is sent into adhesive spraying equipment, and the adhesive spraying printing and forming are carried out to obtain a green body, wherein the thickness of the green body is 150 mu m.
(4) And (3) glue discharging:
and further solidifying the blank body and performing two-step glue discharging treatment of vacuum glue discharging and air glue discharging.
Specifically, firstly placing the blank in a negative pressure glue discharging furnace (the vacuum degree is more than or equal to 0.09 MPa), heating to 800 ℃ at the speed of 5 ℃/min, preserving heat for 8 hours, and cooling to room temperature along with the furnace;
and then placing the blank body in a glue discharging furnace in an air atmosphere, heating to 800 ℃ at a speed of 10 ℃/min, preserving heat for 6 hours, and then cooling the blank body to room temperature along with the furnace.
(5) Infiltration:
and (3) completely immersing the gel-removed green body in a metal precursor solution for 4 hours at room temperature, immersing the green body in an ammonia solution for 10 minutes, taking out, and drying in an oven for 24 hours.
The metal precursor solution of this example was an ethanol solution of zirconium oxychloride octahydrate, yttrium nitrate and magnesium nitrate, and the mass concentration of the metal ion was 0.3mol/L.
(6) Sintering:
sintering the dried blank in an atmosphere sintering furnace at 1850 ℃ and N 2 The flow rate is 0.5L/min, the temperature is kept for 6 hours, and then the mixture is cooled to room temperature along with a furnace, so as to obtain a sintered body. Sintered body is N 2 And (3) carrying out hot isostatic pressing treatment for 2 hours at the temperature of 1600 ℃ and the pressure of 180MPa in a protective atmosphere to obtain the aluminum nitride ceramic.
The aluminum nitride ceramic prepared by the method of this example had a relative density of 64.4%, a Vickers hardness of 14.2GPa, and a thermal conductivity of 126W/(mK).
Comparative example 1
Unlike example 1, the raw material ratio of comparative example 1 was 900g of aluminum nitride powder, 20g of polyvinyl butyral, 40g of yttrium oxide (sintering aid), and no hydrophobizing agent was contained. The ball milling and sieving process in the step (2) lacks a hydrophobic agent, and the rest of the preparation process is the same as that in the example 1.
The aluminum nitride ceramics prepared in comparative example 1 had a relative density of 56.8%, vickers hardness of 9.8GPa, and thermal conductivity of 98W/(mK). The aluminum nitride powder is not subjected to hydrolysis prevention treatment, so that the aluminum nitride powder is hydrolyzed with water-based glue during printing, the oxygen content is increased, and the thermal conductivity of the sintered aluminum nitride ceramic is reduced.
Comparative example 2
Unlike example 1, the raw material ratio of comparative example 2 was 900g of aluminum nitride powder, 40g of yttrium oxide (sintering aid), 40g of phosphoric acid (hydrophobizing agent), no polyvinyl butyral, the (1) powder modification step was absent, and the remaining preparation process was the same as example 1.
The aluminum nitride ceramic body prepared in comparative example 2 was layered after curing in step (4), and the subsequent paste discharging and sintering steps were not performed.
Comparative example 3
In contrast to example 1, in step S3 of comparative example 3, the molding process was specifically such that powder was fed into an adhesive injection molding apparatus, and a green body was produced by adhesive injection printing molding, and the layer thickness was 200 μm. The rest of the material proportion and the preparation flow are the same as in the example 1.
The aluminum nitride ceramic body prepared by the method of comparative example 3 has layering phenomenon after solidification in the step (4), and the subsequent glue discharging and sintering processes cannot be performed. This is because the setting of the thickness of the printed layer is relatively too large, the glue does not completely penetrate the aluminum nitride powder during printing, and the curing effect between layers is not obvious.
Comparative example 4
Unlike example 1, comparative example 4 lacks the infiltration process of step S5. That is, in comparative example 4, the aluminum nitride ceramic was obtained by directly sintering after the completion of the paste discharging process in step S4. The rest of the material proportion and the preparation flow are the same as in the example 1.
The aluminum nitride ceramic prepared in comparative example 4 had a relative density of 50%, a Vickers hardness of 8.3GPa, and a thermal conductivity of 80W/(mK).
Comparative example 5
Unlike example 1, comparative example 5 lacks the hot isostatic pressing treatment in step S6. That is, the aluminum nitride ceramic was obtained after the sintering in step S6 in comparative example 6. The rest of the material proportion and the preparation flow are the same as in the example 1.
The aluminum nitride ceramic prepared in comparative example 5 had a relative density of 60%, a Vickers hardness of 11.8GPa, and a thermal conductivity of 127W/(mK).
In the foregoing embodiments, the descriptions of the embodiments are focused on, and for those portions of one embodiment that are not described in detail, reference may be made to the related descriptions of other embodiments.
While the invention has been described with reference to certain preferred embodiments, it will be understood by those skilled in the art that various changes and substitutions of equivalents may be made and equivalents will be apparent to those skilled in the art without departing from the scope of the invention. Therefore, the protection scope of the invention is subject to the protection scope of the claims.
Claims (10)
1. The method for preparing the aluminum nitride ceramic by using the adhesive injection molding technology is characterized by comprising the following steps of:
s1, mixing 85-90 parts of aluminum nitride powder and 1-5 parts of polyvinyl butyral uniformly at 80-100 ℃ under the action of a solvent according to parts by weight, and then filtering, washing and drying to obtain modified aluminum nitride powder;
s2, ball-milling and uniformly mixing the modified aluminum nitride powder, 1-5 parts of the hydrophobizing agent and 1-10 parts of the sintering aid, drying, and sieving with a 150-200 mesh sieve to obtain printing powder;
s3, feeding the powder obtained in the step S2 into adhesive injection molding equipment, and performing adhesive injection molding to obtain a blank;
s4, solidifying the blank body and performing vacuum glue discharge or atmosphere protection glue discharge-air glue discharge two-step glue discharge treatment;
s5, completely immersing the gel-discharged blank body in a metal precursor solution for 2-4 hours at room temperature, immersing in an ammonia solution for 5-15 minutes, taking out, and drying for 12-48 hours;
s6, placing the green body dried in the S5 in an atmosphere sintering furnace for sintering to obtain a sintered body, and performing hot isostatic pressing treatment on the sintered body to obtain aluminum nitride ceramic;
in the step S1, the particle size of the aluminum nitride powder is submicron.
2. The method for preparing aluminum nitride ceramics by using the adhesive injection molding technology according to claim 1, wherein the hydrophobic agent is one or more of phosphoric acid, silane coupling agents KH550, DP270 and stearic acid.
3. The method of producing aluminum nitride ceramics by binder injection molding according to claim 1, wherein the sintering aid is yttria.
4. The method for preparing aluminum nitride ceramics by using the adhesive injection molding technology according to claim 1, wherein the metal ions in the metal precursor solution are Zr 4+ ，Y 3+ ，Mg 2+ At least one of them.
5. The method for preparing aluminum nitride ceramics by using the adhesive injection molding technology according to claim 1, wherein the concentration of metal ions in the metal precursor solution is 0.1-0.3 mol/L.
6. The method for preparing aluminum nitride ceramics by using the adhesive injection molding technology according to claim 1, wherein in the step S1, the particle size distribution of aluminum nitride powder is 0.2-1 μm.
7. The method for preparing aluminum nitride ceramics by using the adhesive injection molding technology according to claim 1, wherein the thickness of the adhesive injection printed layer is 100-150 μm in the step S3.
8. The method for preparing aluminum nitride ceramics by using the adhesive injection molding technology according to claim 1, wherein the specific operation of vacuum glue discharging is as follows: placing the blank in a vacuum glue discharging furnace with the pressure of-0.1 MPa, heating to 600-1200 ℃ at the speed of 5-10 ℃/min, preserving the temperature for 4-8 hours, and then cooling the blank to the room temperature along with the furnace;
the specific operation of the atmosphere protection glue discharging is as follows: placing the blank in Ar and/or N 2 Heating to 600-1200 ℃ at a speed of 5-10 ℃/min in a protected glue discharging furnace, preserving heat for 4-8h, and then cooling the blank to room temperature along with the furnace;
the specific operation of the air glue discharging is as follows: placing the blank body in a glue discharging furnace in air atmosphere, heating to 800-1000 ℃ at the speed of 5-10 ℃/min, preserving heat for 2-8h, and then cooling the blank body to room temperature along with the furnace.
9. The method for preparing aluminum nitride ceramics by using the binder injection molding technique according to claim 1, wherein in the step S6, sintering conditions are as follows: at N 2 The flow is 0.3-0.8L/min, and the temperature is kept for 6-12 h at 1700-1900 ℃; specific operation of the HIP is, in N 2 Or Ar protective atmosphere, carrying out hot isostatic pressing treatment on the sintered body for 1-2 h at 1350-1500 ℃ and 100-180 MPa.
10. An aluminum nitride ceramic produced by the production method according to any one of claims 1 to 9.
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