CN112591720A - Preparation method of porous aluminum nitride material - Google Patents
Preparation method of porous aluminum nitride material Download PDFInfo
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- CN112591720A CN112591720A CN202011480305.9A CN202011480305A CN112591720A CN 112591720 A CN112591720 A CN 112591720A CN 202011480305 A CN202011480305 A CN 202011480305A CN 112591720 A CN112591720 A CN 112591720A
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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 137
- 239000000463 material Substances 0.000 title claims abstract description 116
- 238000002360 preparation method Methods 0.000 title claims abstract description 69
- 238000003756 stirring Methods 0.000 claims abstract description 66
- 108010058846 Ovalbumin Proteins 0.000 claims abstract description 62
- 229940092253 ovalbumin Drugs 0.000 claims abstract description 62
- 239000000243 solution Substances 0.000 claims abstract description 59
- 238000001035 drying Methods 0.000 claims abstract description 51
- 238000000498 ball milling Methods 0.000 claims abstract description 42
- 239000002270 dispersing agent Substances 0.000 claims abstract description 37
- 239000000843 powder Substances 0.000 claims abstract description 37
- 239000003381 stabilizer Substances 0.000 claims abstract description 37
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000002002 slurry Substances 0.000 claims abstract description 28
- 239000008367 deionised water Substances 0.000 claims abstract description 22
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 22
- 238000005406 washing Methods 0.000 claims abstract description 19
- 238000005187 foaming Methods 0.000 claims abstract description 18
- 238000005245 sintering Methods 0.000 claims abstract description 17
- 238000001291 vacuum drying Methods 0.000 claims abstract description 15
- 238000001816 cooling Methods 0.000 claims abstract description 10
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 9
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000002253 acid Substances 0.000 claims abstract description 8
- 230000001681 protective effect Effects 0.000 claims abstract description 8
- 238000005303 weighing Methods 0.000 claims abstract description 8
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 28
- 238000005554 pickling Methods 0.000 claims description 28
- 238000000034 method Methods 0.000 claims description 24
- 238000010438 heat treatment Methods 0.000 claims description 21
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 14
- 229910017604 nitric acid Inorganic materials 0.000 claims description 14
- 229930006000 Sucrose Natural products 0.000 claims description 13
- 229960004793 sucrose Drugs 0.000 claims description 13
- 238000004519 manufacturing process Methods 0.000 claims description 12
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical group O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 claims description 8
- 235000013601 eggs Nutrition 0.000 claims description 7
- 239000007789 gas Substances 0.000 claims description 7
- 239000011259 mixed solution Substances 0.000 claims description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- QGZKDVFQNNGYKY-UHFFFAOYSA-O ammonium group Chemical group [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 6
- 229920000058 polyacrylate Polymers 0.000 claims description 6
- 239000002994 raw material Substances 0.000 description 11
- 239000005720 sucrose Substances 0.000 description 11
- 238000006243 chemical reaction Methods 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 125000000185 sucrose group Chemical group 0.000 description 5
- 239000006260 foam Substances 0.000 description 3
- 239000004088 foaming agent Substances 0.000 description 3
- 238000011065 in-situ storage Methods 0.000 description 3
- 229920002521 macromolecule Polymers 0.000 description 3
- 239000000178 monomer Substances 0.000 description 3
- 238000006116 polymerization reaction Methods 0.000 description 3
- 108090000623 proteins and genes Proteins 0.000 description 3
- 102000004169 proteins and genes Human genes 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- 229920002125 Sokalan® Polymers 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 239000000615 nonconductor Substances 0.000 description 1
- 239000004584 polyacrylic acid Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/072—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with aluminium
- C01B21/0728—After-treatment, e.g. grinding, purification
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Abstract
A preparation method of a porous aluminum nitride material belongs to the technical field of preparation of aluminum nitride materials. The technical problem to be solved by the present invention is the porous property of aluminum nitride material. The invention adds Al (H) into aluminum nitride2PO4)3Adding the solution into a ball mill for ball milling, performing vacuum drying, adding ovalbumin into deionized water, uniformly stirring, then weighing pretreated aluminum nitride powder, ovalbumin solution, dispersant and stabilizer, adding the aluminum nitride powder into the ovalbumin solution under the stirring condition, adding the dispersant and the stabilizer after stirring to obtain a premix, putting the premix into the ball mill for ball milling, injecting the slurry after ball milling into a mold, standing and foaming for a certain time, putting into an oven for drying, putting into a furnace body, introducing protective gas, sintering, cooling, taking out of the furnace, performing acid washing and water washing, and then drying to obtain the porous aluminum nitride material. The invention has simple operation, simple equipment and low cost.
Description
Technical Field
The invention belongs to the technical field of aluminum nitride material preparation; in particular to a preparation method of a porous aluminum nitride material.
Background
Aluminum nitride materials are atomic crystals, diamond-like nitrides, which are stable up to 2200 ℃. The strength at room temperature is high, and the strength is slowly reduced along with the increase of the temperature. The material has good thermal conductivity and small thermal expansion coefficient, and is a good thermal shock resistant material. The crucible material has strong capability of resisting the corrosion of molten metal and is an ideal crucible material for casting pure iron, aluminum or aluminum alloy. Aluminum nitride is also an electrical insulator, has good dielectric properties, and is promising for use as an electrical component. The existing aluminum nitride material is prepared by simple sintering and purification, and the obtained aluminum nitride material is compact. Has great influence on the volatilization of raw materials and the growth of crystals.
Disclosure of Invention
The invention aims to provide a preparation method of a porous aluminum nitride material with simple production process.
The invention is realized by the following technical scheme:
a preparation method of the porous aluminum nitride material comprises the following steps:
step 1, adding Al (H) with certain mass into aluminum nitride2PO4)3Adding the solution into a ball mill for ball milling, and then drying in vacuum to obtain pretreated aluminum nitride powder for later use;
step 2, adding the ovalbumin into deionized water, and stirring uniformly to obtain an ovalbumin solution for later use;
step 3, respectively weighing the pretreated aluminum nitride powder, the ovalbumin solution, the dispersant and the stabilizer according to a certain volume ratio, adding the weighed aluminum nitride powder into the ovalbumin solution under the stirring condition, stirring for a certain time, then adding the dispersant, continuing stirring for a certain time, adding the stabilizer, and continuously stirring for a certain time to obtain a premix for later use;
step 4, putting the premix obtained in the step 3 into a ball mill for ball milling, injecting the ball-milled slurry into a mould, standing for foaming for a certain time, and then putting into an oven for drying to obtain dried slurry for later use;
and 5, putting the dried slurry obtained in the step 4 into a furnace body, introducing protective gas, sintering, cooling, taking out of the furnace, carrying out acid washing and water washing, and then drying to obtain the porous aluminum nitride material.
The invention relates to a preparation method of a porous aluminum nitride material, wherein Al (H) is adopted in step 12PO4)3The concentration of the solution is 0.5-2 mol/L, aluminum nitride and Al (H)2PO4)3The mass ratio of the solution is 100:1 to 5.
The preparation method of the porous aluminum nitride material comprises the step 1 of ball milling for 2-3 hours according to the ball-to-material mass ratio of 3-4: 1, wherein the vacuum drying temperature is 80-90 ℃, and the vacuum drying time is 1-4 hours.
According to the preparation method of the porous aluminum nitride material, in the step 2, the volume ratio of the ovalbumin to the deionized water is 5-10: 1, the stirring time is 15-30 min, and the ovalbumin is extracted from fresh eggs.
According to the preparation method of the porous aluminum nitride material, in the step 3, the volume ratio of the aluminum nitride powder, the ovalbumin solution, the dispersing agent and the stabilizing agent is 40-50: 100: 1-5: 20-30, the dispersing agent is ammonium polyacrylate, and the stabilizing agent is cane sugar.
According to the preparation method of the porous aluminum nitride material, in the step 3, aluminum nitride powder is added into an ovalbumin solution, a dispersing agent is added after stirring for 20-60 min, a stabilizing agent is added after stirring for 20-60 min, and stirring is continued for 20-60 min to obtain a premix.
According to the preparation method of the porous aluminum nitride material, the ball milling method in the step 4 is to perform ball milling for 4-5 hours according to the mass ratio of balls to materials being 3-7: 1, the standing foaming time is 30-60 min, the drying temperature is 80-90 ℃, and the drying time is 1-2 hours.
The preparation method of the porous aluminum nitride material comprises the steps of (5) introducing nitrogen into a furnace body, heating to 700-800 ℃ at a heating rate of 4 ℃/min, heating to 1500-1550 ℃ at a heating rate of 3 ℃/min, reacting at a constant temperature for 2 hours, and cooling to room temperature along with the furnace.
According to the preparation method of the porous aluminum nitride material, in the step 5, a mixed solution of hydrofluoric acid and nitric acid is adopted for pickling, the volume ratio of the hydrofluoric acid to the nitric acid is 1:2, the pickling temperature is 40-50 ℃, the pickling time is 3-8 hours, the material is washed for 3-5 times by deionized water after pickling, the drying temperature is 80-90 ℃, and the drying time is 1-4 hours.
According to the preparation method of the porous aluminum nitride material, ovalbumin is used as a foaming agent to foam, protein is denatured in the heating process, slurry is solidified through in-situ polymerization of organic monomers, added sucrose is used for maintaining the foaming stability of the slurry, and meanwhile, the network structure of sucrose macromolecules is removed in the sintering process to form holes.
The preparation method of the porous aluminum nitride material has the advantages of simple operation, simple equipment and low cost, and can be used for preparing porous raw materials with various shapes so as to adapt to different crucibles, and substances added in the preparation process are removed in the sintering process without influencing the purity of the raw materials.
Drawings
Fig. 1 is an SEM photograph of a porous aluminum nitride material prepared by a method according to an embodiment.
Detailed Description
The first embodiment is as follows:
a preparation method of the porous aluminum nitride material comprises the following steps:
step 1, adding Al (H) with certain mass into aluminum nitride2PO4)3Adding the solution into a ball mill for ball milling, and then drying in vacuum to obtain pretreated aluminum nitride powder for later use;
step 2, adding the ovalbumin into deionized water, and stirring uniformly to obtain an ovalbumin solution for later use;
step 3, respectively weighing the pretreated aluminum nitride powder, the ovalbumin solution, the dispersant and the stabilizer according to a certain volume ratio, adding the weighed aluminum nitride powder into the ovalbumin solution under the stirring condition, stirring for a certain time, then adding the dispersant, continuing stirring for a certain time, adding the stabilizer, and continuously stirring for a certain time to obtain a premix for later use;
step 4, putting the premix obtained in the step 3 into a ball mill for ball milling, injecting the ball-milled slurry into a mould, standing for foaming for a certain time, and then putting into an oven for drying to obtain dried slurry for later use;
and 5, putting the dried slurry obtained in the step 4 into a furnace body, introducing protective gas, sintering, cooling, taking out of the furnace, carrying out acid washing and water washing, and then drying to obtain the porous aluminum nitride material.
The method for producing a porous aluminum nitride material according to the present embodiment includes Al (H) in step 12PO4)3The concentration of the solution was 1mol/L, aluminum nitride and Al (H)2PO4)3The mass ratio of the solution is 100: 1.
in the preparation method of the porous aluminum nitride material in the embodiment, the ball milling method in the step 1 is to perform ball milling for 2 hours according to the ball-to-material mass ratio of 3:1, the vacuum drying temperature is 80 ℃, and the vacuum drying time is 2 hours.
In the preparation method of the porous aluminum nitride material according to the embodiment, in the step 2, the volume ratio of the ovalbumin to the deionized water is 8:1, the stirring time is 30min, and the ovalbumin is extracted from fresh eggs.
In the preparation method of the porous aluminum nitride material according to the embodiment, in the step 3, the volume ratio of the aluminum nitride powder, the ovalbumin solution, the dispersant and the stabilizer is 40:100:2:25, the dispersant is ammonium polyacrylate, and the stabilizer is sucrose.
In the preparation method of the porous aluminum nitride material according to the embodiment, in the step 3, aluminum nitride powder is added into an ovalbumin solution, a dispersant is added after stirring for 30min, a stabilizer is added after stirring for 30min, and stirring is continued for 30min to obtain a premix.
In the preparation method of the porous aluminum nitride material in the embodiment, the ball milling method in the step 4 is to perform ball milling for 4 hours according to the ball-to-material mass ratio of 7:1, the standing foaming time is 60min, the drying temperature is 80 ℃, and the drying time is 1 hour.
In the preparation method of the porous aluminum nitride material according to the embodiment, in the step 5, after nitrogen is introduced into the furnace body, the temperature is raised to 800 ℃ at the heating rate of 4 ℃/min, then the temperature is raised to 1550 ℃ at the heating rate of 3 ℃/min, the temperature is kept constant for reaction for 2 hours, and then the temperature is cooled to room temperature along with the furnace.
In the preparation method of the porous aluminum nitride material according to the embodiment, in the step 5, a mixed solution of hydrofluoric acid and nitric acid is adopted for pickling, the volume ratio of the hydrofluoric acid to the nitric acid is 1:2, the pickling temperature is 40 ℃, the pickling time is 4 hours, deionized water is used for washing for 5 times after pickling, the drying temperature is 80 ℃, and the drying time is 2 hours.
In the method for preparing a porous aluminum nitride material according to the present embodiment, an SEM picture of the prepared porous aluminum nitride material is shown in fig. 1, and as can be seen from fig. 1, the material is in a porous form, and the form of the material is uniform.
According to the preparation method of the porous aluminum nitride material, ovalbumin is used as a foaming agent to foam, protein is denatured in the heating process, slurry is solidified through in-situ polymerization of organic monomers, added sucrose is used for maintaining the foaming stability of the slurry, and meanwhile, the network structure of the sucrose macromolecules is removed in the sintering process to form holes.
The second embodiment is as follows:
a preparation method of the porous aluminum nitride material comprises the following steps:
step 1, adding Al (H) with certain mass into aluminum nitride2PO4)3Adding the solution into a ball mill for ball milling, and then drying in vacuum to obtain pretreated aluminum nitride powder for later use;
step 2, adding the ovalbumin into deionized water, and stirring uniformly to obtain an ovalbumin solution for later use;
step 3, respectively weighing the pretreated aluminum nitride powder, the ovalbumin solution, the dispersant and the stabilizer according to a certain volume ratio, adding the weighed aluminum nitride powder into the ovalbumin solution under the stirring condition, stirring for a certain time, then adding the dispersant, continuing stirring for a certain time, adding the stabilizer, and continuously stirring for a certain time to obtain a premix for later use;
step 4, putting the premix obtained in the step 3 into a ball mill for ball milling, injecting the ball-milled slurry into a mould, standing for foaming for a certain time, and then putting into an oven for drying to obtain dried slurry for later use;
and 5, putting the dried slurry obtained in the step 4 into a furnace body, introducing protective gas, sintering, cooling, taking out of the furnace, carrying out acid washing and water washing, and then drying to obtain the porous aluminum nitride material.
The method for producing a porous aluminum nitride material according to the present embodiment includes Al (H) in step 12PO4)3The concentration of the solution was 0.5mol/L, aluminum nitride and Al (H)2PO4)3The mass ratio of the solution is 100: 1.
in the preparation method of the porous aluminum nitride material in the embodiment, the ball milling method in the step 1 is to perform ball milling for 3 hours according to the ball-to-material mass ratio of 4:1, the vacuum drying temperature is 90 ℃, and the vacuum drying time is 4 hours.
In the preparation method of the porous aluminum nitride material according to the embodiment, in the step 2, the volume ratio of the ovalbumin to the deionized water is 5:1, the stirring time is 15min, and the ovalbumin is extracted from fresh eggs.
In the preparation method of the porous aluminum nitride material according to the embodiment, in the step 3, the volume ratio of the aluminum nitride powder, the ovalbumin solution, the dispersant and the stabilizer is 50:100:5:30, the dispersant is ammonium polyacrylate, and the stabilizer is sucrose.
In the preparation method of the porous aluminum nitride material according to the embodiment, in the step 3, aluminum nitride powder is added into an ovalbumin solution, a dispersing agent is added after stirring for 60min, a stabilizing agent is added after stirring for 60min, and stirring is continued for 60min to obtain a premix.
In the preparation method of the porous aluminum nitride material in the embodiment, the ball milling method in the step 4 is to perform ball milling for 5 hours according to the ball-to-material mass ratio of 6:1, the standing foaming time is 30min, the drying temperature is 90 ℃, and the drying time is 2 hours.
In the preparation method of the porous aluminum nitride material according to the embodiment, in the step 5, after nitrogen is introduced into the furnace body, the temperature is raised to 800 ℃ at the heating rate of 4 ℃/min, then the temperature is raised to 1550 ℃ at the heating rate of 3 ℃/min, the temperature is kept constant for reaction for 2 hours, and then the temperature is cooled to room temperature along with the furnace.
In the preparation method of the porous aluminum nitride material according to the embodiment, in the step 5, a mixed solution of hydrofluoric acid and nitric acid is adopted for pickling, the volume ratio of the hydrofluoric acid to the nitric acid is 1:2, the pickling temperature is 50 ℃, the pickling time is 8 hours, the material is washed for 5 times by deionized water after pickling, the drying temperature is 80 ℃, and the drying time is 1 hour.
The preparation method of the porous aluminum nitride material has the advantages of simple operation, simple equipment and low cost, and can be used for preparing porous raw materials with various shapes so as to adapt to different crucibles, and substances added in the preparation process are removed in the sintering process without influencing the purity of the raw materials.
The third concrete implementation mode:
a preparation method of the porous aluminum nitride material comprises the following steps:
step 1, adding Al (H) with certain mass into aluminum nitride2PO4)3Adding the solution into a ball mill for ball milling, and then drying in vacuum to obtain pretreated aluminum nitride powder for later use;
step 2, adding the ovalbumin into deionized water, and stirring uniformly to obtain an ovalbumin solution for later use;
step 3, respectively weighing the pretreated aluminum nitride powder, the ovalbumin solution, the dispersant and the stabilizer according to a certain volume ratio, adding the weighed aluminum nitride powder into the ovalbumin solution under the stirring condition, stirring for a certain time, then adding the dispersant, continuing stirring for a certain time, adding the stabilizer, and continuously stirring for a certain time to obtain a premix for later use;
step 4, putting the premix obtained in the step 3 into a ball mill for ball milling, injecting the ball-milled slurry into a mould, standing for foaming for a certain time, and then putting into an oven for drying to obtain dried slurry for later use;
and 5, putting the dried slurry obtained in the step 4 into a furnace body, introducing protective gas, sintering, cooling, taking out of the furnace, carrying out acid washing and water washing, and then drying to obtain the porous aluminum nitride material.
The method for producing a porous aluminum nitride material according to the present embodiment includes Al (H) in step 12PO4)3The concentration of the solution was 2mol/L, aluminum nitride and Al (H)2PO4)3The mass ratio of the solution is 100: 5.
in the preparation method of the porous aluminum nitride material in the embodiment, the ball milling method in the step 1 is to perform ball milling for 2 hours according to the mass ratio of balls to materials of 4:1, the vacuum drying temperature is 80 ℃, and the vacuum drying time is 1 hour.
In the preparation method of the porous aluminum nitride material according to the embodiment, in the step 2, the volume ratio of the ovalbumin to the deionized water is 10:1, the stirring time is 30min, and the ovalbumin is extracted from fresh eggs.
In the preparation method of the porous aluminum nitride material according to the embodiment, in the step 3, the volume ratio of the aluminum nitride powder, the ovalbumin solution, the dispersant and the stabilizer is 50:100:1:20, the dispersant is ammonium polyacrylate, and the stabilizer is sucrose.
In the preparation method of the porous aluminum nitride material according to the embodiment, in the step 3, aluminum nitride powder is added into an ovalbumin solution, a dispersing agent is added after stirring for 20min, a stabilizing agent is added after stirring for 20min, and stirring is continued for 20min to obtain a premix.
In the preparation method of the porous aluminum nitride material in the embodiment, the ball milling method in the step 4 is to perform ball milling for 4 hours according to the ball-to-material mass ratio of 3:1, the standing foaming time is 60min, the drying temperature is 80 ℃, and the drying time is 2 hours.
In the preparation method of the porous aluminum nitride material according to the embodiment, in the step 5, after nitrogen is introduced into the furnace body, the temperature is raised to 700 ℃ at the heating rate of 4 ℃/min, then the temperature is raised to 1500 ℃ at the heating rate of 3 ℃/min, the temperature is kept constant for reaction for 2 hours, and then the temperature is cooled to room temperature along with the furnace.
In the preparation method of the porous aluminum nitride material according to the embodiment, in the step 5, a mixed solution of hydrofluoric acid and nitric acid is adopted for pickling, the volume ratio of the hydrofluoric acid to the nitric acid is 1:2, the pickling temperature is 40 ℃, the pickling time is 3 hours, deionized water is used for washing for 5 times after pickling, the drying temperature is 80 ℃, and the drying time is 4 hours.
The preparation method of the porous aluminum nitride material has the advantages of simple operation, simple equipment and low cost, and can be used for preparing porous raw materials with various shapes so as to adapt to different crucibles, and substances added in the preparation process are removed in the sintering process without influencing the purity of the raw materials.
The fourth concrete implementation mode:
a preparation method of the porous aluminum nitride material comprises the following steps:
step 1, adding Al (H) with certain mass into aluminum nitride2PO4)3Adding the solution into a ball mill for ball milling, and then drying in vacuum to obtain pretreated aluminum nitride powder for later use;
step 2, adding the ovalbumin into deionized water, and stirring uniformly to obtain an ovalbumin solution for later use;
step 3, respectively weighing the pretreated aluminum nitride powder, the ovalbumin solution, the dispersant and the stabilizer according to a certain volume ratio, adding the weighed aluminum nitride powder into the ovalbumin solution under the stirring condition, stirring for a certain time, then adding the dispersant, continuing stirring for a certain time, adding the stabilizer, and continuously stirring for a certain time to obtain a premix for later use;
step 4, putting the premix obtained in the step 3 into a ball mill for ball milling, injecting the ball-milled slurry into a mould, standing for foaming for a certain time, and then putting into an oven for drying to obtain dried slurry for later use;
and 5, putting the dried slurry obtained in the step 4 into a furnace body, introducing protective gas, sintering, cooling, taking out of the furnace, carrying out acid washing and water washing, and then drying to obtain the porous aluminum nitride material.
The method for producing a porous aluminum nitride material according to the present embodiment includes Al (H) in step 12PO4)3The concentration of the solution was 1.5mol/L, aluminum nitride and Al (H)2PO4)3The mass ratio of the solution is 100：3。
In the preparation method of the porous aluminum nitride material in the embodiment, the ball milling method in the step 1 is to perform ball milling for 2 hours according to the ball-to-material mass ratio of 3.5:1, the vacuum drying temperature is 85 ℃, and the vacuum drying time is 2 hours.
In the preparation method of the porous aluminum nitride material according to the embodiment, in the step 2, the volume ratio of the ovalbumin to the deionized water is 6:1, the stirring time is 30min, and the ovalbumin is extracted from fresh eggs.
In the preparation method of the porous aluminum nitride material according to the embodiment, in the step 3, the volume ratio of the aluminum nitride powder, the ovalbumin solution, the dispersant and the stabilizer is 45:100:3:25, the dispersant is ammonium polyacrylate, and the stabilizer is sucrose.
In the preparation method of the porous aluminum nitride material according to the embodiment, in the step 3, aluminum nitride powder is added into an ovalbumin solution, a dispersing agent is added after stirring for 40min, a stabilizing agent is added after stirring for 40min, and stirring is continued for 30min to obtain a premix.
In the preparation method of the porous aluminum nitride material in the embodiment, the ball milling method in the step 4 is to perform ball milling for 5 hours according to the mass ratio of balls to materials being 5:1, the standing and foaming time is 40min, the drying temperature is 80 ℃, and the drying time is 1 hour.
In the preparation method of the porous aluminum nitride material according to the embodiment, in the step 5, after nitrogen is introduced into the furnace body, the temperature is raised to 750 ℃ at the heating rate of 4 ℃/min, then the temperature is raised to 1550 ℃ at the heating rate of 3 ℃/min, the temperature is kept constant for reaction for 2 hours, and then the temperature is cooled to room temperature along with the furnace.
In the preparation method of the porous aluminum nitride material according to the embodiment, in the step 5, a mixed solution of hydrofluoric acid and nitric acid is adopted for pickling, the volume ratio of the hydrofluoric acid to the nitric acid is 1:2, the pickling temperature is 45 ℃, the pickling time is 5 hours, deionized water is used for washing for 5 times after pickling, the drying temperature is 80 ℃, and the drying time is 3 hours.
The preparation method of the porous aluminum nitride material has the advantages of simple operation, simple equipment and low cost, and can be used for preparing porous raw materials with various shapes so as to adapt to different crucibles, and substances added in the preparation process are removed in the sintering process without influencing the purity of the raw materials.
The fifth concrete implementation mode:
a preparation method of the porous aluminum nitride material comprises the following steps:
step 1, adding Al (H) with certain mass into aluminum nitride2PO4)3Adding the solution into a ball mill for ball milling, and then drying in vacuum to obtain pretreated aluminum nitride powder for later use;
step 2, adding the ovalbumin into deionized water, and stirring uniformly to obtain an ovalbumin solution for later use;
step 3, respectively weighing the pretreated aluminum nitride powder, the ovalbumin solution, the dispersant and the stabilizer according to a certain volume ratio, adding the weighed aluminum nitride powder into the ovalbumin solution under the stirring condition, stirring for a certain time, then adding the dispersant, continuing stirring for a certain time, adding the stabilizer, and continuously stirring for a certain time to obtain a premix for later use;
step 4, putting the premix obtained in the step 3 into a ball mill for ball milling, injecting the ball-milled slurry into a mould, standing for foaming for a certain time, and then putting into an oven for drying to obtain dried slurry for later use;
and 5, putting the dried slurry obtained in the step 4 into a furnace body, introducing protective gas, sintering, cooling, taking out of the furnace, carrying out acid washing and water washing, and then drying to obtain the porous aluminum nitride material.
According to the preparation method of the porous aluminum nitride material, ovalbumin is used as a foaming agent to foam, protein is denatured in the heating process, slurry is solidified through in-situ polymerization of organic monomers, added sucrose is used for maintaining the foaming stability of the slurry, and meanwhile, the network structure of the sucrose macromolecules is removed in the sintering process to form holes.
The preparation method of the porous aluminum nitride material has the advantages of simple operation, simple equipment and low cost, and can be used for preparing porous raw materials with various shapes so as to adapt to different crucibles, and substances added in the preparation process are removed in the sintering process without influencing the purity of the raw materials.
The sixth specific implementation mode:
according to the fifth embodiment, in step 1, Al (H) is used as the material of the porous aluminum nitride material2PO4)3The concentration of the solution is 0.5-2 mol/L, aluminum nitride and Al (H)2PO4)3The mass ratio of the solution is 100:1 to 5.
The seventh embodiment:
according to the preparation method of the porous aluminum nitride material, in the step 1, ball milling is carried out for 2-3 hours according to the mass ratio of balls to materials being 3-4: 1, the vacuum drying temperature is 80-90 ℃, and the vacuum drying time is 1-4 hours.
The specific implementation mode is eight:
according to the preparation method of the porous aluminum nitride material, in the step 2, the volume ratio of the ovalbumin to the deionized water is 5-10: 1, the stirring time is 15-30 min, and the ovalbumin is extracted from fresh eggs.
The specific implementation method nine:
according to the fifth specific embodiment, in the step 3, the volume ratio of the aluminum nitride powder, the ovalbumin solution, the dispersant and the stabilizer is 40-50: 100: 1-5: 20-30, the dispersant is polyacrylic acid ammonia, and the stabilizer is sucrose.
The detailed implementation mode is ten:
according to the preparation method of the porous aluminum nitride material, in the step 3, aluminum nitride powder is added into an ovalbumin solution, a dispersing agent is added after stirring for 20-60 min, a stabilizing agent is added after stirring for 20-60 min, and stirring is continued for 20-60 min to obtain a premix.
The concrete implementation mode eleven:
according to the preparation method of the porous aluminum nitride material, in the step 4, ball milling is carried out for 4-5 hours according to the mass ratio of balls to materials being 3-7: 1, standing and foaming time is 30-60 min, drying temperature is 80-90 ℃, and drying time is 1-2 hours.
The specific implementation mode twelve:
according to the preparation method of the porous aluminum nitride material, in the step 5, after nitrogen is introduced into the furnace body, the temperature is raised to 700-800 ℃ at the heating rate of 4 ℃/min, then the temperature is raised to 1500-1550 ℃ at the heating rate of 3 ℃/min, the temperature is kept constant for reaction for 2 hours, and then the temperature is cooled to room temperature along with the furnace.
The specific implementation mode is thirteen:
according to the preparation method of the porous aluminum nitride material, in the step 5, a mixed solution of hydrofluoric acid and nitric acid is adopted for pickling, the volume ratio of the hydrofluoric acid to the nitric acid is 1:2, the pickling temperature is 40-50 ℃, the pickling time is 3-8 hours, the material is washed for 3-5 times by deionized water after pickling, the drying temperature is 80-90 ℃, and the drying time is 1-4 hours.
Claims (9)
1. A preparation method of a porous aluminum nitride material is characterized by comprising the following steps: the method comprises the following steps:
step 1, adding Al (H) with certain mass into aluminum nitride2PO4)3Adding the solution into a ball mill for ball milling, and then drying in vacuum to obtain pretreated aluminum nitride powder for later use;
step 2, adding the ovalbumin into deionized water, and stirring uniformly to obtain an ovalbumin solution for later use;
step 3, respectively weighing the pretreated aluminum nitride powder, the ovalbumin solution, the dispersant and the stabilizer according to a certain volume ratio, adding the weighed aluminum nitride powder into the ovalbumin solution under the stirring condition, stirring for a certain time, then adding the dispersant, continuing stirring for a certain time, adding the stabilizer, and continuously stirring for a certain time to obtain a premix for later use;
step 4, putting the premix obtained in the step 3 into a ball mill for ball milling, injecting the ball-milled slurry into a mould, standing for foaming for a certain time, and then putting into an oven for drying to obtain dried slurry for later use;
and 5, putting the dried slurry obtained in the step 4 into a furnace body, introducing protective gas, sintering, cooling, taking out of the furnace, carrying out acid washing and water washing, and then drying to obtain the porous aluminum nitride material.
2. The method for preparing a porous aluminum nitride material according to claim 1, characterized in that: step 1 Al (H)2PO4)3The concentration of the solution is 0.5-2 mol/L, aluminum nitride and Al (H)2PO4)3The mass ratio of the solution is 100:1 to 5.
3. The method for producing a porous aluminum nitride material according to claim 1 or 2, characterized in that: the ball milling method in the step 1 is to perform ball milling for 2-3 hours according to the ball-to-material mass ratio of 3-4: 1, wherein the vacuum drying temperature is 80-90 ℃, and the vacuum drying time is 1-4 hours.
4. The method for producing a porous aluminum nitride material according to claim 3, characterized in that: in the step 2, the volume ratio of the ovalbumin to the deionized water is 5-10: 1, the stirring time is 15-30 min, and the ovalbumin is extracted from fresh eggs.
5. The method for producing a porous aluminum nitride material according to claim 4, characterized in that: in the step 3, the volume ratio of the aluminum nitride powder, the ovalbumin solution, the dispersing agent and the stabilizing agent is 40-50: 100: 1-5: 20-30, the dispersing agent is ammonium polyacrylate, and the stabilizing agent is cane sugar.
6. The method for producing a porous aluminum nitride material according to claim 5, characterized in that: and 3, adding the aluminum nitride powder into the ovalbumin solution, stirring for 20-60 min, then adding a dispersing agent, continuing to stir for 20-60 min, then adding a stabilizing agent, and continuing to stir for 20-60 min to obtain the premix.
7. The method for producing a porous aluminum nitride material according to claim 6, characterized in that: the ball milling method in the step 4 is to perform ball milling for 4-5 hours according to the ball-to-material mass ratio of 3-7: 1, the standing and foaming time is 30-60 min, the drying temperature is 80-90 ℃, and the drying time is 1-2 hours.
8. The method for producing a porous aluminum nitride material according to claim 7, characterized in that: and 5, after introducing nitrogen into the furnace body, heating to 700-800 ℃ at the heating rate of 4 ℃/min, then heating to 1500-1550 ℃ at the heating rate of 3 ℃/min, reacting at constant temperature for 2h, and cooling to room temperature along with the furnace.
9. The method for producing a porous aluminum nitride material according to claim 8, characterized in that: and in the step 5, a mixed solution of hydrofluoric acid and nitric acid is adopted for pickling, the volume ratio of the hydrofluoric acid to the nitric acid is 1:2, the pickling temperature is 40-50 ℃, the pickling time is 3-8 h, the pickling is carried out for 3-5 times by using deionized water, the drying temperature is 80-90 ℃, and the drying time is 1-4 h.
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