CN113213947A - Aluminum nitride doped modified nano silicon nitride composite ceramic powder and preparation method thereof - Google Patents
Aluminum nitride doped modified nano silicon nitride composite ceramic powder and preparation method thereof Download PDFInfo
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- 229910052581 Si3N4 Inorganic materials 0.000 title claims abstract description 109
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 title claims abstract description 109
- 239000005543 nano-size silicon particle Substances 0.000 title claims abstract description 79
- 239000000919 ceramic Substances 0.000 title claims abstract description 76
- 239000000843 powder Substances 0.000 title claims abstract description 70
- 239000002131 composite material Substances 0.000 title claims abstract description 56
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 58
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 51
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 23
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims abstract description 23
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000011863 silicon-based powder Substances 0.000 claims abstract description 23
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 19
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 56
- 239000000203 mixture Substances 0.000 claims description 50
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 claims description 42
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 28
- 229910052710 silicon Inorganic materials 0.000 claims description 28
- 239000010703 silicon Substances 0.000 claims description 28
- 239000000725 suspension Substances 0.000 claims description 28
- 238000001035 drying Methods 0.000 claims description 23
- 238000002156 mixing Methods 0.000 claims description 22
- 238000003756 stirring Methods 0.000 claims description 21
- 239000002002 slurry Substances 0.000 claims description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- BKHUGLYOPGMVDT-UHFFFAOYSA-N C(C)O.[N+](=O)([O-])[O-].[Y+3].[N+](=O)([O-])[O-].[N+](=O)([O-])[O-] Chemical compound C(C)O.[N+](=O)([O-])[O-].[Y+3].[N+](=O)([O-])[O-].[N+](=O)([O-])[O-] BKHUGLYOPGMVDT-UHFFFAOYSA-N 0.000 claims description 14
- CSCPPACGZOOCGX-UHFFFAOYSA-N acetone Substances CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 14
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 14
- 238000011282 treatment Methods 0.000 claims description 14
- IMNIMPAHZVJRPE-UHFFFAOYSA-N triethylenediamine Chemical compound C1CN2CCN1CC2 IMNIMPAHZVJRPE-UHFFFAOYSA-N 0.000 claims description 14
- 238000005245 sintering Methods 0.000 claims description 10
- 239000007888 film coating Substances 0.000 claims description 8
- 238000009501 film coating Methods 0.000 claims description 8
- 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 claims description 7
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 230000003213 activating effect Effects 0.000 claims description 7
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 239000011248 coating agent Substances 0.000 claims description 7
- 238000000576 coating method Methods 0.000 claims description 7
- 238000005238 degreasing Methods 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 7
- 230000001376 precipitating effect Effects 0.000 claims description 7
- 239000012716 precipitator Substances 0.000 claims description 7
- 230000001235 sensitizing effect Effects 0.000 claims description 7
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- 239000007789 gas Substances 0.000 claims description 2
- 230000001681 protective effect Effects 0.000 claims description 2
- 238000007788 roughening Methods 0.000 claims description 2
- 239000006185 dispersion Substances 0.000 abstract description 4
- 230000003647 oxidation Effects 0.000 abstract description 2
- 238000007254 oxidation reaction Methods 0.000 abstract description 2
- 229910010293 ceramic material Inorganic materials 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- 238000000926 separation method Methods 0.000 description 4
- 238000005260 corrosion Methods 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 239000002585 base Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 229920001577 copolymer Polymers 0.000 description 2
- 238000003746 solid phase reaction Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000000498 ball milling Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000701 coagulant Substances 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005307 ferromagnetism Effects 0.000 description 1
- RPOCFUQMSVZQLH-UHFFFAOYSA-N furan-2,5-dione;2-methylprop-1-ene Chemical compound CC(C)=C.O=C1OC(=O)C=C1 RPOCFUQMSVZQLH-UHFFFAOYSA-N 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000002715 modification method Methods 0.000 description 1
- -1 nano nickel nitride Chemical class 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
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Abstract
The invention discloses aluminum nitride-doped modified nano silicon nitride composite ceramic powder and a preparation method thereof, wherein the aluminum nitride-doped modified nano silicon nitride composite ceramic powder comprises a component A and a component B, wherein the component A comprises the following components in parts by weight: 40-60 parts of aluminum powder and 100 parts of modified nano silicon nitride; the component B comprises the following components in parts by weight: 30 to 40 parts of aluminum powder, 20 to 80 parts of silicon powder, 5 to 10 parts of zirconium dioxide and 8 to 15 parts of yttrium oxide. The aluminum nitride doped modified nano silicon nitride composite ceramic powder prepared by the invention has the advantages of uniform dispersion of all components, good oxidation resistance, mechanical strength and fracture toughness.
Description
Technical Field
The invention relates to the technical field of ceramic materials, in particular to aluminum nitride doped modified nano silicon nitride composite ceramic powder and a preparation method thereof.
Background
The silicon nitride ceramic material is an important nitride ceramic material, has the comprehensive properties of high strength, high hardness, wear resistance, corrosion resistance, stress impact resistance and the like, is an important engineering material, has the characteristics of low dielectric constant and low dielectric loss, and has wide application in the fields of electronic information, energy chemical industry, aerospace, national defense and military industry, civil use and the like. The aluminum nitride and silicon nitride multi-element composite ceramic material is used as an advanced structural ceramic material, has excellent corrosion resistance, mechanical property and impact resistance, and is synthesized into ceramic composite powder by adopting a solid-phase reaction method, ball-milling and mixing by a wet method, drying and calcining in the actual production. However, this synthesis method has a problem of poor purity and structural uniformity.
Chinese patent CN106518040A discloses a method for synthesizing ceramic composite powder, comprising: preparing aqueous slurry of a ceramic raw material, wherein the aqueous slurry comprises the ceramic raw material, water and an organic copolymer with low polymerization degree, and the ceramic raw material comprises at least two components; adding a cross-linking coagulant into the aqueous slurry to obtain a gel; dehydrating and drying the gel to obtain a dried gel; heating the dried gel to the synthesis temperature of the ceramic composite powder and preserving heat to obtain ceramic composite powder or ceramic composite base powder; and carrying out secondary doping on the ceramic composite base powder to obtain ceramic composite powder. According to the patent, the isobutene-maleic anhydride organic copolymer amide-ammonium salt can enable all components in the multi-component ceramic raw material to be uniformly dispersed, and has a rapid gelling function; meanwhile, the problems that the ceramic composite powder synthesized by the traditional solid phase reaction method is easy to cause uneven dispersion of all components and high calcining synthesis temperature are solved. However, the ceramic raw material powder body is optimized, and the dispersion uniformity on the dispersant-ceramic matrix and the uniformity of the ceramic microstructure need to be further optimized.
Disclosure of Invention
In view of the above, the present invention provides an aluminum nitride doped modified nano silicon nitride composite ceramic powder and a preparation method thereof, so as to solve the above technical problems.
The invention provides the following technical scheme:
the aluminum nitride-doped modified nano silicon nitride composite ceramic powder comprises a component A and a component B, wherein the component A comprises the following components in parts by weight: 40-60 parts of aluminum powder and 100 parts of modified nano silicon nitride; the component B comprises the following components in parts by weight: 30 to 40 parts of aluminum powder, 20 to 80 parts of silicon powder, 5 to 10 parts of zirconium dioxide and 8 to 15 parts of yttrium oxide.
Preferably, the aluminum nitride doped modified nano silicon nitride composite ceramic powder comprises a component A and a component B, wherein the component A comprises the following components in parts by weight: 45 parts of aluminum powder and 100 parts of modified nano silicon nitride; the component B comprises the following components in parts by weight: 35 parts of aluminum powder, 60 parts of silicon powder, 8 parts of zirconium dioxide and 12 parts of yttrium oxide.
Preferably, in the component B, the particle sizes of the aluminum powder, the silicon powder, the zirconium dioxide and the yttrium oxide are all less than 10 microns.
Preferably, the preparation of the modified nano silicon nitride comprises the following steps:
adding nickel chloride into water to fully dissolve to prepare a nickel chloride solution with the concentration of 5%; pretreating silicon nitride powder, adding the pretreated silicon nitride powder into a nickel chloride solution, and fully stirring to obtain a uniformly mixed silicon nitride-nickel chloride suspension; slowly dripping the hydrazine solution into the silicon nitride-nickel chloride suspension, simultaneously dripping an ammonia water solution with the concentration of 10%, stopping dripping when the pH value reaches 9-10, keeping the pH value constant at 9-10, then raising the temperature to 70-85 ℃, stirring for 1-3 h with strong electromagnetism, stopping reaction, centrifugally separating, precipitating a product, repeatedly washing with deionized water and absolute ethyl alcohol, placing in a constant-temperature drying box at 60 ℃, and drying for 12h to prepare the modified nano silicon nitride.
More preferably, the pretreatment of the silicon nitride includes degreasing, roughening, sensitizing, and activating treatments.
More preferably, the mass volume ratio of the silicon nitride to the nickel chloride solution in the silicon nitride-nickel chloride suspension is 1g:30 mL-50 mL.
More preferably, the concentration of the hydrazine solution is 5-10%; the adding amount of the hydrazine solution is 20-35% of the volume of the silicon nitride-nickel chloride suspension.
The invention also aims to provide a preparation method of the aluminum nitride doped modified nano silicon nitride composite ceramic powder, which comprises the following steps:
step one, fully mixing the aluminum powder and the modified nano silicon nitride in the component A in parts by weight, placing the mixture in a nitrogen atmosphere, and reacting at 1200-2000 ℃ for 12-48 h to obtain a mixture A;
step two, fully mixing the aluminum powder, the silicon powder, the zirconium dioxide and the yttrium oxide in the component B by weight, placing the mixture in a nitrogen atmosphere, and reacting at 1500-2000 ℃ for 12-48 h to obtain a mixture B;
step three, mixing the mixture A obtained in the step one and the mixture B obtained in the step two through a planetary ball mill, then dispersing the mixture in a coating solution, performing ultrasonic dispersion for 3-5 hours, then adding a precipitator solution until the pH value is 8-9, and continuously stirring for 30-50 min to obtain ceramic slurry; and (3) dehydrating, drying and carrying out plasma sintering treatment on the obtained ceramic slurry to obtain the aluminum nitride doped modified nano silicon nitride composite ceramic powder.
Preferably, in the third step, the film coating solution is a yttrium nitrate-ethanol solution, and the addition amount of yttrium nitrate in the yttrium nitrate-ethanol solution is 5% -12%.
Preferably, in the third step, the precipitant solution is a triethylene diamine-acetone solution, and the addition amount of triethylene diamine in the triethylene diamine-acetone solution is 1% to 6%.
Preferably, the plasma sintering conditions are: the protective gas is nitrogen, the temperature is 1500-1800 ℃, the pressure is 20-50 MPa, and the time is 20-30 min.
According to the technical scheme, the invention has the beneficial effects that:
(1) the modified nano silicon nitride provided by the invention has an obvious modification effect, the nano nickel nitride is uniformly coated on the surface of the modified nano silicon nitride, the modified nano silicon nitride has good dispersibility and compatibility in the composite ceramic powder, and the modified nano silicon nitride can improve the wear resistance and corrosion resistance of the composite ceramic powder and also has good conductivity and ferromagnetism. The modified nano silicon nitride modification method is simple, safe and environment-friendly.
(2) The aluminum nitride-doped modified nano silicon nitride composite ceramic powder provided by the invention is coated with a layer of oxide containing a sintering aid through the film coating solution, so that the thermal conductivity and the surface mechanical strength of the ceramic composite powder can be improved. The aluminum nitride doped modified nano silicon nitride composite ceramic powder prepared by the invention has the advantages of uniform dispersion of all components, good oxidation resistance, high strength and fracture toughness.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. The exemplary embodiments and descriptions of the present invention are provided to explain the present invention, but not to limit the present invention.
Example 1
Aluminum nitride doped modified nano silicon nitride composite ceramic powder and preparation method thereof
The aluminum nitride-doped modified nano silicon nitride composite ceramic powder comprises a component A and a component B, wherein the component A comprises the following components in parts by weight: 40kg of aluminum powder and 100kg of modified nano silicon nitride; the component B comprises the following components in parts by weight: 30kg of aluminum powder, 20kg of silicon powder, 5kg of zirconium dioxide and 8kg of yttrium oxide. In the component B, the particle sizes of the aluminum powder, the silicon powder, the zirconium dioxide and the yttrium oxide are all less than 10 microns.
The preparation of the modified nano silicon nitride comprises the following steps:
adding nickel chloride into water to fully dissolve to prepare a nickel chloride solution with the concentration of 5%; pretreating silicon nitride powder, adding the pretreated silicon nitride powder into a nickel chloride solution, and fully stirring to obtain a uniformly mixed silicon nitride-nickel chloride suspension; slowly dripping the hydrazine solution into the silicon nitride-nickel chloride suspension, simultaneously dripping an ammonia water solution with the concentration of 10%, stopping dripping when the pH value reaches 9-10, keeping the pH value constant at 9, raising the temperature to 70 ℃, stirring for 1h with strong electromagnetism, stopping reaction, performing centrifugal separation, precipitating a product, repeatedly washing with deionized water and absolute ethyl alcohol, placing in a constant-temperature drying box at 60 ℃, and drying for 12h to obtain the modified nano silicon nitride.
The pretreatment of the silicon nitride comprises degreasing, coarsening, sensitizing and activating treatment; the mass volume ratio of silicon nitride to nickel chloride solution in the silicon nitride-nickel chloride suspension is 1g:30 mL; the concentration of the hydrazine solution is 5 percent; the hydrazine solution was added in an amount of 20% by volume based on the volume of the silicon nitride-nickel chloride suspension.
The preparation method of the aluminum nitride doped modified nano silicon nitride composite ceramic powder comprises the following steps:
step one, fully mixing the aluminum powder and the modified nano silicon nitride in the component A in parts by weight, placing the mixture in a nitrogen atmosphere, and reacting at 1200 ℃ for 12 hours to obtain a mixture A;
step two, fully mixing the aluminum powder, the silicon powder, the zirconium dioxide and the yttrium oxide in the component B by weight, placing the mixture in a nitrogen atmosphere, and reacting at 1500 ℃ for 12 hours to obtain a mixture B;
step three, mixing the mixture A obtained in the step one and the mixture B obtained in the step two through a planetary ball mill, then dispersing the mixture in a coating solution, performing ultrasonic dispersion for 3 hours, then adding a precipitator solution until the pH value is 8, and continuing stirring for 30min to obtain ceramic slurry; and (3) dehydrating and drying the obtained ceramic slurry, and carrying out plasma sintering treatment for 20min under the conditions of 1500 ℃ and 20MPa under the protection of nitrogen to obtain the aluminum nitride doped modified nano silicon nitride composite ceramic powder.
In the third step, the film coating solution is yttrium nitrate-ethanol solution, and the addition amount of yttrium nitrate in the yttrium nitrate-ethanol solution is 5%; the precipitant solution is triethylene diamine-acetone solution, and the addition amount of triethylene diamine in the triethylene diamine-acetone solution is 1%.
Example 2
Aluminum nitride doped modified nano silicon nitride composite ceramic powder and preparation method thereof
The aluminum nitride-doped modified nano silicon nitride composite ceramic powder comprises a component A and a component B, wherein the component A comprises the following components in parts by weight: 45kg of aluminum powder and 100kg of modified nano silicon nitride; the component B comprises the following components in parts by weight: 32kg of aluminum powder, 30kg of silicon powder, 6kg of zirconium dioxide and 10kg of yttrium oxide.
In the component B, the particle sizes of the aluminum powder, the silicon powder, the zirconium dioxide and the yttrium oxide are all less than 10 microns.
The preparation of the modified nano silicon nitride comprises the following steps:
adding nickel chloride into water to fully dissolve to prepare a nickel chloride solution with the concentration of 5%; pretreating silicon nitride powder, adding the pretreated silicon nitride powder into a nickel chloride solution, and fully stirring to obtain a uniformly mixed silicon nitride-nickel chloride suspension; slowly dripping hydrazine solution into the silicon nitride-nickel chloride suspension, simultaneously dripping 10% ammonia water solution, stopping dripping when the pH value reaches 9, keeping the pH value constant at 9, raising the temperature to 75 ℃, stirring with strong electromagnetism for 1.5h, stopping reaction, performing centrifugal separation, precipitating a product, repeatedly washing with deionized water and absolute ethyl alcohol, placing in a constant-temperature drying box at 60 ℃, and drying for 12h to obtain the modified nano silicon nitride.
The pretreatment of the silicon nitride comprises degreasing, coarsening, sensitizing and activating treatment; the mass volume ratio of silicon nitride to nickel chloride solution in the silicon nitride-nickel chloride suspension is 1g:35 mL; the concentration of the hydrazine solution is 6 percent; the hydrazine solution was added in an amount of 23% by volume based on the volume of the silicon nitride-nickel chloride suspension.
The preparation method of the aluminum nitride doped modified nano silicon nitride composite ceramic powder comprises the following steps:
step one, fully mixing the aluminum powder and the modified nano silicon nitride in the component A in parts by weight, placing the mixture in a nitrogen atmosphere, and reacting at 1500 ℃ for 18h to obtain a mixture A;
step two, fully mixing the aluminum powder, the silicon powder, the zirconium dioxide and the yttrium oxide in the component B by weight, placing the mixture in a nitrogen atmosphere, and reacting at 1700 ℃ for 20 hours to obtain a mixture B;
step three, mixing the mixture A obtained in the step one and the mixture B obtained in the step two through a planetary ball mill, then dispersing the mixture in a coating solution, performing ultrasonic dispersion for 3.5 hours, then adding a precipitator solution until the pH value is 8, and continuing stirring for 35min to obtain ceramic slurry; and (3) dehydrating and drying the obtained ceramic slurry, and carrying out plasma sintering treatment for 25min under the protection of nitrogen and at 1600 ℃ and 25MPa to obtain the aluminum nitride doped modified nano silicon nitride composite ceramic powder.
In the third step, the film coating solution is yttrium nitrate-ethanol solution, and the addition amount of yttrium nitrate in the yttrium nitrate-ethanol solution is 8%; the precipitant solution is a triethylene diamine-acetone solution, and the addition amount of triethylene diamine in the triethylene diamine-acetone solution is 3%.
Example 3
Aluminum nitride doped modified nano silicon nitride composite ceramic powder and preparation method thereof
The aluminum nitride-doped modified nano silicon nitride composite ceramic powder comprises a component A and a component B, wherein the component A comprises the following components in kg by weight: 45kg of aluminum powder and 100kg of modified nano silicon nitride; the component B comprises the following components in weight kg: 35kg of aluminum powder, 60kg of silicon powder, 8kg of zirconium dioxide and 12kg of yttrium oxide.
In the component B, the particle sizes of the aluminum powder, the silicon powder, the zirconium dioxide and the yttrium oxide are all less than 10 microns.
The preparation of the modified nano silicon nitride comprises the following steps:
adding nickel chloride into water to fully dissolve to prepare a nickel chloride solution with the concentration of 5%; pretreating silicon nitride powder, adding the pretreated silicon nitride powder into a nickel chloride solution, and fully stirring to obtain a uniformly mixed silicon nitride-nickel chloride suspension; slowly dripping hydrazine solution into the silicon nitride-nickel chloride suspension, simultaneously dripping 10% ammonia water solution, stopping dripping when the pH value reaches 10, keeping the pH value constant at 10, raising the temperature to 80 ℃, stirring for 2.5h with strong electromagnetism, stopping reaction, performing centrifugal separation, precipitating a product, repeatedly washing with deionized water and absolute ethyl alcohol, placing in a constant-temperature drying box at 60 ℃, and drying for 12h to obtain the modified nano silicon nitride.
The pretreatment of the silicon nitride comprises degreasing, coarsening, sensitizing and activating treatment; the mass volume ratio of silicon nitride to nickel chloride solution in the silicon nitride-nickel chloride suspension is 1g:35 mL; the concentration of the hydrazine solution is 6 percent; the hydrazine solution was added in an amount of 30% by volume of the silicon nitride-nickel chloride suspension.
The preparation method of the aluminum nitride doped modified nano silicon nitride composite ceramic powder comprises the following steps:
step one, fully mixing the aluminum powder and the modified nano silicon nitride in the component A in parts by weight, placing the mixture in a nitrogen atmosphere, and reacting at 1500 ℃ for 24 hours to obtain a mixture A;
step two, fully mixing the aluminum powder, the silicon powder, the zirconium dioxide and the yttrium oxide in the component B by weight, placing the mixture in a nitrogen atmosphere, and reacting at 1500 ℃ for 24 hours to obtain a mixture B;
step three, mixing the mixture A obtained in the step one and the mixture B obtained in the step two through a planetary ball mill, then dispersing the mixture in a coating solution, performing ultrasonic dispersion for 4 hours, then adding a precipitator solution until the pH value is 9, and continuing stirring for 40min to obtain ceramic slurry; and (3) dehydrating and drying the obtained ceramic slurry, and carrying out plasma sintering treatment for 30min under the protection of nitrogen and at 1600 ℃ and 30MPa to obtain the aluminum nitride doped modified nano silicon nitride composite ceramic powder.
In the third step, the film coating solution is yttrium nitrate-ethanol solution, and the addition amount of yttrium nitrate in the yttrium nitrate-ethanol solution is 9%; the precipitant solution is triethylene diamine-acetone solution, and the addition amount of triethylene diamine in the triethylene diamine-acetone solution is 4.5%.
Example 4
Aluminum nitride doped modified nano silicon nitride composite ceramic powder and preparation method thereof
The aluminum nitride-doped modified nano silicon nitride composite ceramic powder comprises a component A and a component B, wherein the component A comprises the following components in parts by weight: 55kg of aluminum powder and 100kg of modified nano silicon nitride; the component B comprises the following components in parts by weight: 38kg of aluminum powder, 70kg of silicon powder, 8kg of zirconium dioxide and 12kg of yttrium oxide.
In the component B, the particle sizes of the aluminum powder, the silicon powder, the zirconium dioxide and the yttrium oxide are all less than 10 microns.
The preparation of the modified nano silicon nitride comprises the following steps:
adding nickel chloride into water to fully dissolve to prepare a nickel chloride solution with the concentration of 5%; pretreating silicon nitride powder, adding the pretreated silicon nitride powder into a nickel chloride solution, and fully stirring to obtain a uniformly mixed silicon nitride-nickel chloride suspension; slowly dripping the hydrazine solution into the silicon nitride-nickel chloride suspension, simultaneously dripping an ammonia water solution with the concentration of 10%, stopping dripping when the pH value reaches 9-10, keeping the pH value constant at 10, raising the temperature to 8075 ℃, stirring for 2.5 hours by strong electromagnetism, stopping reaction, centrifugally separating, precipitating a product, repeatedly washing by deionized water and absolute ethyl alcohol, placing in a constant-temperature drying box at 60 ℃, and drying for 12 hours to prepare the modified nano silicon nitride.
The pretreatment of the silicon nitride comprises degreasing, coarsening, sensitizing and activating treatment; the mass volume ratio of silicon nitride to nickel chloride solution in the silicon nitride-nickel chloride suspension is 1g:40 mL; the concentration of the hydrazine solution is 5 to 10 percent; the hydrazine solution was added in an amount of 32% by volume of the silicon nitride-nickel chloride suspension.
The preparation method of the aluminum nitride doped modified nano silicon nitride composite ceramic powder comprises the following steps:
step one, fully mixing the aluminum powder and the modified nano silicon nitride in the component A in parts by weight, placing the mixture in a nitrogen atmosphere, and reacting at 1800 ℃ for 40 hours to obtain a mixture A;
step two, fully mixing the aluminum powder, the silicon powder, the zirconium dioxide and the yttrium oxide in the component B by weight, placing the mixture in a nitrogen atmosphere, and reacting at 1800 ℃ for 40h to obtain a mixture B;
step three, mixing the mixture A obtained in the step one and the mixture B obtained in the step two through a planetary ball mill, then dispersing the mixture in a coating solution, performing ultrasonic dispersion for 4.5 hours, then adding a precipitator solution until the pH value is 9, and continuing stirring for 45min to obtain ceramic slurry; and dehydrating and drying the obtained ceramic slurry, and carrying out plasma sintering treatment for 28min under the conditions of 1700 ℃ and 45MPa under the protection of nitrogen to obtain the aluminum nitride doped modified nano silicon nitride composite ceramic powder.
In the third step, the film coating solution is yttrium nitrate-ethanol solution, and the addition amount of yttrium nitrate in the yttrium nitrate-ethanol solution is 10%; the precipitant solution is triethylene diamine-acetone solution, and the addition amount of triethylene diamine in the triethylene diamine-acetone solution is 5%.
Example 5
Aluminum nitride doped modified nano silicon nitride composite ceramic powder and preparation method thereof
The aluminum nitride-doped modified nano silicon nitride composite ceramic powder comprises a component A and a component B, wherein the component A comprises the following components in parts by weight: 60kg of aluminum powder and 100kg of modified nano silicon nitride; the component B comprises the following components in parts by weight: 40kg of aluminum powder, 80kg of silicon powder, 10kg of zirconium dioxide and 15kg of yttrium oxide.
In the component B, the particle sizes of the aluminum powder, the silicon powder, the zirconium dioxide and the yttrium oxide are all less than 10 microns.
The preparation of the modified nano silicon nitride comprises the following steps:
adding nickel chloride into water to fully dissolve to prepare a nickel chloride solution with the concentration of 5%; pretreating silicon nitride powder, adding the pretreated silicon nitride powder into a nickel chloride solution, and fully stirring to obtain a uniformly mixed silicon nitride-nickel chloride suspension; slowly dripping the hydrazine solution into the silicon nitride-nickel chloride suspension, simultaneously dripping an ammonia water solution with the concentration of 10%, stopping dripping when the pH value reaches 9-10, keeping the pH value constant at 10, raising the temperature to 85 ℃, stirring for 3 hours by strong electromagnetism, stopping reaction, performing centrifugal separation, precipitating a product, repeatedly washing with deionized water and absolute ethyl alcohol, placing in a constant-temperature drying box at 60 ℃, and drying for 12 hours to obtain the modified nano silicon nitride.
The pretreatment of the silicon nitride comprises degreasing, coarsening, sensitizing and activating treatment; the mass volume ratio of silicon nitride to nickel chloride solution in the silicon nitride-nickel chloride suspension is 1g:50 mL; the concentration of the hydrazine solution is 10 percent; the hydrazine solution was added in an amount of 35% by volume of the silicon nitride-nickel chloride suspension.
The preparation method of the aluminum nitride doped modified nano silicon nitride composite ceramic powder comprises the following steps:
step one, fully mixing the aluminum powder and the modified nano silicon nitride in the component A in parts by weight, placing the mixture in a nitrogen atmosphere, and reacting for 48 hours at 2000 ℃ to obtain a mixture A;
step two, fully mixing the aluminum powder, the silicon powder, the zirconium dioxide and the yttrium oxide in the component B by weight, placing the mixture in a nitrogen atmosphere, and reacting for 48 hours at 2000 ℃ to obtain a mixture B;
step three, mixing the mixture A obtained in the step one and the mixture B obtained in the step two through a planetary ball mill, then dispersing the mixture in a coating solution, performing ultrasonic dispersion for 3 to 5 hours, then adding a precipitator solution until the pH value is 9, and continuously stirring the mixture for 30 to 50 minutes to obtain ceramic slurry; and dehydrating and drying the obtained ceramic slurry, and carrying out plasma sintering treatment for 30min under the conditions of 1800 ℃ and 50MPa under the protection of nitrogen to obtain the aluminum nitride doped modified nano silicon nitride composite ceramic powder.
In the third step, the film coating solution is yttrium nitrate-ethanol solution, and the addition amount of yttrium nitrate in the yttrium nitrate-ethanol solution is 12%; the precipitant solution is triethylene diamine-acetone solution, and the addition amount of triethylene diamine in the triethylene diamine-acetone solution is 6%.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and various modifications and variations of the embodiment of the present invention may occur to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The aluminum nitride-doped modified nano silicon nitride composite ceramic powder is characterized by comprising a component A and a component B, wherein the component A comprises the following components in parts by weight: 40-60 parts of aluminum powder and 100 parts of modified nano silicon nitride; the component B comprises the following components in parts by weight: 30 to 40 parts of aluminum powder, 20 to 80 parts of silicon powder, 5 to 10 parts of zirconium dioxide and 8 to 15 parts of yttrium oxide.
2. The aluminum nitride-doped modified nano silicon nitride composite ceramic powder of claim 1, wherein in the component B, the particle sizes of the aluminum powder, the silicon powder, the zirconium dioxide and the yttrium oxide are all less than 10 microns.
3. The aluminum nitride-doped modified nano silicon nitride composite ceramic powder according to claim 1, wherein the preparation of the modified nano silicon nitride comprises the following steps:
adding nickel chloride into water to fully dissolve to prepare a nickel chloride solution with the concentration of 5%; pretreating silicon nitride powder, adding the pretreated silicon nitride powder into a nickel chloride solution, and fully stirring to obtain a uniformly mixed silicon nitride-nickel chloride suspension; slowly dripping the hydrazine solution into the silicon nitride-nickel chloride suspension, simultaneously dripping an ammonia water solution with the concentration of 10%, stopping dripping when the pH value reaches 9-10, keeping the pH value constant at 9-10, then raising the temperature to 70-85 ℃, stirring for 1-3 h with strong electromagnetism, stopping reaction, centrifugally separating, precipitating a product, repeatedly washing with deionized water and absolute ethyl alcohol, placing in a constant-temperature drying box at 60 ℃, and drying for 12h to prepare the modified nano silicon nitride.
4. The aluminum nitride-doped modified nano silicon nitride composite ceramic powder of claim 3, wherein the pretreatment of the silicon nitride comprises degreasing, roughening, sensitizing and activating treatment.
5. The aluminum nitride-doped modified nano silicon nitride composite ceramic powder as claimed in claim 3, wherein the mass-to-volume ratio of silicon nitride to nickel chloride solution in the silicon nitride-nickel chloride suspension is 1g:30 mL-50 mL.
6. The aluminum nitride-doped modified nano silicon nitride composite ceramic powder according to claim 3, wherein the concentration of the hydrazine solution is 5-10%; the adding amount of the hydrazine solution is 20-35% of the volume of the silicon nitride-nickel chloride suspension.
7. The preparation method of the aluminum nitride-doped modified nano silicon nitride composite ceramic powder according to any one of claims 1 to 6, which is characterized by comprising the following steps of:
step one, fully mixing the aluminum powder and the modified nano silicon nitride in the component A in parts by weight, placing the mixture in a nitrogen atmosphere, and reacting at 1200-2000 ℃ for 12-48 h to obtain a mixture A;
step two, fully mixing the aluminum powder, the silicon powder, the zirconium dioxide and the yttrium oxide in the component B by weight, placing the mixture in a nitrogen atmosphere, and reacting at 1500-2000 ℃ for 12-48 h to obtain a mixture B;
step three, mixing the mixture A obtained in the step one and the mixture B obtained in the step two through a planetary ball mill, then dispersing the mixture in a coating solution, performing ultrasonic dispersion for 3-5 hours, then adding a precipitator solution until the pH value is 8-9, and continuously stirring for 30-50 min to obtain ceramic slurry; and (3) dehydrating, drying and carrying out plasma sintering treatment on the obtained ceramic slurry to obtain the aluminum nitride doped modified nano silicon nitride composite ceramic powder.
8. The method for preparing the aluminum nitride-doped modified nano silicon nitride composite ceramic powder according to claim 7, wherein in the third step, the film coating solution is yttrium nitrate-ethanol solution, and the addition amount of yttrium nitrate in the yttrium nitrate-ethanol solution is 5-12%.
9. The method for preparing aluminum nitride-doped modified nano silicon nitride composite ceramic powder according to claim 7, wherein in the third step, the precipitant solution is a triethylene diamine-acetone solution, and the addition amount of triethylene diamine in the triethylene diamine-acetone solution is 1-6%.
10. The method for preparing the aluminum nitride-doped modified nano silicon nitride composite ceramic powder according to claim 7, wherein the plasma sintering conditions are as follows: the protective gas is nitrogen, the temperature is 1500-1800 ℃, the pressure is 20-50 MPa, and the time is 20-30 min.
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