CN114149273B - Preparation method of alumina ceramic powder for electronic ceramics - Google Patents
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- CN114149273B CN114149273B CN202111621235.9A CN202111621235A CN114149273B CN 114149273 B CN114149273 B CN 114149273B CN 202111621235 A CN202111621235 A CN 202111621235A CN 114149273 B CN114149273 B CN 114149273B
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- 239000000843 powder Substances 0.000 title claims abstract description 40
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 239000000919 ceramic Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 238000010438 heat treatment Methods 0.000 claims abstract description 31
- 238000005121 nitriding Methods 0.000 claims abstract description 22
- 239000002243 precursor Substances 0.000 claims abstract description 18
- 238000001035 drying Methods 0.000 claims abstract description 16
- 238000000227 grinding Methods 0.000 claims abstract description 16
- 238000005516 engineering process Methods 0.000 claims abstract description 12
- 238000000137 annealing Methods 0.000 claims abstract description 10
- 238000001354 calcination Methods 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 238000002791 soaking Methods 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims description 47
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 31
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 24
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims description 23
- 239000006229 carbon black Substances 0.000 claims description 23
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 18
- 239000004202 carbamide Substances 0.000 claims description 18
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 16
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- 229910052757 nitrogen Inorganic materials 0.000 claims description 15
- 238000002156 mixing Methods 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 13
- 239000002070 nanowire Substances 0.000 claims description 13
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 13
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 13
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 229960000583 acetic acid Drugs 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 239000012362 glacial acetic acid Substances 0.000 claims description 8
- 239000004312 hexamethylene tetramine Substances 0.000 claims description 8
- 235000010299 hexamethylene tetramine Nutrition 0.000 claims description 8
- 229910052574 oxide ceramic Inorganic materials 0.000 claims description 8
- 239000011224 oxide ceramic Substances 0.000 claims description 8
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 8
- 238000005245 sintering Methods 0.000 claims description 7
- 238000005470 impregnation Methods 0.000 claims description 2
- 229910001873 dinitrogen Inorganic materials 0.000 claims 1
- 229910010293 ceramic material Inorganic materials 0.000 abstract description 4
- 230000000052 comparative effect Effects 0.000 description 7
- 238000010304 firing Methods 0.000 description 5
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 description 4
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 2
- 238000007598 dipping method Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000000877 morphologic effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000013001 point bending Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
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Abstract
The invention relates to the field of electronic ceramic materials, in particular to a preparation method of alumina ceramic powder for electronic ceramics, which comprises the steps of nitriding a precursor and then treating the precursor by using a low-temperature plasma technology; and adding the gel, soaking for 5-20s, taking out, drying at 80-90 ℃ for 5-10h, heating to 950-1200 ℃, calcining for 3-10h, cooling to 700-750 ℃, annealing for 2-2.5h, and naturally recovering to room temperature for grinding.
Description
Technical Field
The invention relates to the field of electronic ceramic materials, in particular to a preparation method of alumina ceramic powder for electronic ceramics.
Background
The electronic ceramic powder is the main raw material for manufacturing ceramic components, and the core requirements of the electronic ceramic powder are purity, particle size, shape and the like. The electronic ceramic powder is essentially different from common electric power ceramic in chemical components, microstructures and electromechanical properties. These differences are due to a series of special technical requirements of the electronics industry for electronic ceramics, the most important of which is to have high mechanical strength, high temperature and humidity resistance, radiation resistance, wide variation of dielectric constant, small dielectric loss tangent, high dielectric strength and insulation resistance, and excellent aging performance.
The alumina ceramic is prepared from alumina (Al) 2 O 3 ) The ceramic material used as the main body has better conductivity, mechanical strength and high temperature resistance, and is widely used as a ceramic with wide application, because of excellent thermal conductivity and conductivity, the ceramic material is also widely used as an electronic ceramic raw material in the electronic industry, and the shrinkage rate of the alumina ceramic powder in the high-end electronic industry field is higher during high-temperature sintering at present, so that the subsequent use is influenced.
Disclosure of Invention
The purpose of the invention is as follows: aiming at the defects or improvement requirements of the prior art, the invention provides a preparation method of alumina ceramic powder for electronic ceramics.
The technical scheme adopted by the invention is as follows:
a preparation method of alumina ceramic powder for electronic ceramics comprises the following steps:
s1: adding butyl titanate into absolute ethyl alcohol, uniformly stirring to obtain a solution A, mixing glacial acetic acid, the absolute ethyl alcohol and water, uniformly stirring to obtain a solution B, adding urea, hexamethylenetetramine and carbon black into the absolute ethyl alcohol, and uniformly stirring to obtain a solution C;
s2: dropwise adding the solution A into the solution B, stirring for 30-60min, dropwise adding the solution C into the reaction system, stirring for 30-60min, heating to 30-50 ℃, standing for 10-20h, heating to 70-80 ℃, drying for 10-20h, and grinding to obtain a precursor;
s3: placing the precursor in nitriding equipment, heating to 1100-1500 ℃, preserving heat for 6-10h, recovering room temperature to obtain a product after nitriding and sintering, and treating the product by using a low-temperature plasma technology;
s4: adding aluminum nitrate, urea and silicon carbide nanowires into deionized water, stirring for 2-5h at 90-95 ℃ to obtain gel, adding the product, soaking for 5-20s, taking out, drying for 5-10h at 80-90 ℃, heating to 950-1200 ℃, calcining for 3-10h, cooling to 700-750 ℃, annealing for 2-2.5h, naturally recovering to room temperature, and grinding to obtain the aluminum oxide ceramic powder.
Further, the mass ratio of the butyl titanate to the carbon black is 14-18:1.
further, the mass ratio of the butyl titanate to the carbon black is 15:1.
when the mass ratio of the butyl titanate to the carbon black is less than 14, the phase of the product after nitriding is relatively complicated, and when the mass ratio of the butyl titanate to the carbon black is 14-18, the phase of the product is mainly TiN phase, which also contains relatively small amounts of Ti and TiO 2 The mass ratio of the butyl titanate to the carbon black is 15:1, pure-phase TiN is obtained after nitridation, and when the mass ratio of the butyl titanate to the carbon black is more than 18, a mixed phase appears in the product, so that the mass ratio of the butyl titanate to the carbon black is preferably 14-18:1, more preferably 15:1.
furthermore, the purity of nitrogen introduced into the nitriding equipment in S3 is more than or equal to 99.9 percent, and the flow rate is 300-500mL/min.
Furthermore, the temperature rise speed of the nitriding equipment in S3 is 10-15 ℃/min.
Further, when the low-temperature plasma technology is used for processing in S3, firstly nitrogen with the purity of more than or equal to 99.9 percent is introduced, the power supply of the equipment is turned on after air in the equipment is removed, the power of the equipment is controlled to be 800-1000W, and the processing time is 5-10S.
Further, the mass ratio of the aluminum nitrate to the urea to the silicon carbide nanowires in the S4 is 1.4-1.6:1:0.3-0.5.
Further, the dipping temperature in S4 is 25-40 ℃.
Furthermore, the temperature rising speed in S4 is 15-25 ℃/min, and the temperature reduction speed is 5-10 ℃/min.
The invention has the beneficial effects that:
the invention provides a preparation method of alumina ceramic powder for electronic ceramics, which adopts titanium nitride as a core and alumina as a body structure, and utilizes silicon carbide nano-wires to toughen and modify the powder so as to enhance the structural strength between the core and the body, wherein the titanium nitride has high melting point, high strength, high hardness, high-temperature chemical stability, excellent electric conduction and heat conduction properties, and good thermal shock resistance, can well improve the problem of alumina shrinkage in a sintering process, and has certain improvement on the mechanical properties, and the titanium nitride core can be activated by low-temperature plasma technology treatment in preparation, so that the titanium nitride core is fully attached to gel and the silicon carbide nano-wires in impregnation so as to improve the bonding strength.
Drawings
FIG. 1 is a TEM image of the alumina ceramic powder prepared in example 1 of the present invention.
Detailed Description
The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
Example 1:
a preparation method of alumina ceramic powder for electronic ceramics comprises the following steps:
adding butyl titanate into absolute ethyl alcohol, uniformly stirring to obtain a solution A, mixing glacial acetic acid, the absolute ethyl alcohol and water, uniformly stirring to obtain a solution B, adding urea, hexamethylenetetramine and carbon black into the absolute ethyl alcohol, uniformly stirring to obtain a solution C, wherein the mass ratio of the butyl titanate to the carbon black is 15:1, dropwise adding the solution A into the solution B, stirring for 60min, dropwise adding the solution C into the reaction system, stirring for 60min, heating to 40 ℃, standing for 15h, heating to 70 ℃, drying for 15h, grinding to obtain a precursor, placing the precursor into nitriding equipment, introducing nitrogen with the purity of more than or equal to 99.9 percent and the flow rate of 500mL/min, heating to 1450 ℃ at the speed of 10 ℃/min, keeping the temperature for 8h, recovering the room temperature to obtain a product after nitriding and sintering, treating the product by using a low-temperature plasma technology, introducing nitrogen with the purity of more than or equal to 99.9 percent during treatment, removing air in the equipment, then turning on a power supply of the equipment, controlling the power of the equipment to be 1000W, treating for 10s, and mixing the solution C with the mass ratio of 1.4:1: adding 0.5 of aluminum nitrate, urea and silicon carbide nanowires into deionized water, stirring for 5h at 95 ℃ to obtain gel, adding the product, soaking for 10s at 30 ℃, taking out, drying for 10h at 90 ℃, heating to 1100 ℃ at a speed of 15 ℃/min, calcining for 5h, cooling to 720 ℃ at a speed of 5 ℃/min, annealing for 2.5h, naturally recovering to room temperature, and grinding to obtain the aluminum oxide ceramic powder.
Example 2:
a preparation method of alumina ceramic powder for electronic ceramics comprises the following steps:
adding butyl titanate into absolute ethyl alcohol, uniformly stirring to obtain a solution A, mixing glacial acetic acid, the absolute ethyl alcohol and water, uniformly stirring to obtain a solution B, adding urea, hexamethylenetetramine and carbon black into the absolute ethyl alcohol, uniformly stirring to obtain a solution C, wherein the mass ratio of the butyl titanate to the carbon black is 15:1, dropwise adding the solution A into the solution B, stirring for 50min, dropwise adding the solution C into the reaction system, stirring for 50min, heating to 30 ℃, standing for 20h, heating to 80 ℃, drying for 15h, grinding to obtain a precursor, placing the precursor into nitriding equipment, introducing nitrogen with the purity of more than or equal to 99.9 percent and the flow rate of 500mL/min, heating to 1500 ℃ at the speed of 15 ℃/min, keeping the temperature for 10h, recovering the room temperature to obtain a product after nitriding firing, treating the product by using a low-temperature plasma technology, introducing nitrogen with the purity of more than or equal to 99.9 percent during treatment, removing air in the equipment, then turning on a power supply of the equipment, controlling the power of the equipment to be 1000W, treating for 8s, and mixing the solution C and the solution C in a mass ratio of 1.6:1: adding 0.5 of aluminum nitrate, urea and silicon carbide nanowires into deionized water, stirring for 3h at 95 ℃ to obtain gel, adding the product, soaking for 20s at 40 ℃, taking out, drying for 10h at 90 ℃, heating to 1200 ℃ at a speed of 25 ℃/min, calcining for 8h, cooling to 720 ℃ at a speed of 10 ℃/min, annealing for 2.5h, and naturally recovering to room temperature for grinding to obtain the aluminum oxide ceramic powder.
Example 3:
a preparation method of alumina ceramic powder for electronic ceramics comprises the following steps:
adding butyl titanate into absolute ethyl alcohol, uniformly stirring to obtain a solution A, mixing glacial acetic acid, the absolute ethyl alcohol and water, uniformly stirring to obtain a solution B, adding urea, hexamethylenetetramine and carbon black into the absolute ethyl alcohol, and uniformly stirring to obtain a solution C, wherein the mass ratio of the butyl titanate to the carbon black is 15:1, dropwise adding the solution A into the solution B, stirring for 30min, dropwise adding the solution C into the reaction system, stirring for 60min, heating to 30 ℃, standing for 20h, heating to 70 ℃, drying for 20h, grinding to obtain a precursor, placing the precursor into nitriding equipment, introducing nitrogen with the purity of more than or equal to 99.9 percent and the flow rate of 300mL/min, heating to 1500 ℃ at the speed of 15 ℃/min, keeping the temperature for 10h, recovering the room temperature to obtain a product after nitriding firing, treating the product by using a low-temperature plasma technology, introducing nitrogen with the purity of more than or equal to 99.9 percent during treatment, removing air in the equipment, then turning on an equipment power supply, controlling the equipment power to be 800W, treating for 10s, and mixing the solutions in a mass ratio of 1.4:1: adding 0.5 of aluminum nitrate, urea and silicon carbide nanowires into deionized water, stirring for 5h at 90 ℃ to obtain gel, adding the product, soaking for 20s at 25 ℃, taking out, drying for 10h at 80 ℃, heating to 1200 ℃ at a speed of 15 ℃/min, calcining for 3h, cooling to 700 ℃ at a speed of 10 ℃/min, annealing for 2.5h, and naturally recovering to room temperature for grinding to obtain the aluminum oxide ceramic powder.
Example 4:
a preparation method of alumina ceramic powder for electronic ceramics comprises the following steps:
adding butyl titanate into absolute ethyl alcohol, uniformly stirring to obtain a solution A, mixing glacial acetic acid, the absolute ethyl alcohol and water, uniformly stirring to obtain a solution B, adding urea, hexamethylenetetramine and carbon black into the absolute ethyl alcohol, uniformly stirring to obtain a solution C, wherein the mass ratio of the butyl titanate to the carbon black is 15:1, dropwise adding a solution A into a solution B, stirring for 60min, dropwise adding a solution C into the reaction system, stirring for 30min, heating to 50 ℃, standing for 10h, heating to 80 ℃, drying for 10h, grinding to obtain a precursor, placing the precursor into nitriding equipment, introducing nitrogen with the purity of more than or equal to 99.9% and the flow of 500mL/min, heating to 1500 ℃ at the speed of 10 ℃/min, keeping the temperature for 6h, recovering the room temperature to obtain a product after nitriding firing, treating the product by using a low-temperature plasma technology, introducing nitrogen with the purity of more than or equal to 99.9% during treatment, removing air in the equipment, then turning on the power supply of the equipment, controlling the power of the equipment to be 1000W, treating for 5s, and mixing the solution C and the solution C in a mass ratio of 1.6:1:0.3 of aluminum nitrate, urea and silicon carbide nanowires are added into deionized water, stirring is carried out for 2h at 95 ℃ to obtain gel, the product is added, dipping is carried out for 5s at 40 ℃, then the product is taken out, drying is carried out for 5h at 90 ℃, then the temperature is raised to 1150 ℃ at the speed of 25 ℃/min for 10h, the product is cooled to 750 ℃ at the speed of 5 ℃/min for annealing for 2h, and then the product is naturally recovered to room temperature for grinding, thus obtaining the aluminum oxide ceramic powder.
Example 5:
a preparation method of alumina ceramic powder for electronic ceramics comprises the following steps:
adding butyl titanate into absolute ethyl alcohol, uniformly stirring to obtain a solution A, mixing glacial acetic acid, the absolute ethyl alcohol and water, uniformly stirring to obtain a solution B, adding urea, hexamethylenetetramine and carbon black into the absolute ethyl alcohol, uniformly stirring to obtain a solution C, wherein the mass ratio of the butyl titanate to the carbon black is 15:1, dropwise adding a solution A into a solution B, stirring for 60min, dropwise adding a solution C into the reaction system, stirring for 60min, heating to 50 ℃, standing for 20h, heating to 80 ℃, drying for 20h, grinding to obtain a precursor, placing the precursor into nitriding equipment, introducing nitrogen with the purity of more than or equal to 99.9% and the flow of 500mL/min, heating to 1500 ℃ at the speed of 15 ℃/min, keeping the temperature for 10h, recovering the room temperature to obtain a product after nitriding firing, treating the product by using a low-temperature plasma technology, introducing nitrogen with the purity of more than or equal to 99.9% during treatment, removing air in the equipment, then turning on the power supply of the equipment, controlling the power of the equipment to be 1000W, treating for 10s, and mixing the solution C with the reaction system according to the mass ratio of 1.6:1: adding 0.5 of aluminum nitrate, urea and silicon carbide nanowires into deionized water, stirring for 5h at 95 ℃ to obtain gel, adding the product, soaking for 20s at 40 ℃, taking out, drying for 10h at 90 ℃, heating to 1200 ℃ at a speed of 25 ℃/min, calcining for 10h, cooling to 750 ℃ at a speed of 10 ℃/min, annealing for 2.5h, and naturally recovering to room temperature for grinding to obtain the aluminum oxide ceramic powder.
Example 6
A preparation method of alumina ceramic powder for electronic ceramics comprises the following steps:
adding butyl titanate into absolute ethyl alcohol, uniformly stirring to obtain a solution A, mixing glacial acetic acid, the absolute ethyl alcohol and water, uniformly stirring to obtain a solution B, adding urea, hexamethylenetetramine and carbon black into the absolute ethyl alcohol, uniformly stirring to obtain a solution C, wherein the mass ratio of the butyl titanate to the carbon black is 15:1, dropwise adding the solution A into the solution B, stirring for 50min, dropwise adding the solution C into the reaction system, stirring for 50min, heating to 50 ℃, standing for 15h, heating to 80 ℃, drying for 10h, grinding to obtain a precursor, placing the precursor into nitriding equipment, introducing nitrogen with the purity of more than or equal to 99.9 percent and the flow rate of 400mL/min, heating to 1400 ℃ at the speed of 12 ℃/min, preserving heat for 10h, recovering the room temperature to obtain a product after nitriding firing, treating the product by using a low-temperature plasma technology, introducing nitrogen with the purity of more than or equal to 99.9 percent during treatment, removing air in the equipment, then turning on an equipment power supply, controlling the equipment power to be 1000W, treating for 5s, and mixing the solutions in a mass ratio of 1.4:1:0.4 of aluminum nitrate, urea and silicon carbide nanowires are added into deionized water, the mixture is stirred for 5 hours at the temperature of 95 ℃ to obtain gel, the gel is added, the gel is soaked for 20 seconds at the temperature of 40 ℃ and then taken out, the gel is dried for 10 hours at the temperature of 85 ℃, then the temperature is increased to 1200 ℃ at the speed of 25 ℃/min and calcined for 8 hours, the temperature is reduced to 700 ℃ at the speed of 10 ℃/min, annealing is carried out for 2 hours, and then the room temperature is naturally recovered and ground, so that the aluminum oxide ceramic powder can be obtained.
Comparative example 1
Comparative example 1 is essentially the same as example 1 except that the product was not subjected to low temperature plasma techniques.
Comparative example 2
Comparative example 2 is substantially the same as example 1 except that the silicon carbide nanowires were not added.
Comparative example 3
Comparative example 3 is substantially the same as example 1 except that no annealing treatment was performed.
And (3) performance testing:
10g of each of the alumina ceramic powders prepared in examples 1 to 6 and comparative examples 1 to 3 and a commercial nano alumina powder (manufacturer: xuancheng crystal new material) were dried at 105 ℃ for 4 hours, pressed at 100MPa into green sheets having a diameter of 98mm × 21mm × 0.63mm, and then sintered at 1580 ℃ for 2 hours, and the shrinkage after sintering was measured, and the results are shown in the following table 1:
table 1:
the three-point bending method is adopted to measure the flexural strength of the blank sheet, the loading rate is 0.5mm/min, the unilateral incision method is adopted to measure the fracture toughness of the blank sheet, and the results are shown in the following table 2:
table 2:
as can be seen from the above Table 1, the alumina ceramic powder prepared by the invention has low shrinkage rate in the sintering process, and can well maintain the morphological integrity, and as can be seen from the above Table 2, the alumina ceramic powder prepared by the invention has good mechanical properties, the breaking strength is more than or equal to 515MPa, and the fracture toughness is more than or equal to 8.1.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (9)
1. A preparation method of alumina ceramic powder for electronic ceramics is characterized by comprising the following steps:
s1: adding butyl titanate into absolute ethyl alcohol, uniformly stirring to obtain a solution A, mixing glacial acetic acid, the absolute ethyl alcohol and water, uniformly stirring to obtain a solution B, adding urea, hexamethylenetetramine and carbon black into the absolute ethyl alcohol, and uniformly stirring to obtain a solution C;
s2: dropwise adding the solution A into the solution B, stirring for 30-60min, dropwise adding the solution C into the reaction system, stirring for 30-60min, heating to 30-50 ℃, standing for 10-20h, heating to 70-80 ℃, drying for 10-20h, and grinding to obtain a precursor;
s3: placing the precursor in nitriding equipment, heating to 1100-1500 ℃, preserving heat for 6-10h, recovering room temperature to obtain a product after nitriding and sintering, and treating the product by using a low-temperature plasma technology;
s4: adding aluminum nitrate, urea and silicon carbide nanowires into deionized water, stirring for 2-5h at 90-95 ℃ to obtain gel, adding the product, soaking for 5-20s, taking out, drying for 5-10h at 80-90 ℃, heating to 950-1200 ℃, calcining for 3-10h, cooling to 700-750 ℃, annealing for 2-2.5h, naturally recovering to room temperature, and grinding to obtain the aluminum oxide ceramic powder.
2. The method for preparing the alumina ceramic powder for electronic ceramics according to claim 1, wherein the mass ratio of the butyl titanate to the carbon black is 14-18:1.
3. the method for preparing the alumina ceramic powder for electronic ceramics according to claim 2, wherein the mass ratio of the butyl titanate to the carbon black is 15:1.
4. the method for preparing alumina ceramic powder for electronic ceramics according to claim 1, wherein the purity of nitrogen gas introduced into the nitriding equipment in S3 is not less than 99.9%, and the flow rate is 300-500mL/min.
5. The method for preparing alumina ceramic powder for electronic ceramics according to claim 1, wherein the temperature rise rate of the nitriding device in S3 is 10 to 15 ℃/min.
6. The method for preparing the alumina ceramic powder for electronic ceramics according to claim 1, wherein in the step of low temperature plasma technology treatment in S3, nitrogen with the purity of more than or equal to 99.9 percent is firstly introduced, the power supply of the equipment is turned on after air in the equipment is removed, the power of the equipment is controlled to be 800-1000W, and the treatment time is 5-10S.
7. The method for preparing the alumina ceramic powder for electronic ceramics according to claim 1, wherein the mass ratio of the aluminum nitrate to the urea to the silicon carbide nanowires in S4 is 1.4-1.6:1:0.3-0.5.
8. The method for preparing the alumina ceramic powder for electronic ceramics according to claim 1, wherein the impregnation temperature in S4 is 25 to 40 ℃.
9. The method for preparing alumina ceramic powder for electronic ceramics according to claim 1, wherein the temperature rise rate in S4 is 15 to 25 ℃/min and the temperature drop rate is 5 to 10 ℃/min.
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