CN114149273A - Preparation method of alumina ceramic powder for electronic ceramics - Google Patents
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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)2O3) 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 the 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, and naturally recovering to room temperature for 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 butyl titanate to 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 a TiN phase which also contains relatively small amounts of Ti and TiO2The 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 the nitrogen gas introduced into the nitriding equipment in S3 is more than or equal to 99.9%, and the flow rate is 300-500 mL/min.
Further, 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% 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 ℃.
Further, in S4, the temperature rising speed is 15-25 ℃/min, and the temperature reducing 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 performance, good thermal shock resistance and can well improve the problem of alumina shrinkage in the sintering process, the mechanical property of the titanium nitride is improved to a certain extent, the titanium nitride core can be activated by low-temperature plasma technology treatment in preparation, so that the titanium nitride core is fully adhered with gel and the silicon carbide nano-wires in impregnation so as to improve the bonding strength, the alumina ceramic powder prepared by the invention has low shrinkage in the sintering process and can well keep the appearance integrity, as can be known from the above table 2, the alumina ceramic powder prepared by the invention has good mechanical property, the fracture toughness is more than or equal to 8.1, and the use requirement of the electronic ceramic can be completely met.
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, and naturally recovering to room temperature for 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, 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 the solution A into the solution B, stirring for 60min, dropwise adding the 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 percent and the flow rate 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 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 components in a mass ratio of 1.6: 1: adding 0.3 of aluminum nitrate, urea and silicon carbide nanowires into deionized water, stirring for 2h at 95 ℃ to obtain gel, adding the product, soaking for 5s at 40 ℃, taking out, drying for 5h at 90 ℃, heating to 1150 ℃ at a speed of 25 ℃/min, calcining for 10h, cooling to 750 ℃ at a speed of 5 ℃/min, annealing for 2h, naturally recovering to room temperature, and grinding to obtain 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 the solution A into the solution B, stirring for 60min, dropwise adding the 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 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 10s, and mixing the solution C with the reaction system in a 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 the 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, and naturally recovering to room temperature for 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 as claimed in 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 300-500 mL/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 alumina ceramic powder for electronic ceramics as claimed in claim 1, wherein the low temperature plasma technique in S3 is performed by introducing nitrogen with purity not less than 99.9%, removing air in the equipment and then turning on the power supply of the equipment, controlling the power of the equipment to be 800-.
7. The method for preparing the alumina ceramic powder for electronic ceramics according to claim 1, wherein the mass ratio of the aluminum nitrate, the urea and the silicon carbide nanowires in S4 is 1.4-1.6: 1: 0.3-0.5.
8. The method for preparing 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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Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5213591A (en) * | 1992-07-28 | 1993-05-25 | Ahmet Celikkaya | Abrasive grain, method of making same and abrasive products |
| CN1349950A (en) * | 2001-11-30 | 2002-05-22 | 中国科学院上海硅酸盐研究所 | Prepn of conductive composite nanometer titanium nitride-alumina material |
| CN1417163A (en) * | 2002-11-28 | 2003-05-14 | 中国科学院上海硅酸盐研究所 | Prepn of nano titanium nitride-silicon nitride composite material |
| WO2006120803A1 (en) * | 2005-05-10 | 2006-11-16 | Sumitomo Precision Products Co., Ltd | Highly thermally conductive composite material |
| CN101172852A (en) * | 2007-10-30 | 2008-05-07 | 景德镇陶瓷学院 | Method for producing aluminium titanates film by using colloidal sols-gel rubber technique |
| SE0702194L (en) * | 2007-09-26 | 2009-03-27 | Sandvik Intellectual Property | Coated cutting tool |
| CN104446396A (en) * | 2014-12-11 | 2015-03-25 | 中国石油大学(华东) | Preparation method of micro-nano composite aluminum oxide-titanium nitride-zirconium oxide-nickel-molybdenum ceramic material |
| CN104803695A (en) * | 2015-04-13 | 2015-07-29 | 安徽省含山瓷业股份有限公司 | High-strength carbon fiber enhanced boron nitride ceramic matrix composite and preparation method thereof |
| CN105367112A (en) * | 2015-11-19 | 2016-03-02 | 宁波科森净化器制造有限公司 | Vehicle exhaust purifier and preparation method thereof |
-
2021
- 2021-12-28 CN CN202111621235.9A patent/CN114149273B/en active Active
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5213591A (en) * | 1992-07-28 | 1993-05-25 | Ahmet Celikkaya | Abrasive grain, method of making same and abrasive products |
| CN1349950A (en) * | 2001-11-30 | 2002-05-22 | 中国科学院上海硅酸盐研究所 | Prepn of conductive composite nanometer titanium nitride-alumina material |
| CN1417163A (en) * | 2002-11-28 | 2003-05-14 | 中国科学院上海硅酸盐研究所 | Prepn of nano titanium nitride-silicon nitride composite material |
| WO2006120803A1 (en) * | 2005-05-10 | 2006-11-16 | Sumitomo Precision Products Co., Ltd | Highly thermally conductive composite material |
| SE0702194L (en) * | 2007-09-26 | 2009-03-27 | Sandvik Intellectual Property | Coated cutting tool |
| CN101172852A (en) * | 2007-10-30 | 2008-05-07 | 景德镇陶瓷学院 | Method for producing aluminium titanates film by using colloidal sols-gel rubber technique |
| CN104446396A (en) * | 2014-12-11 | 2015-03-25 | 中国石油大学(华东) | Preparation method of micro-nano composite aluminum oxide-titanium nitride-zirconium oxide-nickel-molybdenum ceramic material |
| CN104803695A (en) * | 2015-04-13 | 2015-07-29 | 安徽省含山瓷业股份有限公司 | High-strength carbon fiber enhanced boron nitride ceramic matrix composite and preparation method thereof |
| CN105367112A (en) * | 2015-11-19 | 2016-03-02 | 宁波科森净化器制造有限公司 | Vehicle exhaust purifier and preparation method thereof |
Non-Patent Citations (4)
| Title |
|---|
| CHOI, SW等: "Plasma enhanced atomic layer deposition of Al2O3 and TiN", 《JOURNAL OF THE KOREAN PHYSICAL SOCIETY》 * |
| 张丽红等: "优质超滤ZrO_2复合膜制备研究", 《化学工程师》 * |
| 方豪杰等: "烧结助剂对非等温烧结法制备氧化铝陶瓷微观结构和性能的影响", 《粉末冶金材料科学与工程》 * |
| 贡锡娜: "反应球磨法制备Ti（C，N）/Al2O3复合粉末及其烧结性能的研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
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