WO2017079878A1 - Method for preparing composite powder of aluminium oxide and aluminium nitride - Google Patents

Method for preparing composite powder of aluminium oxide and aluminium nitride Download PDF

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WO2017079878A1
WO2017079878A1 PCT/CN2015/094138 CN2015094138W WO2017079878A1 WO 2017079878 A1 WO2017079878 A1 WO 2017079878A1 CN 2015094138 W CN2015094138 W CN 2015094138W WO 2017079878 A1 WO2017079878 A1 WO 2017079878A1
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powder
alumina
aluminum nitride
composite powder
carbon
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PCT/CN2015/094138
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张甘霖
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深圳市博世知识产权运营有限公司
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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
    • C04B35/111—Fine ceramics
    • C04B35/117—Composites
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B

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  • the present invention relates to the field of composite powder manufacturing, and in particular to a method for producing an aluminum oxide or aluminum nitride composite powder.
  • the mixed powder of alumina and aluminum nitride is of great value as a raw material of alumina-aluminum nitride composite ceramic material, alumina-aluminum nitride-aluminum oxynitride composite ceramic material, and aluminum oxynitride transparent ceramic material.
  • the alumina-aluminum nitride composite ceramic has good thermal conductivity under the condition of controlling the content of aluminum nitride, and can be used in the field of high thermal conductivity and expansion coefficient, such as heat dissipation of LED lamps.
  • the aluminum oxynitride transparent ceramic has good optical properties and mechanical properties, and has important national defense value as an armor material.
  • the mixed powder obtained by this method is not highly active in the subsequent sintering into a ceramic, and it is difficult to obtain a high quality ceramic.
  • Another way is to nitride the nano-alumina powder and the nano-carbon powder in nitrogen to obtain a composite powder of aluminum oxide and aluminum nitride.
  • the raw material of this method is readily available, and the obtained composite powder of alumina and aluminum nitride is also more favorable for sintering.
  • this method has the disadvantage that the degree of reaction is susceptible to reaction conditions such as nitrogen pressure and flow rate, reaction temperature and reaction time, alumina powder and particle size of carbon powder. Therefore, it is difficult to control the content of aluminum nitride.
  • the present invention provides a method for producing an alumina or aluminum nitride composite powder which can accurately control the aluminum nitride content.
  • a method for producing an alumina or aluminum nitride composite powder wherein the alumina and aluminum nitride composite powder are obtained by oxidizing a mixed powder of alumina and carbon powder in flowing nitrogen gas and then oxidizing.
  • the nano-alumina powder has a particle diameter of 50 to 500 nm, preferably 50 to 100 nm.
  • the nanocarbon powder has a particle diameter of 50 to 500 nm, preferably 50 to 200 nm.
  • the nano-alumina powder with mass Mo is weighed and mixed with a certain amount of nano-carbon powder.
  • the mixed powder is placed in flowing nitrogen at 1100 ° C - 1500 ° C for 4-6 hours to obtain oxidation of residual carbon.
  • the mixed powder of the carbon-containing alumina and aluminum nitride is heated to 500 ° C - 700 ° C in air and kept for 3-5 hours to obtain a mixed powder of carbon-free alumina and aluminum nitride. And weigh out its quality as M.
  • the content of aluminum nitride in the mixed powder was 4.1 ⁇ (Mo-M)/M ⁇ 100%.
  • the aluminum nitride aluminum nitride composite powder having an aluminum nitride mass content of w (w ⁇ 4.1 ⁇ (Mo-M)/M ⁇ 100%) is preliminarily obtained, the above aluminum nitride content may be 4.1 ⁇ (Mo-M).
  • the /M ⁇ 100% mixed powder was obtained by uniformly mixing with 4.1 ⁇ (Mo-M)/wM alumina.
  • the method of the present invention is simple and does not require strict control of the reaction conditions. It is also possible to obtain a highly reactive alumina aluminum nitride composite powder without expensive imported aluminum nitride powder. Further, any powder having an aluminum nitride content of between 0% and 100% can be obtained by controlling the nitriding reaction conditions.
  • the mass of the nano-alumina powder weighed is represented by Mo
  • the mass of the mixed powder of the obtained carbon-free alumina and aluminum nitride is represented by M
  • w represents the mass content of the pre-obtained aluminum nitride.
  • 500 g of the alumina powder having a particle diameter of 100 nm was uniformly mixed with carbon having a particle diameter of 200 nm, wherein the mass percentage of the carbon powder was 10%.
  • the obtained mixed powder was kept at 1200 ° C for 4 hours in flowing nitrogen gas to obtain a mixed powder of alumina and aluminum nitride containing residual carbon.
  • the mixed powder was kept in air at 500 ° C for 5 hours to obtain a mixed powder of alumina and aluminum nitride, and the mass was 480 g. According to 4.1 ⁇ (Mo-M)/M ⁇ 100%, the content of aluminum nitride was 17.08%.
  • 500 g of the alumina powder having a particle diameter of 200 nm was uniformly mixed with carbon having a particle diameter of 100 nm, wherein the mass percentage of the carbon powder was 20%.
  • the obtained mixed powder was kept at 1200 ° C for 5 hours in flowing nitrogen to obtain a mixed powder of alumina and aluminum nitride containing residual carbon.
  • the mixed powder was kept in air at 600 ° C for 5 hours to obtain a mixed powder of alumina and aluminum nitride, and the mass was 450 g. According to 4.1 ⁇ (Mo-M)/M ⁇ 100%, the content of aluminum nitride was 41%.
  • the powder is uniformly mixed with 183 g of the 200 nm alumina powder according to 4.1 ⁇ (Mo-M)/wM. Available.
  • alumina powder having a particle diameter of 50 nm was uniformly mixed with carbon having a particle diameter of 50 nm, wherein the mass percentage of the carbon powder was 30%.
  • the obtained mixed powder was kept at 1300 ° C for 6 hours in flowing nitrogen to obtain a mixed powder of alumina and aluminum nitride containing residual carbon.
  • This mixed powder was kept in air at 600 ° C for 5 hours to obtain a mixed powder of alumina and aluminum nitride, and the mass was 400 g. According to 4.1 ⁇ (Mo-M)/M ⁇ 100%, the content of aluminum nitride was 82%.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Composite Materials (AREA)
  • Inorganic Chemistry (AREA)
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Abstract

Provided is a method for preparing a composite powder of aluminium oxide and aluminium nitride. The composite powder of aluminium oxide and aluminium nitride is prepared by means of incubation of a powder mixture consisting of aluminium oxide and a carbon powder in flowing nitrogen and then oxidation of the powder mixture. The method is simple and does not require strict control on reaction conditions. By means of the method, a highly reactive composite powder of aluminium oxide and aluminium nitride can be prepared without an expensive imported aluminium nitride powder. Moreover, any powder with the aluminium nitride content being 0%-100% can further be prepared by controlling the reaction conditions of carbonization and nitridation.

Description

一种氧化铝、氮化铝复合粉体的制造方法Method for producing alumina and aluminum nitride composite powder 技术领域Technical field
本发明涉及复合粉体制造领域，具体地说是涉及一种氧化铝、氮化铝复合粉体的制造方法。The present invention relates to the field of composite powder manufacturing, and in particular to a method for producing an aluminum oxide or aluminum nitride composite powder.
背景技术Background technique
氧化铝和氮化铝的混合粉体作为氧化铝-氮化铝复合陶瓷材料、氧化铝-氮化铝-氧氮化铝复合陶瓷材料以及氧氮化铝透明陶瓷材料的原材料具有重要价值。其中氧化铝-氮化铝复合陶瓷在控制适量的氮化铝的含量的情况下具有良好的热导率，可以用在对热导率和膨胀系数有较高要求的领域如作为LED灯的散热基板。而氧氮化铝透明陶瓷则兼具良好的光学性能和力学性能，作为装甲材料具有重要国防价值。获得此种复合粉体的最直接的方法是将氧化铝和氮化铝按所需的比例混合。然而此种方法对于原材料粉体特别是其中的氮化铝粉体在纯度上有较高的要求。而高纯度的氮化铝粉体不仅价格昂贵，而且需要进口。The mixed powder of alumina and aluminum nitride is of great value as a raw material of alumina-aluminum nitride composite ceramic material, alumina-aluminum nitride-aluminum oxynitride composite ceramic material, and aluminum oxynitride transparent ceramic material. Among them, the alumina-aluminum nitride composite ceramic has good thermal conductivity under the condition of controlling the content of aluminum nitride, and can be used in the field of high thermal conductivity and expansion coefficient, such as heat dissipation of LED lamps. Substrate. The aluminum oxynitride transparent ceramic has good optical properties and mechanical properties, and has important national defense value as an armor material. The most straightforward way to obtain such a composite powder is to mix alumina and aluminum nitride in the desired ratio. However, this method has high requirements on the purity of the raw material powder, especially the aluminum nitride powder therein. High-purity aluminum nitride powder is not only expensive but also requires import.
此外，此种方法获得的混合粉体在后续的烧结成陶瓷过程中活性不高，难以得到高质量的陶瓷。另一种方式是将纳米氧化铝粉体与纳米碳粉在氮气中氮化得到氧化铝和氮化铝的复合粉体。此种方法原料易得，获得的氧化铝和氮化铝的复合粉体也更有利于烧结。然而，此方法的缺点是反应程度易受反应条件如氮气的压力和流速、反应温度及反应的时间、氧化铝粉和碳粉的粒径大小等影响。因此，难以控制氮化铝的含量。Further, the mixed powder obtained by this method is not highly active in the subsequent sintering into a ceramic, and it is difficult to obtain a high quality ceramic. Another way is to nitride the nano-alumina powder and the nano-carbon powder in nitrogen to obtain a composite powder of aluminum oxide and aluminum nitride. The raw material of this method is readily available, and the obtained composite powder of alumina and aluminum nitride is also more favorable for sintering. However, this method has the disadvantage that the degree of reaction is susceptible to reaction conditions such as nitrogen pressure and flow rate, reaction temperature and reaction time, alumina powder and particle size of carbon powder. Therefore, it is difficult to control the content of aluminum nitride.
发明内容Summary of the invention
鉴于现有技术存在的不足，本发明提供了一种可以精确控制氮化铝含量的氧化铝、氮化铝复合粉体的制造方法。In view of the deficiencies of the prior art, the present invention provides a method for producing an alumina or aluminum nitride composite powder which can accurately control the aluminum nitride content.
为了实现上述的目的，本发明采用了如下的技术方案：In order to achieve the above object, the present invention adopts the following technical solutions:
一种氧化铝、氮化铝复合粉体的制造方法，所述的氧化铝、氮化铝复合粉体由氧化铝和碳粉的混合粉体在流动的氮气中保温后氧化后制得。 A method for producing an alumina or aluminum nitride composite powder, wherein the alumina and aluminum nitride composite powder are obtained by oxidizing a mixed powder of alumina and carbon powder in flowing nitrogen gas and then oxidizing.
所述的纳米氧化铝粉体的粒径为50-500nm，最好为50-100纳米。The nano-alumina powder has a particle diameter of 50 to 500 nm, preferably 50 to 100 nm.
所述的纳米碳粉的粒径为50-500nm，最好为50-200纳米。The nanocarbon powder has a particle diameter of 50 to 500 nm, preferably 50 to 200 nm.
秤取质量为Mo的纳米氧化铝粉，并与一定质量的纳米碳粉混合均匀，均混合粉体置于流动的氮气中在1100℃-1500℃保温4-6小时，得含有余碳的氧化铝和氮化铝的混合粉体。The nano-alumina powder with mass Mo is weighed and mixed with a certain amount of nano-carbon powder. The mixed powder is placed in flowing nitrogen at 1100 ° C - 1500 ° C for 4-6 hours to obtain oxidation of residual carbon. A mixed powder of aluminum and aluminum nitride.
将所述的含有余碳的氧化铝和氮化铝的混合粉体在空气中加热至500℃-700℃并保温3-5小时，得到不含碳的氧化铝和氮化铝的混合粉体，并秤出其质量为M。该混合粉体中氮化铝的含量为4.1·(Mo-M)/M·100％。The mixed powder of the carbon-containing alumina and aluminum nitride is heated to 500 ° C - 700 ° C in air and kept for 3-5 hours to obtain a mixed powder of carbon-free alumina and aluminum nitride. And weigh out its quality as M. The content of aluminum nitride in the mixed powder was 4.1·(Mo-M)/M·100%.
若预获得氮化铝质量含量为w(w<4.1·(Mo-M)/M·100％)的氧化铝氮化铝复合粉，可将上述氮化铝含量为4.1·(Mo-M)/M·100％的混合粉体与4.1·(Mo-M)/w-M的氧化铝混合均匀后获得。If the aluminum nitride aluminum nitride composite powder having an aluminum nitride mass content of w (w<4.1·(Mo-M)/M·100%) is preliminarily obtained, the above aluminum nitride content may be 4.1·(Mo-M). The /M·100% mixed powder was obtained by uniformly mixing with 4.1·(Mo-M)/wM alumina.
本发明所述的方法简易，无需严格控制反应条件。也无需昂贵的进口的氮化铝粉体，即可制得具有良好反应活性的氧化铝氮化铝复合粉体。此外，还可以通过控制碳化氮化反应条件制得氮化铝含量在0％-100％之间的任何粉体。The method of the present invention is simple and does not require strict control of the reaction conditions. It is also possible to obtain a highly reactive alumina aluminum nitride composite powder without expensive imported aluminum nitride powder. Further, any powder having an aluminum nitride content of between 0% and 100% can be obtained by controlling the nitriding reaction conditions.
具体实施方式detailed description
为了使本发明的目的、技术方案及优点更加清楚明白，以下结合附图及实施例，对本发明进一步详细说明。应当理解，此处所描述的具体实施例仅仅用以解释本发明，并不用于限定本发明。The present invention will be further described in detail below with reference to the accompanying drawings and embodiments. It is understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
一下实施例中，以Mo表示秤取的纳米氧化铝粉的质量，以M表示得到的不含碳的氧化铝和氮化铝的混合粉体的质量，w表示预获得氮化铝质量含量。In the following examples, the mass of the nano-alumina powder weighed is represented by Mo, the mass of the mixed powder of the obtained carbon-free alumina and aluminum nitride is represented by M, and w represents the mass content of the pre-obtained aluminum nitride.
实施例1Example 1
将粒径为100nm的500g氧化铝粉体与粒径为200nm的碳混合均匀，其中碳粉的质量百分比为10％。将所得到的混合粉体在流动氮气中在1200℃保温4小时，得含有余碳的氧化铝和氮化铝混合粉体。将此混合粉体在500℃的空气中保温5小时，得氧化铝和氮化铝的混合粉体，质量为480g。根据4.1·(Mo-M)/M·100％可知，氮化铝的含量为17.08％。若预获得氮化铝含量为10％的氧化铝氮化铝混合粉体，则根据4.1·(Mo-M)/w-M可知，将上述粉体与320g的100nm的氧化铝粉体混合均匀后即可获得。500 g of the alumina powder having a particle diameter of 100 nm was uniformly mixed with carbon having a particle diameter of 200 nm, wherein the mass percentage of the carbon powder was 10%. The obtained mixed powder was kept at 1200 ° C for 4 hours in flowing nitrogen gas to obtain a mixed powder of alumina and aluminum nitride containing residual carbon. The mixed powder was kept in air at 500 ° C for 5 hours to obtain a mixed powder of alumina and aluminum nitride, and the mass was 480 g. According to 4.1·(Mo-M)/M·100%, the content of aluminum nitride was 17.08%. When the alumina aluminum nitride mixed powder having an aluminum nitride content of 10% is obtained in advance, it is understood that the powder is uniformly mixed with 320 g of the 100 nm alumina powder according to 4.1·(Mo-M)/wM. Available.
实施例2 Example 2
将粒径为200nm的500g氧化铝粉体与粒径为100nm的碳混合均匀，其中碳粉的质量百分比为20％。将所得到的混合粉体在流动氮气中在1200℃保温5小时，得含有余碳的氧化铝和氮化铝混合粉体。将此混合粉体在600℃的空气中保温5小时，得氧化铝和氮化铝的混合粉体，质量为450g。根据4.1·(Mo-M)/M·100％可知，氮化铝的含量为41％。若预获得氮化铝含量为30％的氧化铝氮化铝混合粉体，则根据4.1·(Mo-M)/w-M可知，将上述粉体与183g的200nm的氧化铝粉体混合均匀后即可获得。500 g of the alumina powder having a particle diameter of 200 nm was uniformly mixed with carbon having a particle diameter of 100 nm, wherein the mass percentage of the carbon powder was 20%. The obtained mixed powder was kept at 1200 ° C for 5 hours in flowing nitrogen to obtain a mixed powder of alumina and aluminum nitride containing residual carbon. The mixed powder was kept in air at 600 ° C for 5 hours to obtain a mixed powder of alumina and aluminum nitride, and the mass was 450 g. According to 4.1·(Mo-M)/M·100%, the content of aluminum nitride was 41%. When the alumina aluminum nitride mixed powder having an aluminum nitride content of 30% is obtained in advance, it is understood that the powder is uniformly mixed with 183 g of the 200 nm alumina powder according to 4.1·(Mo-M)/wM. Available.
实施例3Example 3
将粒径为50nm的500g氧化铝粉体与粒径为50nm的碳混合均匀，其中碳粉的质量百分比为30％。将所得到的混合粉体在流动氮气中在1300℃保温6小时，得含有余碳的氧化铝和氮化铝混合粉体。将此混合粉体在600℃的空气中保温5小时，得氧化铝和氮化铝的混合粉体，质量为400g。根据4.1·(Mo-M)/M·100％可知，氮化铝的含量为82％。若预获得氮化铝含量为50％的氧化铝氮化铝混合粉体，则根据4.1·(Mo-M)/w-M可知，将上述粉体与320g的50nm的氧化铝粉体混合均匀后即可获得。500 g of alumina powder having a particle diameter of 50 nm was uniformly mixed with carbon having a particle diameter of 50 nm, wherein the mass percentage of the carbon powder was 30%. The obtained mixed powder was kept at 1300 ° C for 6 hours in flowing nitrogen to obtain a mixed powder of alumina and aluminum nitride containing residual carbon. This mixed powder was kept in air at 600 ° C for 5 hours to obtain a mixed powder of alumina and aluminum nitride, and the mass was 400 g. According to 4.1·(Mo-M)/M·100%, the content of aluminum nitride was 82%. When aluminum alumina aluminum nitride mixed powder having an aluminum nitride content of 50% is obtained in advance, it is understood that the powder is uniformly mixed with 320 g of 50 nm alumina powder according to 4.1·(Mo-M)/wM. Available.
以上所述仅是本申请的具体实施方式，应当指出，对于本技术领域的普通技术人员来说，在不脱离本申请原理的前提下，还可以做出若干改进和润饰，这些改进和润饰也应视为本申请的保护范围。 The above description is only a specific embodiment of the present application, and it should be noted that those skilled in the art can also make several improvements and retouchings without departing from the principles of the present application. It should be considered as the scope of protection of this application.

Claims (7)

  1. 一种氧化铝、氮化铝复合粉体的制造方法，其中，所述的氧化铝、氮化铝复合粉体由氧化铝和碳粉的混合粉体在流动的氮气中保温后氧化后制得。The invention relates to a method for producing an aluminum oxide and aluminum nitride composite powder, wherein the aluminum oxide and aluminum nitride composite powder are prepared by oxidizing a mixed powder of alumina and carbon powder in flowing nitrogen gas and then oxidizing .
  2. 根据权利要求1所述的氧化铝、氮化铝复合粉体的制造方法，其中，所述氧化铝和碳粉的混合粉体的保温温度为1100℃-1500℃。The method for producing an alumina or aluminum nitride composite powder according to claim 1, wherein the mixed powder of the alumina and the carbon powder has a temperature of from 1100 ° C to 1500 ° C.
  3. 根据权利要求2所述的氧化铝、氮化铝复合粉体的制造方法，其中，所述氧化铝和碳粉的混合粉体的保温时间为4-6小时，制得不含碳的氧化铝、氮化铝复合粉体。The method for producing an alumina or aluminum nitride composite powder according to claim 2, wherein the mixed powder of the alumina and the carbon powder is kept for 4 to 6 hours to obtain a carbon-free alumina. , aluminum nitride composite powder.
  4. 根据权利要求1所述的氧化铝、氮化铝复合粉体的制造方法，其中，保温后的氧化温度为500-600℃。The method for producing an alumina or aluminum nitride composite powder according to claim 1, wherein the oxidation temperature after the heat retention is 500 to 600 °C.
  5. 根据权利要求4所述的氧化铝、氮化铝复合粉体的制造方法，其中，保温后的氧化时间为4-6小时。The method for producing an alumina or aluminum nitride composite powder according to claim 4, wherein the oxidation time after the heat retention is 4 to 6 hours.
  6. 根据权利要求3所述的氧化铝、氮化铝复合粉体的制造方法，其中，用于加入的所述的氧化铝、氮化铝复合粉体中氮化铝的含量为4.1·(Mo-M)/M·100％，其中Mo为初始氧化铝和碳粉混合粉体中的氧化铝的质量，M是所述不含碳的氧化铝、氮化铝复合粉体的质量。The method for producing an alumina or aluminum nitride composite powder according to claim 3, wherein the content of aluminum nitride in the alumina or aluminum nitride composite powder used for the addition is 4.1·(Mo- M) / M · 100%, wherein Mo is the mass of alumina in the initial alumina and carbon powder mixed powder, and M is the mass of the carbon-free alumina or aluminum nitride composite powder.
  7. 根据权利要求6所述的氧化铝、氮化铝复合粉体的制造方法，用于加入的所述的氧化铝、氮化铝复合粉体中氧化铝的用量为4.1·(Mo-M)/w-M，其中w为所述不含碳的氧化铝、氮化铝复合粉体中氮化铝的含量。 The method for producing an alumina or aluminum nitride composite powder according to claim 6, wherein the amount of alumina in the alumina or aluminum nitride composite powder to be added is 4.1·(Mo-M)/ wM, wherein w is the content of aluminum nitride in the carbon-free alumina or aluminum nitride composite powder.
PCT/CN2015/094138 2015-11-09 2015-11-09 Method for preparing composite powder of aluminium oxide and aluminium nitride WO2017079878A1 (en)

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