CN104909762A - Spherical large particle aluminum nitride powder preparation method - Google Patents
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Abstract
一种球形大颗粒氮化铝粉末的制备方法，属于粉末冶金领域。其特征在于，将氮化铝粉末、粘结剂、助烧剂，分散剂在有机溶剂中进行混合，配成浆料，通过喷雾造粒制得球形氮化铝团聚体作为造粒料，再经高温煅烧、球磨分散工艺制得球形氮化铝粉末。所得球形氮化铝粉末，球形度在0.65～0.9，粒度在5～80μm，松装密度为0.85～1.1g/cm3，振实密度为1.0～1.25g/cm3。本发明方法制备的氮化铝粉末球形度高，粒径均匀，流动性好。制备工艺简单，生产成本低，制备的粉末可应用于导热塑料填料。The invention discloses a method for preparing spherical large-grain aluminum nitride powder, which belongs to the field of powder metallurgy. It is characterized in that aluminum nitride powder, binder, sintering aid, and dispersant are mixed in an organic solvent to form a slurry, and spherical aluminum nitride aggregates are obtained by spray granulation as granulation materials, and then Spherical aluminum nitride powder is prepared by high temperature calcination and ball milling dispersion process. The obtained spherical aluminum nitride powder has a sphericity of 0.65-0.9, a particle size of 5-80 μm, a bulk density of 0.85-1.1 g/cm 3 and a tap density of 1.0-1.25 g/cm 3 . The aluminum nitride powder prepared by the method of the invention has high sphericity, uniform particle size and good fluidity. The preparation process is simple, the production cost is low, and the prepared powder can be applied to heat-conducting plastic fillers.
Description
技术领域technical field
本发明属于粉末冶金领域，涉及一种球形大颗粒氮化铝粉末的制备方法。The invention belongs to the field of powder metallurgy and relates to a method for preparing spherical large-grain aluminum nitride powder.
技术背景technical background
氮化铝陶瓷具有较高的热导率，其理论值为320W/m.K，较高的电绝缘性，与硅相匹配的热膨胀系数，目前广泛应用于电子元器件中作为散热材料。但这些应用属于直接使用氮化铝陶瓷，而随着照明行业的发展，导热塑料用于制造LED灯罩以及汽车中，导热塑料是利用导热填料对高分子基体材料进行均匀填充，以提高其导热性能。与传统铝材相比，导热塑料制品具有重量轻，成形加工方便，可以和其它塑料一样，经过一次成形，生产薄壁及复杂形状零件，产品设计自由度高；此外，由于金属壳体导电，内部必须采用隔离启动系统，以防止触电，而导热塑料绝缘，当做散热系统时可以采用非隔离系统启动，节省成本且所占空间较小。Aluminum nitride ceramics have high thermal conductivity, with a theoretical value of 320W/m.K, high electrical insulation, and a thermal expansion coefficient that matches silicon, and are currently widely used in electronic components as heat dissipation materials. However, these applications belong to the direct use of aluminum nitride ceramics. With the development of the lighting industry, thermally conductive plastics are used in the manufacture of LED lampshades and automobiles. Thermally conductive plastics use thermally conductive fillers to evenly fill polymer matrix materials to improve their thermal conductivity. . Compared with traditional aluminum materials, thermally conductive plastic products are light in weight and easy to form and process. Like other plastics, they can be formed at one time to produce thin-walled and complex-shaped parts, and the product design freedom is high; in addition, because the metal shell is conductive, An isolated start-up system must be used inside to prevent electric shock, and the heat-conducting plastic is insulated. When used as a heat dissipation system, a non-isolated system can be used to start, which saves costs and takes up less space.
导热塑料主要成分包括基体材料和填料，基体材料包括PPS、PA6/PA66、PC、PP等，填料包括AlN、SiC、Al2O3、BN等。其导热性能利用热导率(单位：W/m.K)来衡量。而提高其导热性能的方法为提高基体材料的导热系数和采用高导热材质作为填料、提高填料比例、以及通过改善填料与基体材质的结合界面几方面来进行，而填料加入的比例对于导热塑料的导热性能具有较高的影响，为了提高粉末的装填量，必须制备粒径在数微米与几十微米的球形氮化铝粉末，以获得流动性好，强度高，粉末填充量大的导热塑料。而传统制备的氮化铝粉末采用直接氮化法或者碳热还原法生产，前者制备出的粉末经过破碎后，获得粉末粗细不均，形状不规则，后者制备的粉末粒径较小，一般在1微米左右，且形状为非球形，因此很难得到高填充量导热塑料。The main components of thermally conductive plastics include matrix materials and fillers. The matrix materials include PPS, PA6/PA66, PC, PP, etc., and the fillers include AlN, SiC, Al 2 O 3 , BN, etc. Its thermal conductivity is measured by thermal conductivity (unit: W/mK). The method to improve its thermal conductivity is to improve the thermal conductivity of the matrix material, use high thermal conductivity materials as fillers, increase the proportion of fillers, and improve the bonding interface between fillers and matrix materials. The thermal conductivity has a high impact. In order to increase the powder loading, it is necessary to prepare spherical aluminum nitride powder with a particle size of several microns and tens of microns to obtain a thermally conductive plastic with good fluidity, high strength and large powder filling. The traditionally prepared aluminum nitride powder is produced by the direct nitriding method or the carbothermal reduction method. After the powder prepared by the former is crushed, the obtained powder is uneven in thickness and irregular in shape, and the powder prepared by the latter has a smaller particle size. It is around 1 micron, and the shape is non-spherical, so it is difficult to obtain high-filling thermally conductive plastics.
关于制备球形氮化铝的专利已有几种如(CN103079995A)以及(CN102686511A)中将氧化铝或氧化铝水合物与碳粉及助熔剂进行混合，使用该混合粉末在一定温度下反应，合成氮化铝粉，在空气中加热除去多余碳，从而得到球形氮化铝粉末，但该方法制备的氮化铝粉末，碳粉易包裹或碳原子固溶于氮化铝粉末中，影响氮化铝粉末热导率，且制得粉末颜色较深，用于导热塑料中影响美观。There are several patents on the preparation of spherical aluminum nitride, such as (CN103079995A) and (CN102686511A), in which alumina or alumina hydrate is mixed with carbon powder and flux, and the mixed powder is used to react at a certain temperature to synthesize nitrogen Aluminum nitride powder is heated in air to remove excess carbon to obtain spherical aluminum nitride powder, but the aluminum nitride powder prepared by this method is easy to wrap carbon powder or carbon atoms are solid-dissolved in aluminum nitride powder, which affects the aluminum nitride powder. The thermal conductivity of the powder is low, and the color of the prepared powder is darker, which affects the appearance when used in heat-conducting plastics.
发明内容Contents of the invention
本发明的目的是提供一种球形大颗粒氮化铝粉末的制备方法。The purpose of the present invention is to provide a method for preparing spherical large particle aluminum nitride powder.
技术方案是：将氮化铝粉末、粘结剂、助烧剂，分散剂在有机溶剂中进行混合，配成浆料，通过喷雾造粒制得球形氮化铝团聚体作为造粒料，再经高温煅烧、球磨分散工艺制得球形氮化铝粉末。The technical solution is: mix aluminum nitride powder, binder, sintering aid, and dispersant in an organic solvent to form a slurry, and obtain spherical aluminum nitride aggregates as granulation materials through spray granulation, and then Spherical aluminum nitride powder is prepared by high temperature calcination and ball milling dispersion process.
本发明所采用的操作步骤是：The operating steps adopted in the present invention are:
步骤一，配料：将氮化铝粉末、粘结剂、助烧剂，分散剂、酒精按照质量百分比配料：氮化铝粉体30％-60％，粘结剂0.03％-5％，助烧剂2％-10％，分散剂0.5％-5％，，酒精30％-65％；Step 1, ingredients: mix aluminum nitride powder, binder, sintering aid, dispersant, alcohol according to mass percentage: 30%-60% of aluminum nitride powder, 0.03%-5% of binder, sintering aid Agent 2%-10%, dispersant 0.5%-5%, alcohol 30%-65%;
步骤二，配制浆料：采用球磨，搅拌、或超声波分散将步骤一中原料进行混合，制成稳定的浆料；Step 2, prepare slurry: mix the raw materials in step 1 by ball milling, stirring, or ultrasonic dispersion to make a stable slurry;
步骤三，喷雾造粒：将步骤二中制备的浆料通过蠕动泵控制进料加入喷雾造粒机中。通过控制料浆进口、出口温度，喷雾压力，得到氮化铝造粒料Step 3, spray granulation: the slurry prepared in step 2 is fed into the spray granulator through a peristaltic pump. By controlling the inlet and outlet temperature of the slurry and the spray pressure, the aluminum nitride pellets can be obtained
步骤四，煅烧:将制得氮化铝造粒料置于烧舟中，在流动氮气气氛下于烧结炉中煅烧，制得球形氮化铝粉末。煅烧温度根据助烧剂的不同，选择1450℃到1850℃，煅烧时间30min—1000min。Step 4, calcining: the obtained aluminum nitride granulated material is placed in a sintering boat, and calcined in a sintering furnace under a flowing nitrogen atmosphere to obtain spherical aluminum nitride powder. The calcination temperature is selected from 1450°C to 1850°C according to the different sintering aids, and the calcination time is 30min-1000min.
步骤五，球磨分散：制得球形氮化铝粉末，球形度在0.65～0.9，粒度在5～80μm，松装密度为0.85～1.1g/cm3，振实密度为1.0～1.25g/cm3。所述氮化铝粉末原料粒度为0.5微米～5微米。Step 5, ball milling dispersion: obtain spherical aluminum nitride powder with a sphericity of 0.65-0.9, a particle size of 5-80 μm, a bulk density of 0.85-1.1 g/cm 3 and a tap density of 1.0-1.25 g/cm 3 . The particle size of the aluminum nitride powder raw material is 0.5 micron to 5 micron.
步骤一中助烧剂为氧化钇、氧化镧、氧化铈、氧化镁、氧化钙、氧化锂中的一种或几种；粘结剂为橡胶汽油、EVA、酚醛树脂、环氧树脂中的一种或几种；In step 1, the sintering aid is one or more of yttrium oxide, lanthanum oxide, cerium oxide, magnesium oxide, calcium oxide, and lithium oxide; the binder is one of rubber gasoline, EVA, phenolic resin, and epoxy resin. species or several;
步骤一中分散剂为硬脂酸，己烯基双硬脂酰胺、三硬脂酸甘油酯、聚乙二醇中的一种或几种；In step 1, the dispersant is one or more of stearic acid, hexenyl bisstearamide, glyceryl tristearate, and polyethylene glycol;
在该方法中，将氮化铝粉末与分散剂，粘结剂，助烧剂通过搅拌，球磨与超声波分散，制成流动性好的浆料，将浆料通过送料器送入喷雾造粒及中，通过控制温度与压力，送料速度等制得喷雾造粒料，将喷雾造粒料置于烧结炉中煅烧，制得球形氮化铝粉末。通过扫描电子显微镜观察粉末原料、造粒料、最终产物的形貌；利用松装密度仪与振实密度仪测量粉末的松装密度与振实密度。In this method, the aluminum nitride powder, dispersant, binder, and sintering aid are stirred, ball milled, and ultrasonically dispersed to make a slurry with good fluidity, and the slurry is sent to the spray granulation and In the process, the spray granulation material is prepared by controlling the temperature and pressure, the feeding speed, etc., and the spray granulation material is calcined in a sintering furnace to obtain spherical aluminum nitride powder. Observe the morphology of powder raw materials, granulated materials, and final products through a scanning electron microscope; use a bulk density meter and a tap density meter to measure the bulk density and tap density of the powder.
本发明所得球形氮化铝粉末，球形度在0.65～0.9，粒度在5～80μm，松装密度为0.85～1.1g/cm3，振实密度为1.0～1.25g/cm3。本发明方法制备的氮化铝粉末球形度高，粒径均匀，流动性好。制备工艺简单，生产成本低，制备的粉末可应用于导热塑料填料。The spherical aluminum nitride powder obtained in the present invention has a sphericity of 0.65-0.9, a particle size of 5-80 μm, an apparent density of 0.85-1.1 g/cm 3 and a tap density of 1.0-1.25 g/cm 3 . The aluminum nitride powder prepared by the method of the invention has high sphericity, uniform particle size and good fluidity. The preparation process is simple, the production cost is low, and the prepared powder can be applied to heat-conducting plastic fillers.
具体实施方式detailed description
以下对本发明进行进一步说明，实施实例中的参数指标通过下述方法来测定。The present invention is further described below, and the parameter indexes in the implementation examples are determined by the following methods.
1.平均粒径1. Average particle size
平均粒径(D50)为将试样在溶液中进行超声波分散，再利用激光粒度仪测定。The average particle size (D50) is measured by ultrasonically dispersing the sample in the solution and then using a laser particle size analyzer.
2.球形度2. Sphericity
利用扫描电子显微镜附带标尺功能，随机选取50个颗粒，测定颗粒短径(DS)与颗粒长径(DL)之比，即球形度为：DS/DL。Using the scale function attached to the scanning electron microscope, 50 particles were randomly selected, and the ratio of the short diameter (DS) to the long diameter (DL) of the particles was measured, that is, the sphericity was: DS/DL.
3.松装密度与振实密度3. Bulk density and tap density
松装密度是指粉末在规定条件下自由充满标准容器后所测得的堆积密度，即粉末松散填装时单位体积的质量，单位以g/cm3表示。振实密度是指在规定条件下容器中的粉末经振实后所测得的单位容积的质量，单位以g/cm3表示。The bulk density refers to the bulk density measured after the powder is freely filled in a standard container under specified conditions, that is, the mass per unit volume of the powder when it is loosely packed, and the unit is expressed in g/cm3. Tap density refers to the mass per unit volume measured after the powder in the container is tapped under specified conditions, and the unit is expressed in g/cm3.
实施例1：Example 1:
将氮化铝粉末1000g(D50＝0.5μm)，氧化钇粉50g(D50＝50nm)，EVA30g，三硬脂酸甘油酯10g，酒精1500g，放入球磨罐中，研磨12小时，配得浆料，然后将浆料通过蠕动泵送入喷雾干燥器离心雾化器中，离心雾化器转速为8500rpm，进风口温度220℃，出风口温度115℃，将收得造粒料过80目筛后，将造粒料放入氮化硼坩埚中，在真空碳管炉中，通入流动氮气，以10℃/min加热到1820℃，保温2小时，将煅烧后粉末在球磨罐中，放入酒精，以氧化铝球进行球磨，经干燥后得到球形氮化铝粉末。Put 1000g of aluminum nitride powder (D50=0.5μm), 50g of yttrium oxide powder (D50=50nm), 30g of EVA, 10g of glyceryl tristearate, and 1500g of alcohol into a ball mill jar, and grind for 12 hours to obtain a slurry , and then send the slurry into the centrifugal atomizer of the spray dryer through a peristaltic pump. , put the granulated material into the boron nitride crucible, in the vacuum carbon tube furnace, flow nitrogen into it, heat it to 1820°C at 10°C/min, keep it warm for 2 hours, put the calcined powder in the ball mill tank, put it into Alcohol, milled with alumina balls, and dried to obtain spherical aluminum nitride powder.
由上述工艺制备的氮化铝粉末，其球形度为0.7，粉末直径为D50＝10μm，松装密度为0.9g/cm3,振实密度为1.05g/cm3。The aluminum nitride powder prepared by the above process has a sphericity of 0.7, a powder diameter of D50=10 μm, a bulk density of 0.9 g/cm 3 and a tap density of 1.05 g/cm 3 .
实施例2：Example 2:
将氮化铝粉末1000g(D50＝0.5μm)，氧化镧粉50g(D50＝50nm)，EVA30g，己烯基双硬脂酰胺15g，酒精1200g，放入球磨罐中，研磨12小时，配得浆料，然后将浆料通过蠕动泵送入喷雾干燥器离心雾化器中，离心雾化器转速为8500rpm，进风口温度220℃，出风口温度115℃，将收得造粒料过80目筛后，将造粒料放入氮化硼坩埚中，在真空碳管炉中，通入流动氮气，以10℃/min加热到1850℃，保温2小时，将煅烧后粉末在球磨罐中，放入酒精，以氧化铝球进行球磨分散，经干燥后得到球形氮化铝粉末。Put 1000g of aluminum nitride powder (D50=0.5μm), 50g of lanthanum oxide powder (D50=50nm), 30g of EVA, 15g of hexenyl bisstearamide, and 1200g of alcohol into a ball mill jar, and grind for 12 hours to obtain a slurry Then the slurry is sent into the centrifugal atomizer of the spray dryer through the peristaltic pump. Finally, put the granulated material into a boron nitride crucible, and in a vacuum carbon tube furnace, flow nitrogen into it, heat it to 1850°C at 10°C/min, keep it warm for 2 hours, put the calcined powder in a ball mill tank, put Alcohol was added, and aluminum oxide balls were used for ball milling to disperse, and after drying, spherical aluminum nitride powder was obtained.
由上述工艺制备的氮化铝粉末，其球形度为0.8，粉末直径为D50＝25μm，松装密度为0.97g/cm3,振实密度为1.16g/cm3。The aluminum nitride powder prepared by the above process has a sphericity of 0.8, a powder diameter of D50=25 μm, a bulk density of 0.97 g/cm 3 and a tap density of 1.16 g/cm 3 .
实施例3：Example 3:
将氮化铝粉末1000g(D50＝0.5μm)，氧化铈粉50g(D50＝50nm)，EVA30g，聚乙二醇10g，酒精1000g，放入球磨罐中，研磨12小时，配得浆料，然后将浆料通过蠕动泵送入喷雾干燥器离心雾化器中，离心雾化器转速为8500rpm，进风口温度220℃，出风口温度115℃，将收得造粒料过80目筛后，将造粒料放入氮化硼坩埚中，在真空碳管炉中，通入流动氮气，以10℃/min加热到1840℃，保温2小时，将煅烧后粉末在球磨罐中，放入酒精，以氧化铝球进行球磨分散，经干燥后得到球形氮化铝粉末。Put aluminum nitride powder 1000g (D50=0.5 μm), cerium oxide powder 50g (D50=50nm), EVA30g, polyethylene glycol 10g, alcohol 1000g, put into ball mill jar, grind 12 hours, prepare slurry, then Send the slurry into the centrifugal atomizer of the spray dryer through a peristaltic pump. The rotational speed of the centrifugal atomizer is 8500rpm, the temperature of the air inlet is 220°C, and the temperature of the air outlet is 115°C. The granulated material is put into a boron nitride crucible, and in a vacuum carbon tube furnace, flow nitrogen gas, heat it to 1840°C at 10°C/min, keep it warm for 2 hours, put the calcined powder in a ball mill tank, put alcohol, Disperse by ball milling with alumina balls, and obtain spherical aluminum nitride powder after drying.
由上述工艺制备的氮化铝粉末，其球形度为0.83，粉末直径为D50＝40μm，松装密度为1.01g/cm3,振实密度为1.22g/cm3。The aluminum nitride powder prepared by the above process has a sphericity of 0.83, a powder diameter of D50=40μm, a bulk density of 1.01g/cm 3 and a tap density of 1.22g/cm 3 .
实施例4：Example 4:
将氮化铝粉末1000g(D50＝0.5μm)，氧化镁粉50g(D50＝50nm)，环氧树脂30g，聚乙二醇10g，酒精1000g，放入球磨罐中，研磨12小时，配得浆料，然后将浆料通过蠕动泵送入喷雾干燥器离心雾化器中，离心雾化器转速为8500rpm，进风口温度220℃，出风口温度115℃，将收得造粒料过80目筛后，将造粒料放入氮化硼坩埚中，在真空碳管炉中，通入流动氮气，以10℃/min加热到1500℃，保温6小时，将煅烧后粉末在球磨罐中，放入酒精，以氧化铝球进行球磨分散，经干燥后得到球形氮化铝粉末。Put 1000g of aluminum nitride powder (D50=0.5μm), 50g of magnesium oxide powder (D50=50nm), 30g of epoxy resin, 10g of polyethylene glycol, and 1000g of alcohol into a ball mill jar, and grind for 12 hours to obtain a slurry Then the slurry is sent into the centrifugal atomizer of the spray dryer through the peristaltic pump. Finally, put the granulated material into a boron nitride crucible, in a vacuum carbon tube furnace, feed flowing nitrogen gas, heat to 1500°C at 10°C/min, keep it warm for 6 hours, put the calcined powder in a ball mill tank, put Alcohol was added, and aluminum oxide balls were used for ball milling to disperse, and after drying, spherical aluminum nitride powder was obtained.
由上述工艺制备的氮化铝粉末，其球形度为0.75，粉末直径为D50＝35μm，松装密度为0.85g/cm3,振实密度为1.01g/cm3。The aluminum nitride powder prepared by the above process has a sphericity of 0.75, a powder diameter of D50=35 μm, a bulk density of 0.85 g/cm 3 and a tap density of 1.01 g/cm 3 .
实施例5：Example 5:
将氮化铝粉末1000g(D50＝0.5μm)，氧化钙粉50g(D50＝50nm)，环氧树脂30g，聚乙二醇10g，酒精1000g，放入球磨罐中，研磨12小时，配得浆料，然后将浆料通过蠕动泵送入喷雾干燥器离心雾化器中，离心雾化器转速为8000rpm，进风口温度225℃，出风口温度115℃，将收得造粒料过80目筛后，将造粒料放入氮化硼坩埚中，在真空碳管炉中，通入流动氮气，以10℃/min加热到1600℃，保温4小时，将煅烧后粉末在球磨罐中，放入酒精，以氧化铝球进行球磨分散，经干燥后得到球形氮化铝粉末。Put 1000g of aluminum nitride powder (D50=0.5μm), 50g of calcium oxide powder (D50=50nm), 30g of epoxy resin, 10g of polyethylene glycol, and 1000g of alcohol into a ball mill jar, and grind for 12 hours to obtain a slurry Then the slurry is sent into the centrifugal atomizer of the spray dryer through a peristaltic pump. The rotational speed of the centrifugal atomizer is 8000rpm, the temperature of the air inlet is 225°C, and the temperature of the air outlet is 115°C. Finally, put the granulated material into the boron nitride crucible, in the vacuum carbon tube furnace, feed flowing nitrogen gas, heat to 1600°C at 10°C/min, keep it warm for 4 hours, put the calcined powder in the ball mill tank, put Alcohol was added, and aluminum oxide balls were used for ball milling to disperse, and after drying, spherical aluminum nitride powder was obtained.
由上述工艺制备的氮化铝粉末，其球形度为0.9，粉末直径为D50＝60μm，松装密度为0.9g/cm3,振实密度为1.05g/cm3。The aluminum nitride powder prepared by the above process has a sphericity of 0.9, a powder diameter of D50=60 μm, a bulk density of 0.9 g/cm 3 and a tap density of 1.05 g/cm 3 .
实施例6：Embodiment 6:
将氮化铝粉末1000g(D50＝0.5μm)，氧化钙粉50g(D50＝50nm)，环氧树脂30g，聚乙二醇10g，酒精900g，放入球磨罐中，研磨12小时，配得浆料，然后将浆料通过蠕动泵送入喷雾干燥器离心雾化器中，离心雾化器转速为7000rpm，进风口温度230℃，出风口温度115℃，将收得造粒料过80目筛后，将造粒料放入氮化硼坩埚中，在真空碳管炉中，通入流动氮气，以10℃/min加热到1600℃，保温4小时，将煅烧后粉末在球磨罐中，放入酒精，以氧化铝球进行球磨分散，经干燥后得到球形氮化铝粉末。Put 1000g of aluminum nitride powder (D50=0.5μm), 50g of calcium oxide powder (D50=50nm), 30g of epoxy resin, 10g of polyethylene glycol, and 900g of alcohol into a ball mill jar, and grind for 12 hours to obtain a slurry Then the slurry is sent into the centrifugal atomizer of the spray dryer through a peristaltic pump. The rotational speed of the centrifugal atomizer is 7000rpm, the temperature of the air inlet is 230°C, and the temperature of the air outlet is 115°C. Finally, put the granulated material into the boron nitride crucible, in the vacuum carbon tube furnace, feed flowing nitrogen gas, heat to 1600°C at 10°C/min, keep it warm for 4 hours, put the calcined powder in the ball mill tank, put Alcohol was added, and aluminum oxide balls were used for ball milling to disperse, and after drying, spherical aluminum nitride powder was obtained.
由上述工艺制备的氮化铝粉末，其球形度为0.9，粉末直径为D50＝70μm，松装密度为1.10g/cm3,振实密度为1.21g/cm3。The aluminum nitride powder prepared by the above process has a sphericity of 0.9, a powder diameter of D50=70 μm, a bulk density of 1.10 g/cm 3 and a tap density of 1.21 g/cm 3 .
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| CN106631046A (en) * | 2016-11-30 | 2017-05-10 | 莱鼎电子材料科技有限公司 | Composite sintering aid for producing aluminum nitride ceramic substrate |
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| CN115196970A (en) * | 2022-08-08 | 2022-10-18 | 四川大学 | A kind of preparation method of high fluidity AlON spherical powder |
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