CN114249594A - 一种超细碳化硅粉体的制备工艺 - Google Patents
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- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 239000002994 raw material Substances 0.000 claims abstract description 27
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- 239000000843 powder Substances 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 19
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 17
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- 239000006229 carbon black Substances 0.000 claims abstract description 9
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- 238000003825 pressing Methods 0.000 claims abstract description 4
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 4
- 238000009694 cold isostatic pressing Methods 0.000 claims description 4
- 238000007580 dry-mixing Methods 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
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- 229910052593 corundum Inorganic materials 0.000 description 6
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Abstract
本发明公开了一种制备碳化硅超细陶瓷粉体的方法,包括如下步骤:1)按照质量分数,将40~70%的炭黑粉末、0~30%的二氧化硅粉末、0~30%鳞片石墨粉、0~70%的熔石英粉末混合均匀,得到原料;2)将原料置于球磨机中,球磨至粒径小于20μm得到混合粉料;3)将均匀混合的粉体置于模具中,采用冷压的方式使其变为块状样品,压力为10‑50MPa,保压2‑8分钟;4)加热坯料后降温即得所述含有碳化硅的陶瓷材料。该制备方法简单,降低了原料成本,可大规模制备。
Description
技术领域
本发明涉及一种超细碳化硅粉体的制备工艺,属于高温结构功能一体化陶瓷的技术领域,可适用于磨料、高温半导体器件、各种冶炼炉衬、高温炉窑构件、碳化硅板、衬板、支撑件等。
背景技术
碳化硅(SiC)是是由碳原子和硅原子以共价键为主结合而成,具有很高的硬度和熔点。SiC不仅具有导热率高,热膨胀系数小,且抗震性很高的优点,还具有很高的化学稳定性和优异的热稳定性。
SiC粉体的制备方法有激光气相合成法、等离子体法、高能球磨法等,这些方法有的制备工艺相对复杂,有的需要制备的环境苛刻,导致碳化硅成本较高。
通过固相反应制备碳化硅纳米粉体,具有制备方法简单,制备环境要求较低,可实现大规模产业化生产。实验制备的碳化硅纳米粉体性能优于传统的碳化硅粉体,能够达到高新技术领域的严格要求,具有更为广泛的用途。
发明内容
本发明的目的是解决了合成碳化硅陶瓷材料制备工艺成本较高,简化了制备超细碳化硅纳米粉体的生产工艺,拓宽该技术的应用领域。本发明通过高温固相反应制备了碳化硅纳米粉体,提供了一种高效简洁的方法,该方法对原料要求简单,且危险性小,可大量制备,该方法以炭黑、二氧化硅和鳞片石墨为原料,制备出碳化硅陶瓷材料。
本发明所采用的技术方案是:一种超细碳化硅粉体的制备工艺,包括如下步骤:
1)按照质量分数,将40~70%的炭黑粉末、0~30%的鳞片石墨粉末、0~50%二氧化硅粉、0~70%的熔石英粉末混合均匀,得到原料。
2)将所述原料置于球磨机中对其进行球磨,待其混合均匀后,干燥,得到粒径小于20μm得到混合粉料。
3)将均匀混合的粉体置于模具中,采用冷压的方式使其变为块状样品,压力为10-50MPa,保压2-8分钟。
4)将所述坯料置于加热炉内,真空度约为1.0×10-2Pa,以5~15℃/min的速率升温到1400-2500℃,保温1-6h后降温冷却。
5)将所制备的试样通过球磨机进行球磨,球磨时间为1-8h,取出粉料。即得所述的含有超细碳化硅陶瓷材料。
进一步的,所述的二氧化硅粉末、鳞片石墨粉末、炭黑粉末、硅粉的粒径均小于20μm。
进一步的,所述的步骤2)原料混合过程中的球磨方式分为干混和湿混两种方式,其中湿混的球磨介质为无水乙醇。
进一步的,所述的步骤3)制备坯料的方法为冷等静压成型,模压成型。
进一步的,所述的步骤4)的升温过程分为三步,第一步以10~15℃/min的速率由室温升温到1200~1400℃,第二步以6~10℃/min的速率升温到1500~1700℃,第三步以3~8℃/min的速率升温到1800~2500℃。
进一步的,所述的步骤4)的降温冷却为随炉冷却,或者在400~50℃出炉后于空气中强制冷却。
进一步的,所述的步骤4)所述的将温度升到1400~2500℃,并保温时间为1-6h。
进一步的,所述的步骤5)所述的球磨机器为高能球磨机。
进一步的,所述的步骤5)所述的球磨过程中球料比为5:1。
本发明的有益效果是:利用炭黑、熔石英和鳞片石墨为原料,通过冷压成型制成坯料,在2500℃以下通过高温固相反应制备碳化硅陶瓷材料。相比于其现有的制备工艺,本发明提供的制备工艺简单,原料成本降低,安全性高,易于控制,可用于产业化生产。
附图说明
图1:C-Si的相图;
图2:SiC样品的XRD图。
具体实施方式
以下结合实施例对本发明超细碳化硅的制备方法进行详细描述。
实施例1
一种合成超细碳化硅材料的制备方法,包括如下步骤:
1)按照体积分数,将70Vol% 炭黑和30Vol%熔石英粉末混合均匀,得到原料;
2)将所述原料置于球磨机中,按照原料与刚玉球质量比为1:3加入刚玉球,湿法球磨2h后烘干,得到粒径小于20μm的混合粉料;
3)将原料放入模具中,加压成型,压力为25MPa,保压3分钟,脱模后得到坯料;
4)将所述坯料置于加热炉内, 煅烧制度为:以10℃/min的升温速率从室温升温至500℃;再以7℃/min的升温速率升温至1400 ℃;然后以5℃/min的升温速率升温至1800℃;保温180min;随炉冷却;即得含有碳化硅的陶瓷材料。
实施例2
一种合成超细碳化硅材料的制备方法,包括如下步骤:
1)按照物质的量之比,将鳞片石墨和二氧化硅的物质的量之比为3:2的粉末混合均匀,得到原料;
2)将所述原料置于球磨机中,按照原料与刚玉球质量比为1:3加入刚玉球,湿法球磨2.5h后烘干,得到粒径小于20μm的混合粉料;
3)将样品置入橡胶模具中,在50MPa冷等静压下成型,脱模后得到坯料;
4)将所述坯料置于真空加热炉内, 煅烧制度为:以10℃/min的升温速率从室温升温至500 ℃;再以7℃/min的升温速率升温至1400 ℃;然后以5℃/min的升温速率升温至1800℃;保温180min;随炉冷却;即得含有碳化硅的陶瓷材料。
实施例3
一种合成十二硼化锆材料的制备方法,包括如下步骤:
1)按照物质的量之比,将石墨粉和沙子物质的量之比为3:2的粉末混合均匀,得到原料;
2)将所述原料置于球磨机中,按照原料与刚玉球质量比为1:3加入刚玉球,湿法球磨2.5h后烘干,得到粒径小于20μm的混合粉料;
3)将样品置入橡胶模具中,在50MPa冷等静压下成型,脱模后得到坯料;
4)将所述坯料置于真空加热炉内, 煅烧制度为:以10℃/min的升温速率从室温升温至500 ℃;再以7℃/min的升温速率升温至1400 ℃;然后以5℃/min的升温速率升温至1800℃;保温180min;随炉冷却;即得含有碳化硅的陶瓷材料。
综上,本发明公开了一种制备碳化硅超细陶瓷粉体的方法,包括如下步骤:1)按照质量分数,将40~70%的炭黑粉末、0~30%的二氧化硅粉末、0~30%鳞片石墨粉、0~70%的熔石英粉末混合均匀,得到原料;2)将原料置于球磨机中,球磨至粒径小于20μm得到混合粉料;3)将均匀混合的粉体置于模具中,采用冷压的方式使其变为块状样品,压力为10-50MPa,保压2-8分钟;4)加热坯料后降温即得所述含有碳化硅的陶瓷材料。该制备方法简单,降低了原料成本,可大规模制备。
尽管上面对本发明的优选实施例进行了描述,但是本发明并不局限于上述的具体实施方式,上述的具体实施方式仅仅是示意性的,并不是限制性的,本领域的技术人员在本发明的启示下,在不脱离本发明宗旨和权利要求所保护的范围情况下,还可以做出很多形式,这些均属于本发明的保护范围之内。
Claims (9)
1.一种超细碳化硅粉体的制备工艺,其特征在于,包括如下实验步骤:
1)按照质量分数,将40~70%的炭黑粉末、0~50%的二氧化硅粉末、0~30%硅粉、0~30%的鳞片石墨粉末混合均匀,得到原料;
2)将所述原料置于球磨机中对其进行球磨,待其混合均匀后,干燥,得到粒径小于20μm得到混合粉料,其中混合方式可以分为干混和湿混;
3)将均匀混合的粉体置于模具中,采用冷压的方式使其变为块状样品,压力为10-50MPa,保压2-8分钟;
4)将所述坯料置于加热炉内,真空度约为1.0×10-2Pa,以3~15℃/min的速率升温到1300-2500℃,保温1-6h后降温冷却;
5)将所制备的试样通过球磨机进行球磨,球磨时间为1-8h,取出粉料,
即得所述的含有超细碳化硅陶瓷材料。
2.根据权利要求1所述的制备方法,其特征在于,步骤1)所述二氧化硅粉末、鳞片石墨粉末、炭黑粉末、硅粉的粒径均小于20μm。
3.根据权利要求1所述的制备方法,其特征在于,步骤2)原料混合过程中的球磨方式分为干混和湿混两种方式,其中湿混的球磨介质为无水乙醇。
4.根据权利要求1所述的制备方法,其特征在于,步骤3)制备坯料的方法为冷等静压成型,模压成型。
5.根据权利要求1所述的制备方法,其特征在于,步骤4)的升温过程分为三步,第一步以10~15℃/min的速率由室温升温到1200~1400℃,第二步以6~10℃/min的速率升温到1500~1700℃,第三步以3~8℃/min的速率升温到1800~2500℃。
6.根据权利要求1所述的制备方法,其特征在于,步骤4)的降温冷却为随炉冷却,或者在400~50℃出炉后于空气中强制冷却。
7.根据权利要求1所述的制备方法,其特征在于,步骤4)所述的将温度升到1400~2500℃,并保温时间为1-6h。
8.根据权利要求1所述的制备方法,其特征在于,步骤5)所述的球磨机器为高能球磨机。
9.根据权利要求1所述的制备方法,其特征在于,步骤5)所述的球磨过程中球料比为5:1。
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