CN116573940A - 一种高韧性碳化硅陶瓷材料及其制备方法 - Google Patents
一种高韧性碳化硅陶瓷材料及其制备方法 Download PDFInfo
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- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 83
- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 238000005245 sintering Methods 0.000 claims abstract description 56
- 238000000034 method Methods 0.000 claims abstract description 21
- IRPGOXJVTQTAAN-UHFFFAOYSA-N 2,2,3,3,3-pentafluoropropanal Chemical compound FC(F)(F)C(F)(F)C=O IRPGOXJVTQTAAN-UHFFFAOYSA-N 0.000 claims abstract description 15
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- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 15
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000001816 cooling Methods 0.000 claims abstract description 12
- 239000002002 slurry Substances 0.000 claims abstract description 12
- 238000000498 ball milling Methods 0.000 claims abstract description 11
- 239000000919 ceramic Substances 0.000 claims abstract description 11
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- 239000011812 mixed powder Substances 0.000 claims abstract description 11
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 7
- 238000000227 grinding Methods 0.000 claims abstract description 6
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- 229910001208 Crucible steel Inorganic materials 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
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- 230000009471 action Effects 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- 229910052731 fluorine Inorganic materials 0.000 description 4
- 239000011737 fluorine Substances 0.000 description 4
- 239000012299 nitrogen atmosphere Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
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- 238000006243 chemical reaction Methods 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 238000000280 densification Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 229910003923 SiC 4 Inorganic materials 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 230000002708 enhancing effect Effects 0.000 description 2
- 238000001272 pressureless sintering Methods 0.000 description 2
- 230000004075 alteration Effects 0.000 description 1
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- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
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- 230000035939 shock Effects 0.000 description 1
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Abstract
本发明公开了一种高韧性碳化硅陶瓷材料及其制备方法,属于陶瓷材料技术领域,该制备方法包括以下步骤:(1)将碳化硅粉末和烧结助剂的混合粉末进行球磨,得到碳化硅浆料;(2)将碳化硅浆料烘干、机械研磨并过筛后,压制成型,得到碳化硅素坯;(3)将碳化硅素坯转入真空烧结炉中,在温度为1650‑1750℃、抽真空条件下烧结1‑2h,得到碳化硅陶瓷体;(4)向真空烧结炉中通入氮气,并降温至1300‑1400℃保温1‑2h,冷却至室温后,得到高韧性碳化硅陶瓷材料;本发明将铝粉和氟化铝粉复配为烧结助剂,并结合简单易行的烧结工艺和保温处理,提高了碳化硅陶瓷材料的致密性和断裂韧性。
Description
技术领域
本发明属于陶瓷材料技术领域,具体涉及一种高韧性碳化硅陶瓷材料及其制备方法。
背景技术
碳化硅陶瓷材料因具有硬度高、高温强度高、热膨胀系数小、热稳定性好、抗热震性好以及耐化学腐蚀性好等优良特性,在航空航天、新能源、化工、运输等领域有广泛的用途。目前碳化硅陶瓷材料主要有三种烧结方法,即反应烧结法、无压烧结法和热压烧结法;三种方法各有优缺点:反应烧结法生产的碳化硅有烧结温度低、能耗低的优点,但存在结构颗粒粗,机械强度低,韧性差的缺点;无压烧结法生产的碳化硅具有高机械强度、高韧性、结构颗粒细的优点,但存在烧结温度高,能耗大的缺点;热压烧结碳化硅因成本高、烧结设备技术要求高等缺点。
现有的碳化硅陶瓷材料的断裂韧性较低,容易从表面开始发生脆性断裂,不能满足机械密封行业对陶瓷材料高韧性的要求,而单一的碳化硅粉末难以直接烧结致密,需要添加适当的烧结助剂进行优化,如何将烧结助剂与烧结方法相结合,以制造出高韧性的碳化硅陶瓷材料是目前亟需解决的问题。
发明内容
本发明的目的在于提供一种高韧性碳化硅陶瓷材料及其制备方法,以解决背景技术中的问题。
本发明的目的可以通过以下技术方案实现:
一种高韧性碳化硅陶瓷材料的制备方法,包括以下步骤:
(1)将碳化硅粉末和烧结助剂的混合粉末加入球磨机中,球磨1-2h,得到碳化硅浆料;
(2)将碳化硅浆料置于80-100℃的鼓风干燥箱内烘干40-60mi n,机械研磨并过100目筛后,压制成型,得到碳化硅素坯;
(3)将碳化硅素坯转入真空烧结炉中,在温度为1650-1750℃、抽真空条件下烧结1-2h,得到碳化硅陶瓷体;
(4)向真空烧结炉中通入氮气,并降温至1300-1400℃保温1-2h,冷却至室温后,得到高韧性碳化硅陶瓷材料。
进一步地,所述烧结助剂的用量为碳化硅粉末质量的9-10%,所述碳化硅粉末的粒径为500nm-1μm。
进一步地,所述烧结助剂为铝粉和氟化铝粉按照质量比1-2:1混合组成;氟化铝粉中的氟元素作用于碳化硅颗粒表面,使硅碳键发生断裂后,有一部分产物以单质硅和碳形式存在,硅和碳能够与铝粉反应,生成Al4SiC4并分布于晶界处,Al4SiC4为规则的六方片层结构,能够使裂纹扩展方向产生偏移或分层,释放裂纹扩展能,增强碳化硅陶瓷材料的断裂韧性;此外,在氟元素的作用下碳化硅颗粒表面发生了分解,相当于碳化硅颗粒的原先表面发生了剥离,露出的新的表面具有更强的活性,使得烧结致密化更容易进行。
进一步地,所述铝粉的粒径为100-200nm,所述氟化铝粉的粒径为300-500nm;铝粉粒径与氟化铝粉粒径相互配合,有利于液相的产生,促进晶粒生长及致密化,在烧结时起到更好的助烧作用,
进一步地,所述球磨机中混合粉末、无水乙醇和球磨介质的质量比为1:1:4-5。
进一步地,所述压制成型为使用铸钢模具在成型压力为140-160MPa下,保压30-50s。
一种高韧性碳化硅陶瓷材料,包括碳化硅粉末和烧结助剂,在真空条件下烧结后,再在1300-1400℃的氮气氛围下保温处理,保温处理后能够将烧结产生的多余游离硅含量减少,有效避免碳化硅陶瓷材料从表面开始发生脆性断裂,从而得到高韧性碳化硅陶瓷材料。
本发明的有益效果:
本发明以铝粉和氟化铝粉复配为烧结助剂,氟化铝粉中的氟元素能使硅碳键发生断裂,产生游离的单质硅和碳,硅和碳能够与铝粉反应,生成Al4S iC4并分布于晶界处,能够使裂纹扩展方向产生偏移或分层,释放裂纹扩展能,增强碳化硅陶瓷材料的断裂韧性;同时,氟元素的作用下碳化硅颗粒表面分解后,露出的新表面具有更强的活性,使得烧结致密化更容易进行,达到更好的烧结效果;
本发明在氮气氛围、1300-1400℃下对碳化硅陶瓷体进行保温处理,碳化硅颗粒表面分解出的多余单质硅与氮气发生氮化反应,使得碳化硅陶瓷体表面力学性能较差的游离硅的含量减少,同时在碳化硅陶瓷体表面生成力学性能优异的致密Si3N4保护层,起到进一步增强材料断裂韧性的作用;
本发明的制备方法简单易行,选用的烧结助剂不仅在烧结阶段起到助烧作用,得到断裂韧性优异的碳化硅陶瓷体,还能与后续的保温处理工序配合,进一步提升碳化硅陶瓷材料的断裂韧性。
具体实施方式
下面将结合本发明实施例,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其它实施例,都属于本发明保护的范围。
实施例1
一种高韧性碳化硅陶瓷材料,通过以下制备方法制得:
(1)将平均粒径为100nm的铝粉和平均粒径为300nm的氟化铝粉按照质量比1:1混合制成烧结助剂,然后将平均粒径为500nm的碳化硅粉末和碳化硅粉末9wt%的烧结助剂混合均匀后,得到混合粉末,将混合粉末、无水乙醇和球磨介质按照质量比为1:1:4加入球磨机中,球磨1h,得到碳化硅浆料;
(2)将碳化硅浆料置于80℃的鼓风干燥箱内,烘干60mi n,机械研磨并过100目筛后,使用铸钢模具在成型压力为140MPa下,保压50s压制成型,得到碳化硅素坯;
(3)将碳化硅素坯转入真空烧结炉中,在温度为1650℃、抽真空条件下烧结2h,得到碳化硅陶瓷体;
(4)向真空烧结炉中通入氮气,并降温至1300℃保温2h,冷却至室温后,得到高韧性碳化硅陶瓷材料。
实施例2
一种高韧性碳化硅陶瓷材料,通过以下制备方法制得:
(1)将平均粒径为150nm的铝粉和平均粒径为400nm的氟化铝粉按照质量比1:1混合制成烧结助剂,然后将平均粒径为800nm的碳化硅粉末和碳化硅粉末10wt%的烧结助剂混合均匀后,得到混合粉末,将混合粉末、无水乙醇和球磨介质按照质量比为1:1:4加入球磨机中,球磨1h,得到碳化硅浆料;
(2)将碳化硅浆料置于90℃的鼓风干燥箱内,烘干50mi n,机械研磨并过100目筛后,使用铸钢模具在成型压力为150MPa下,保压40s压制成型,得到碳化硅素坯;
(3)将碳化硅素坯转入真空烧结炉中,在温度为1700℃、抽真空条件下烧结2h,得到碳化硅陶瓷体;
(4)向真空烧结炉中通入氮气,并降温至1350℃保温2h,冷却至室温后,得到高韧性碳化硅陶瓷材料。
实施例3
一种高韧性碳化硅陶瓷材料,通过以下制备方法制得:
(1)将平均粒径为200nm的铝粉和平均粒径为500nm的氟化铝粉按照质量比2:1混合制成烧结助剂,然后将平均粒径为1μm的碳化硅粉末和碳化硅粉末10wt%的烧结助剂混合均匀后,得到混合粉末,将混合粉末、无水乙醇和球磨介质按照质量比为1:1:5加入球磨机中,球磨2h,得到碳化硅浆料;
(2)将碳化硅浆料置于100℃的鼓风干燥箱内,烘干40mi n,机械研磨并过100目筛后,使用铸钢模具在成型压力为160MPa下,保压30s压制成型,得到碳化硅素坯;
(3)将碳化硅素坯转入真空烧结炉中,在温度为1750℃、抽真空条件下烧结1h,得到碳化硅陶瓷体;
(4)向真空烧结炉中通入氮气,并降温至1400℃保温1h,冷却至室温后,得到高韧性碳化硅陶瓷材料。
对比例1
本对比例与实施例2相比,不添加氟化铝粉,仅使用铝粉作为烧结助剂,且铝粉用量为碳化硅粉末的10wt%,其余步骤和参数均与实施例2相同。
对比例2
本对比例与实施例2相比,不添加铝粉,仅使用氟化铝粉作为烧结助剂,且氟化铝粉用量为碳化硅粉末的5wt%,其余步骤和参数均与实施例2相同。
对比例3
本对比例与实施例2相比,不在氮气气氛中保温处理,其余步骤和参数均与实施例2相同。
对实施例1-实施例3和对比例1-对比例3制得的碳化硅陶瓷材料的密度、维氏硬度和断裂韧性进行性能测试,采用排水法测定密度,使用微维氏硬度计直接测量维氏硬度,采用压痕法测试断裂韧性,结果如表1所示:
表1
由表1数据可以看出,实施例1-实施例3制得的碳化硅陶瓷材料具有较高的密度、硬度和优异的断裂韧性,说明本发明的制备方法能够提高碳化硅陶瓷材料的致密性和力学性能;对比例1-对比例3制得的碳化硅陶瓷材料在致密性和断裂韧性方面均低于本发明的碳化硅陶瓷材料,单一的烧结助剂并不能带来综合的力学性能,经过氮气气氛保温处理能够进一步提高碳化硅陶瓷材料的断裂韧性。
需要说明的是,在本文中,诸如第一和第二等之类的关系术语仅仅用来将一个实体或者操作与另一个实体或操作区分开来,而不一定要求或者暗示这些实体或操作之间存在任何这种实际的关系或者顺序。而且,术语“包括”、“包含”或者其任何其他变体意在涵盖非排他性的包含,从而使得包括一系列要素的过程、方法、物品或者设备不仅包括那些要素,而且还包括没有明确列出的其他要素,或者是还包括为这种过程、方法、物品或者设备所固有的要素。
尽管已经示出和描述了本发明的实施例,对于本领域的普通技术人员而言,可以理解在不脱离本发明的原理和精神的情况下可以对这些实施例进行多种变化、修改、替换和变型,本发明的范围由所附权利要求及其等同物限定。
Claims (7)
1.一种高韧性碳化硅陶瓷材料的制备方法,其特征在于,包括以下步骤:
(1)将碳化硅粉末和烧结助剂的混合粉末加入球磨机中,球磨1-2h,得到碳化硅浆料;
(2)将碳化硅浆料置于80-100℃的鼓风干燥箱内烘干40-60min,机械研磨并过100目筛后,压制成型,得到碳化硅素坯;
(3)将碳化硅素坯转入真空烧结炉中,在温度为1650-1750℃、抽真空条件下烧结1-2h,得到碳化硅陶瓷体;
(4)向真空烧结炉中通入氮气,并降温至1300-1400℃保温1-2h,冷却至室温后,得到高韧性碳化硅陶瓷材料。
2.根据权利要求1所述的一种高韧性碳化硅陶瓷材料的制备方法,其特征在于,所述烧结助剂的用量为碳化硅粉末质量的9-10%,所述碳化硅粉末的粒径为500nm-1μm。
3.根据权利要求2所述的一种高韧性碳化硅陶瓷材料的制备方法,其特征在于,所述烧结助剂为铝粉和氟化铝粉按照质量比1-2:1混合组成。
4.根据权利要求3所述的一种高韧性碳化硅陶瓷材料的制备方法,其特征在于,所述铝粉的粒径为100-200nm,所述氟化铝粉的粒径为300-500nm。
5.根据权利要求1所述的一种高韧性碳化硅陶瓷材料的制备方法,其特征在于,所述球磨机中混合粉末、无水乙醇和球磨介质的质量比为1:1:4-5。
6.根据权利要求1所述的一种高韧性碳化硅陶瓷材料的制备方法,其特征在于,所述压制成型为使用铸钢模具在成型压力为140-160MPa下,保压30-50s。
7.一种高韧性碳化硅陶瓷材料,其特征在于,由权利要求1-6任意一项所述制备方法制得。
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Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH0733528A (ja) * | 1993-06-28 | 1995-02-03 | Kyocera Corp | セラミック複合焼結体及びその製法、並びにそれを用いた半導体製造用治具 |
US5571758A (en) * | 1993-08-19 | 1996-11-05 | General Electric Company | Nitrogen-reacted silicon carbide material |
CN111499387A (zh) * | 2020-04-22 | 2020-08-07 | 衡阳凯新特种材料科技有限公司 | 高强度氮化硅复合碳化硅陶瓷及其制备方法和应用 |
CN111747752A (zh) * | 2020-07-15 | 2020-10-09 | 山田研磨材料有限公司 | 一种表面改性的反应烧结碳化硅陶瓷及制备工艺 |
CN113307644A (zh) * | 2021-06-17 | 2021-08-27 | 山田研磨材料有限公司 | 一种氮化改性反应烧结碳化硅陶瓷表面的方法 |
-
2023
- 2023-04-28 CN CN202310477908.0A patent/CN116573940A/zh active Pending
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH0733528A (ja) * | 1993-06-28 | 1995-02-03 | Kyocera Corp | セラミック複合焼結体及びその製法、並びにそれを用いた半導体製造用治具 |
US5571758A (en) * | 1993-08-19 | 1996-11-05 | General Electric Company | Nitrogen-reacted silicon carbide material |
CN111499387A (zh) * | 2020-04-22 | 2020-08-07 | 衡阳凯新特种材料科技有限公司 | 高强度氮化硅复合碳化硅陶瓷及其制备方法和应用 |
CN111747752A (zh) * | 2020-07-15 | 2020-10-09 | 山田研磨材料有限公司 | 一种表面改性的反应烧结碳化硅陶瓷及制备工艺 |
CN113307644A (zh) * | 2021-06-17 | 2021-08-27 | 山田研磨材料有限公司 | 一种氮化改性反应烧结碳化硅陶瓷表面的方法 |
Non-Patent Citations (3)
Title |
---|
付振东: "碳化硅陶瓷新型烧结助剂体系研究", 《万方学位论文》, pages 22 - 24 * |
周松青, 唐绍裘, 肖汉宁, 邹长元: "碳化硅及其复合材料的烧结", 陶瓷学报, no. 01 * |
杨一明, 冯春祥: "用聚碳硅烷作粘结剂制备碳化硅烧结体", 炭素, no. 04 * |
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