CN108439998A - 一种凝胶注模成型氮化钛陶瓷素坯的制备方法 - Google Patents
一种凝胶注模成型氮化钛陶瓷素坯的制备方法 Download PDFInfo
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Abstract
本发明公开了一种凝胶注模成型氮化钛陶瓷素坯的制备方法,其特征在于,采用单烷氧基不饱和脂肪酸钛酸酯和正庚醇对氮化钛粉体进行预处理,得到预处理氮化钛粉体;采用卡波姆941和三异丙醇胺配制凝胶溶液;然后,在球磨机中,按体积百分比加入,预处理氮化钛粉体:48%~53%,凝胶溶液:43%~48%,碳酸铵:2%~5%,各组分之和为百分之百,研磨16~18h,真空除泡处理,得到氮化钛陶瓷浆料;将氮化钛陶瓷浆料注入模具中,缓慢加热,温度至65±3℃恒温18~20 h,自然冷却后,经干燥,脱模,得到氮化钛素坯。该方法制备的氮化钛素坯具有固含量高,有机物含量低,环保,烧结后所得的氮化钛陶瓷致密度高。
Description
技术领域
本发明属于陶瓷材料成型与制备领域,具体涉及一种凝胶注模成型氮化钛陶瓷素坯的制备方法,是一种操作简单、环保、高固含量,可成型复杂形状部件及大尺寸部件,所制备的氮化钛陶瓷制品致密度。
背景技术
氮化钛是一种新型的多功能金属陶瓷材料,它能熔点高、硬度大、摩擦系数小,是热和电的良导体。首先,氮化钛是用于高强度的金属陶瓷工具、喷汽推进器、以及火箭等优良的结构材料。另外,氮化钛有较低的摩擦系数,可作为高温润滑剂。氮化钛合金用作轴承和密封环可显示出优异的效果。氮化钛有高的导电性,可用作熔盐电解的电极以及点触头薄膜膜电阻等材料。氮化钛有较高的趋导临界温度,是优良的趋导材料。尤其引人注目的是,氮化钛涂层及其烧结体具有令人满意的金黄色,可作为代金装饰材料,具有很好的仿金致果,装饰价值,并具有防腐延长工艺品的寿命。氮化钛的熔点比大多数过渡金属氮化物都高,而密度却比大多数金属氮化物都低,因为它是一种很有特色的耐火材料。氮化钛具有很高的化学稳定性。一般情况下、它与水,水蒸汽、盐酸,硫酸等均不作用,但在氢氟酸中有一定的溶解度。
在20世纪90年代初,美国橡树岭国家重点实验室Janney等提出了凝胶注模成型技术(gelcasting),首次将传统制备工艺和聚合物化学有机结合起来,开创了在陶瓷成型工艺中利用高分子单体聚合进行成型的技术。该技术可制备密度均匀、大尺寸、精度高的复杂形状的陶瓷部件,该方法具有工艺简单、成本低等优点。至今,国内外有关凝胶注模成型的研究中,以氧化铝、碳化硅、氮化硅、氮化钛等陶瓷材料居多,传统的凝胶注模成型工艺采用毒性较强具有刺激味道的单体聚丙烯酰胺或N,N-二甲基丙烯酰胺,交联剂为N,N-亚甲基双丙烯酰胺,引发剂为过硫酸铵,分散剂为聚丙烯酸。传统胶态成型工艺所制备的坯体在干燥过程中收缩通常比较大,从而造成坯体在干燥过程中发生变形、开裂等问题;并且由于成型坯体的强度较低,在脱模过程中坯体容易损坏,特别对于大尺寸、复杂形状的成型坯体有时甚至无法脱模。陶瓷材料在成型干燥、烧结过程中不可避免地存在坯体尺寸收缩现象。为了克服传统凝胶注模成型缺点,研究新的凝胶注模体系,寻找优良的胶粘剂单体、分散剂等,研究凝胶注模体系的条件制备陶瓷素坯受到关注。
卡波姆(英文名:Carbomer)为白色疏松状粉末;有特征性微臭;有引湿性,是药用辅料。卡波姆为丙烯酸键合烯丙基蔗糖或季戊四醇烯丙醚的高分子聚合物。按干燥品计算,含羧酸基(—COOH)应为56.0%~68.0%。卡波姆940:短流变性、高粘度、高清澈度,低耐离子性及耐剪切性,适用于凝胶及膏霜中。卡波姆941:长流变性、低粘度、高清澈度,中等耐离子性及耐剪切,适用于凝胶及乳液。卡波姆934:交联聚丙烯酸树脂,局部给药系统,在高粘度时稳定,用于浓凝胶剂、乳剂、混悬剂。卡波姆无毒性,广泛应用到化妆品、药物辅料中。
本发明采用单烷氧基不饱和脂肪酸钛酸酯作为分散剂,既能提高固体含量,又能降低浆料的粘度。采用卡波姆941作为凝胶胶粘剂,采用碳酸胺分解提高体系的pH值而引发凝胶聚合反应制备氮化钛陶瓷的素坯,然后经过高温烧结制备氮化钛陶瓷,本申请体系可以是固含量的体积比达到55%,成型精度高,素坯强度高,所制备的氮化钛陶瓷的致密度达到99%,结构均匀,无裂纹。制备工艺简单,环保,成本低。
发明内容
本发明的目的通过以下技术方案实现。
一种凝胶注模成型氮化钛陶瓷素坯的制备方法,其特征在于,该方法具有以下工艺步骤:
(1)氮化钛粉体预处理:在球磨机中,按质量百分比加入,氮化钛:91%~95%,烧结助剂:0.1%~2%,单烷氧基不饱和脂肪酸钛酸酯:2%~4%,正庚醇:2%~4%,各组分之和为百分之百,开启球磨机研磨3-5h,干燥,得到预处理氮化钛粉体;
(2)凝胶溶液配制:在反应器中,按质量百分浓度加入,去离子水:95%~98%,卡波姆941:0.5%~2.5%,三异丙醇胺:0.63~3.2%,各组分之和为百分之百,搅拌溶解,得到凝胶溶液;
(3)氮化钛陶瓷浆料配制:在球磨机中,按体积百分比加入,预处理氮化钛粉体:48%~53%,凝胶溶液:43%~48%,碳酸铵:2%~5%,各组分之和为百分之百,研磨16~18h,真空除泡处理,得到氮化钛陶瓷浆料;
(4)氮化钛素坯的制备:将步骤(3)氮化钛陶瓷浆料注入模具中,缓慢加热,温度至65±3℃恒温18~20 h,自然冷却后,经干燥,脱模,得到氮化钛素坯。
在步骤(1)中所述的氮化钛粉体的粒径在0.1~0.2μm范围内。
在步骤(1)中所述的烧结助剂为三氧化二钪、氧化镁、氧化铍中的一种或两种混合。
在步骤(2)中所述的卡波姆与三异丙醇胺的质量比为1:1.3。
在步骤(4)中所述的素坯经高温烧结后得到氮化钛陶瓷。
本发明与现有技术比较,具有如下优点及有益效果:
(1)本发明是通过加热碳酸铵分解为氨提高体系的pH值,使卡波姆941低粘度凝胶,交联成为凝胶,是均相反应,可以很好的控制凝胶的均匀性,卡波姆941在pH值低时粘度小的情况下可以提高固含量,本方法固含量体积比可达55%。
(2)混料时不需要加热,注模成型后加热在碳酸铵分解作用下固化成型,所制备陶瓷的致密性可达99%。
(3)所制备的陶瓷素坯中有机物含量极少,干燥成型过程不会裂缝,所制备的素坯具有一定的强度,可以在烧结前进行加工。
(4)该方法可以制备各种复杂形状部件,可以制备大尺寸的陶瓷部件,成型的精度高。
(5)本申请中采用单烷氧基不饱和脂肪酸钛酸酯作为分散剂,既能提高固体含量,又能降低浆料的粘度。
具体实施方式
实施例1
(1)氮化钛粉体预处理:在球磨机中,分别加入,氮化钛:930g,氧化镁:10g,单烷氧基不饱和脂肪酸钛酸酯:30g,正庚醇:37 mL,开启球磨机研磨4h,干燥,得到预处理氮化钛粉体;
(2)凝胶溶液配制:在反应器中,分别加入,去离子水:960 mL,卡波姆941:18g,三异丙醇胺:22g,搅拌溶解,得到凝胶溶液;
(3)氮化钛陶瓷浆料配制:在球磨机中,分别加入,预处理氮化钛粉体:500mL,凝胶溶液:460mL,碳酸铵:40g,研磨17h,超声除泡处理,得到氮化钛陶瓷浆料;
(4)氮化钛素坯的制备:将氮化钛陶瓷浆料注入模具中,缓慢加热,温度至65±3℃恒温19 h,自然冷却后,经干燥,脱模,得到氮化钛素坯。
实施例2
(1)氮化钛粉体预处理:在球磨机中,分别加入,氮化钛:910g,氧化铍:15g,单烷氧基不饱和脂肪酸钛酸酯:40g,正庚醇:43 mL,开启球磨机研磨4h,干燥,得到预处理氮化钛粉体;
(2)凝胶溶液配制:在反应器中,分别加入,去离子水:950 mL,卡波姆941:20g,三异丙醇胺:26g,搅拌溶解,得到凝胶溶液;
(3)氮化钛陶瓷浆料配制:在球磨机中,分别加入,预处理氮化钛粉体:480 mL,凝胶溶液:470 mL,碳酸铵:50g,研磨16h,超声除泡处理,得到氮化钛陶瓷浆料;
(4)氮化钛素坯的制备:将氮化钛陶瓷浆料注入模具中,缓慢加热,温度至65±3℃恒温18 h,自然冷却后,经干燥,脱模,得到氮化钛素坯。
实施例3
(1)氮化钛粉体预处理:在球磨机中,分别加入,氮化钛:950g,三氧化二钪:2g,单烷氧基不饱和脂肪酸钛酸酯:20g,正庚醇:34 mL,开启球磨机研磨5h,干燥,得到预处理氮化钛粉体;
(2)凝胶溶液配制:在反应器中,分别加入,去离子水:970 mL,卡波姆941:13g,三异丙醇胺:17g,搅拌溶解,得到凝胶溶液;
(3)氮化钛陶瓷浆料配制:在球磨机中,分别加入,预处理氮化钛粉体:530mL,凝胶溶液:450mL,碳酸铵:20g,研磨18h,超声除泡处理,得到氮化钛陶瓷浆料;
(4)氮化钛素坯的制备:将氮化钛陶瓷浆料注入模具中,缓慢加热,温度至65±3℃恒温20 h,自然冷却后,经干燥,脱模,得到氮化钛素坯。
实施例4
(1)氮化钛粉体预处理:在球磨机中,分别加入,氮化钛:920g,氧化镁:10g,三氧化二钪:8g,单烷氧基不饱和脂肪酸钛酸酯:22g,正庚醇:49mL,开启球磨机研磨4.5h,干燥,得到预处理氮化钛粉体;
(2)凝胶溶液配制:在反应器中,分别加入,去离子水:980 mL,卡波姆941:8g,三异丙醇胺:12g,搅拌溶解,得到凝胶溶液;
(3)氮化钛陶瓷浆料配制:在球磨机中,分别加入,预处理氮化钛粉体:520mL,凝胶溶液:430mL,碳酸铵:50g,研磨17.5h,超声除泡处理,得到氮化钛陶瓷浆料;
(4)氮化钛素坯的制备:将氮化钛陶瓷浆料注入模具中,缓慢加热,温度至65±3℃恒温19.5 h,自然冷却后,经干燥,脱模,得到氮化钛素坯。
实施例5
(1)氮化钛粉体预处理:在球磨机中,分别加入,氮化钛:940g,氧化铍:10g,氧化镁:10g,单烷氧基不饱和脂肪酸钛酸酯:40g,正庚醇:24 mL,开启球磨机研磨4.5h,干燥,得到预处理氮化钛粉体;
(2)凝胶溶液配制:在反应器中,分别加入,去离子水:950 mL,卡波姆941:20g,三异丙醇胺:26g,搅拌溶解,得到凝胶溶液;
(3)氮化钛陶瓷浆料配制:在球磨机中,分别加入,预处理氮化钛粉体:490 mL,凝胶溶液:480 mL,碳酸铵:30g,研磨16.5h,超声除泡处理,得到氮化钛陶瓷浆料;
(4)氮化钛素坯的制备:将氮化钛陶瓷浆料注入模具中,缓慢加热,温度至65±3℃恒温18.5 h,自然冷却后,经干燥,脱模,得到氮化钛素坯。
本申请所制备的氮化钛素坯经过简单加工,进行高温烧结即可得到氮化钛陶瓷。所制备陶瓷的致密性可达99%。
Claims (4)
1.一种凝胶注模成型氮化钛陶瓷素坯的制备方法,其特征在于,该方法具有以下工艺步骤:
(1)氮化钛粉体预处理:在球磨机中,按质量百分比加入,氮化钛:91%~95%,烧结助剂:0.1%~2%,单烷氧基不饱和脂肪酸钛酸酯:2%~4%,正庚醇:2%~4%,各组分之和为百分之百,开启球磨机研磨3-5h,干燥,得到预处理氮化钛粉体;
(2)凝胶溶液配制:在反应器中,按质量百分浓度加入,去离子水:95%~98%,卡波姆941:0.5%~2.5%,三异丙醇胺:0.63~3.2%,各组分之和为百分之百,搅拌溶解,得到凝胶溶液;
(3)氮化钛陶瓷浆料配制:在球磨机中,按体积百分比加入,预处理氮化钛粉体:48%~53%,凝胶溶液:43%~48%,碳酸铵:2%~5%,各组分之和为百分之百,研磨16~18h,真空除泡处理,得到氮化钛陶瓷浆料;
(4)氮化钛素坯的制备:将步骤(3)氮化钛陶瓷浆料注入模具中,缓慢加热,温度至65±3℃恒温18~20 h,自然冷却后,经干燥,脱模,得到氮化钛素坯。
2.根据权利要求1所述的一种凝胶注模成型氮化钛陶瓷素坯的制备方法,其特征在于,步骤(1)中所述的氮化钛粉体的粒径在0.1~0.2μm范围内。
3.根据权利要求1所述的一种凝胶注模成型氮化钛陶瓷素坯的制备方法,其特征在于,步骤(1)中所述的烧结助剂为三氧化二钪、氧化镁、氧化铍中的一种或两种混合。
4.根据权利要求1所述的一种凝胶注模成型氮化钛陶瓷素坯的制备方法,其特征在于,步骤(2)中所述的卡波姆与三异丙醇胺的质量比为1:1.3。
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