CN108164269A - 一种模量可调控凝胶注模生坯的制作方法 - Google Patents
一种模量可调控凝胶注模生坯的制作方法 Download PDFInfo
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Abstract
本发明公布一种模量可调控凝胶注模生坯的制备方法,其制备基本过程包括:配制单分子增塑剂乳化液;配制预混液;加入陶瓷粉料;注模成型;生坯脱模、干燥。完成后,即可根据加入单分子增塑剂量的多少获得所需范围的储能模量。本发明与现有技术相比,具有以下优点:可以通过调整邻苯二甲酸二丁酯在增塑剂乳化液中的百分含量,来调整控制凝胶注模生坯的储能模量;邻苯二甲酸二丁酯是一种单分子增塑剂,将其乳化后引入凝胶注模成型体系中,不会引起凝胶注模浆料粘度升高;***树胶在本发明中既是邻苯二甲酸二丁酯的乳化剂,也是陶瓷粉末的分散剂,避免引入额外杂质。
Description
技术领域
本发明涉及一种陶瓷凝胶注模生坯制备方法,特别涉及一种模量可调控凝胶注模生坯的制备方法,属于无机材料成型领域。
背景技术
凝胶注模成型技术是美国橡树岭国家实验室在20 世纪90 年代初首先发明的一种新的陶瓷材料胶态快速成型工艺。与其他湿法成型工艺相比,该工艺具有设备简单、成型坯体组成均匀、缺陷少、不需要脱脂、不易变形、净尺寸成型复杂形状零件及实用性很强等突出优点,受到国内外学术界和工业界的极大关注。
凝胶注模成型技术较多地采用丙烯酰胺作为单体,N,N-亚甲基双丙烯酰胺作交联剂为分散在浆料中,然后将单体引发,形成聚丙烯酰胺将氧化铝颗粒紧紧固定住,得到凝胶注模生坯。通常用干燥生坯的模量大小表征凝胶注模生坯的再加工性能,模量高,说明生坯硬度高,刚性大,加工难度也随之增大;模量低,说明生坯硬度低,刚性较低,意味着生坯柔性较好,更易于进行二次加工。用丙烯酰胺体系形成的凝胶注模生坯具有较高的模量,一般在1000~100000Pa之间,意味着硬度高,刚性大,这是由于聚丙烯酰胺是极性高分子,分子力间作用力较强,因此对干燥的生坯在二次加工时,样品往往容易发生脆性断裂,加工工具也容易受到磨损,表现为二次加工成本较高、相对困难。有学者曾尝试加入高分子类增塑剂(如聚乙二醇、聚乙烯醇、PVP等)来改善其二次加工性能,但额外引入高分子,会使凝胶注模浆料粘度升高,可用固含量上限降低,牺牲了凝胶注模可用范围。
发明内容
鉴于以上提出的问题,本发明提供了一种模量可调控凝胶注模生坯的制作方法。本发明制备陶瓷凝胶注模生坯是有良好塑性的生坯,该生坯模量通过单分子增塑剂的添加比例进行调节(20-600Pa),意味着其加工可塑能力可以根据实际需要进行控制,同时,在整个凝胶注模成型过程中,不会使凝胶注模浆料粘度升高,不会降低可用固含量上限。
本发明提出的塑性可调控凝胶注模生坯的制作方法包括以下步骤:
(1)配制单分子增塑剂乳化液:取一定量的去离子水、单分子增塑剂、乳化剂放在球磨罐中,球磨混合10-22h,获得乳白色均匀悬浊液;
(2)配制预混液:计算好配比,取一定量步骤(1)中获得的乳浊液,向其中加入分散剂、有机单体、交联剂,放入球磨罐中球磨15-35min,调节至合适的pH值,配成预混液;
(3)加入陶瓷粉料:计算配比,取一定量步骤(2)中获得的预混液,将所需含量的陶瓷粉末及烧结助剂粉料与预混液加入到球磨罐中,球磨8-30h,得到一定固含量的凝胶注模浆料;
(4)注模成型:在一定温度下,将球磨罐中的浆料倒入引发反应容器,静置5-30min,将一定量的催化剂、引发剂依次加入浆料中,搅拌均匀后注入所需的模具中,静置10-60min,待其成型;
(5)生坯脱模、干燥:将成型后的生坯脱模,然后放置在特定环境中,干燥5-20天,获得加工性能良好的干燥生坯。
在上述制作方法中,所述单分子增塑剂为邻苯二甲酸二丁酯,乳化剂为***树胶,分散剂为***树胶,有机单体为丙烯酰胺,交联剂为N,N-亚甲基双丙烯酰胺,催化剂为四甲基乙二胺,引发剂为12wt%过硫酸铵水溶液,球磨机为滚筒球磨机。
在上述制作方法步骤(1)中,单分子增塑剂与离子水质量比为(0.1-15):100,单分子增塑剂与乳化剂质量比为(2-5):1,球磨机转速为25-35r/min。
在上述制作方法步骤(2)中,分散剂的加入量为陶瓷粉料的0.5-5wt%,有机单体加入量为乳浊液的10-40wt%,有机单体与交联剂质量比为(10-20):1,用氨水调节PH至7-12。
在上述制作方法步骤(3)中,所述陶瓷粉料包括氧化铝,氧化锆,碳化硅,纯度不低于99%,粒径不大于100μm,最终获得凝胶注模体积固含量为25~57vol%。
在上述制作方法步骤(4)中,所述注模成型环境温度为25℃,引发剂与催化剂加入量之比为3:2,引发剂质量为步骤(2)中有机单体质量的1~5wt%。
在上述制作方法步骤(5)中,干燥环境具体为无阳光直射,温度25℃,湿度95%,干燥后的生坯,以模量大小表征其二次加工能力的强弱。
本发明涉及一种塑性可调控凝胶注模生坯的制作方法,与现有技术相比,具有以下优点:
(1)本发明中,可以通过调整邻苯二甲酸二丁酯在增塑剂乳化液中的百分含量,来调整凝胶注模生坯的模量(20-600Pa)和可塑性,并以此根据实际需求调整生坯二次加工性能;
(2)本发明中,利用滚动式球磨机进行邻苯二甲酸二丁酯乳化过程,所得增塑剂乳化液在7-15天内保持均匀且物化性质稳定;
(3)本发明中,邻苯二甲酸二丁酯是一种单分子增塑剂,将其乳化后引入凝胶注模成型体系中,不会引起凝胶注模浆料粘度升高,因此不会降低可用固含量上限;
(4)本发明中,***树胶既是邻苯二甲酸二丁酯的乳化剂,也是陶瓷粉末的分散剂,避免引入额外杂质,保持本体系的稳定性;
(5)本发明适用于不同形状以及不同陶瓷种类的生坯二次加工,尤其适用于复杂形状陶瓷生坯的二次加工和生产;
(6)本发明操作简单,易于制备,所用增塑剂和成型助剂价格低廉,方便工业化推广。
具体实施方式
实施例1:低模量高固相含量氧化铝凝胶注模生坯的制备:
(1)配制单分子增塑剂乳化液:取100ml去离子水,2.5g邻苯二甲酸二丁酯,1g***树胶放在球磨罐中球磨15h,获得乳白色均匀悬浊液;
(2)配制预混液:将7.3g***树胶、18g丙烯酰胺单体、1.5gN,N-亚甲基双丙烯酰胺与步骤(1)中的增塑剂乳化液混合,放入球磨罐球磨20min,用氨水调节PH值至9;
(3)加陶瓷粉料:取510g氧化铝粉,27g烧结助剂(包括二氧化钛和氧化镁),与步骤(2)中得到的预混液一起加入到球磨罐中,球磨22h,得到粘度极低(0.2pa.s)的氧化铝凝胶注模浆料;
(4)注模成型:在25℃环境下,将所得到的凝胶注模浆料放在大烧杯中静置10min,依次加入催化剂0.4g,引发剂12wt%过硫酸铵水溶液0.6g,搅拌均匀后注入模具中,静置30min;
(5)生坯脱模、干燥:打开模具,取出其中的生坯,在无阳光直射,温度25℃,湿度95%的环境中干燥12天,获得干燥生坯,测得其模量为220Pa,柔性较好,刚性小,满足二次加工性能需求。
实施例2:中等模量高固相含量氧化铝凝胶注模生坯的制备:
(1)配制单分子增塑剂乳化液:取100ml去离子水,0.5g邻苯二甲酸二丁酯,1g***树胶放在球磨罐中球磨15h,获得乳白色均匀悬浊液;
(2)配制预混液:将7.3g***树胶、18g丙烯酰胺单体、1.5gN,N-亚甲基双丙烯酰胺与步骤(1)中的增塑剂乳化液混合,放入球磨罐球磨20min,用氨水调节PH值至9;
(3)加陶瓷粉料:取510g氧化铝粉,27g烧结助剂(包括二氧化钛和氧化镁),与步骤(2)中得到的预混液一起加入到球磨罐中,球磨22h,得到粘度极低(260mpa.s)的氧化铝凝胶注模浆料;
(4)注模成型:在25℃环境下,将所得到的凝胶注模浆料放在大烧杯中静置10min,依次加入催化剂0.4g,引发剂12wt%过硫酸铵水溶液0.6g,搅拌均匀后注入模具中,静置30min;
(5)生坯脱模、干燥:打开模具,取出其中的生坯,在无阳光直射,温度25℃,湿度95%的环境中干燥12天,获得干燥生坯,测得其模量为500Pa,同实施例(1)比较,只改变邻苯二甲酸二丁酯的添加量,其模量发生相应变化,此时生坯表现为柔性一般,刚性一般,但依然满足二次加工性能需求。
实施例3:极低模量高固相含量3Y-ZrO2凝胶注模生坯:
(1)配制单分子增塑剂乳化液:取50ml去离子水,3g邻苯二甲酸二丁酯,1.5g***树胶放在球磨罐中球磨20h,获得乳白色均匀悬浊液;
(2)配制预混液:将3.5g***树胶、8.5g丙烯酰胺单体、0.6gN,N-亚甲基双丙烯酰胺与步骤(1)中的增塑剂乳化液混合,放入球磨罐球磨18min,用氨水调节PH值至10;
(3)加陶瓷粉料:取250g3Y-ZrO2瓷粉,与步骤(2)中得到的预混液一起加入到球磨罐中,球磨19h,得到粘度极低(0.1pa.s)的氧化铝凝胶注模浆料;
(4)注模成型:在25℃环境下,将所得到的3Y-ZrO2凝胶注模浆料放在大烧杯中静置7min,依次加入催化剂0.2g,引发剂12wt%过硫酸铵水溶液0.3g,搅拌均匀后注入模具中,静置25min;
(5)生坯脱模、干燥:打开模具,取出其中的生坯,在无阳光直射,温度25℃,湿度95%的环境中干燥9天,获得干燥生坯,测得其模量为95Pa,柔性较好,满足二次加工性能需求。
Claims (7)
1.一种模量可调控凝胶注模生坯的制备方法,其特征在于,包括以下步骤:
(1)配制单分子增塑剂乳化液:取一定量的去离子水、单分子增塑剂、乳化剂放在球磨罐中,球磨混合10-22h,获得乳白色均匀悬浊液;
(2)配制预混液:计算好配比,取一定量步骤(1)中获得的乳浊液,向其中加入分散剂、有机单体、交联剂,放入球磨罐中球磨15~35min,调节至合适的PH值,配成预混液;
(3)加入陶瓷粉料:计算配比,取一定量步骤(2)中获得的预混液,将所需含量的陶瓷粉末及烧结助剂粉料与预混液加入到球磨罐中,球磨8-30h,得到一定固含量的凝胶注模浆料;
(4)注模成型:在一定温度下,将球磨罐中的浆料倒入引发反应容器,静置5-30min,将一定量的催化剂、引发剂依次加入浆料中,搅拌均匀后注入所需的模具中,静置10-60min,待其成型;
(5)生坯脱模、干燥:将成型后的生坯脱模,然后放置在特定环境中,干燥5-20天,获得加工性能良好的干燥生坯。
2.根据权利要求1所述一种模量可调控凝胶注模生坯的制备方法,其特征在于,所述单分子增塑剂为邻苯二甲酸二丁酯,乳化剂为***树胶,分散剂为***树胶,有机单体为丙烯酰胺,交联剂为N,N-亚甲基双丙烯酰胺,催化剂为四甲基乙二胺,引发剂为12wt%过硫酸铵水溶液,球磨机为滚筒球磨机。
3.根据权利要求1所述一种模量可调控凝胶注模生坯的制备方法,其特征在于,步骤(1)中,单分子增塑剂与离子水质量比为(0.1-15):100,单分子增塑剂与乳化剂质量比为(2-5):1,球磨机转速为25-35r/min。
4.根据权利要求1所述一种模量可调控凝胶注模生坯的制备方法,其特征在于,步骤(2)中,分散剂的加入量为陶瓷粉料的0.5-5wt%,有机单体加入量为乳浊液的10-40wt%,有机单体与交联剂质量比为(10-20):1,用氨水调节PH至7-12。
5.根据权利要求1所述一种模量可调控凝胶注模生坯的制备方法,其特征在于,步骤(3)中,所述陶瓷粉料包括氧化铝,氧化锆,碳化硅,纯度不低于99%,粒径不大于100μm,最终获得凝胶注模体积固含量为25~57vol%。
6.根据权利要求1所述一种模量可调控凝胶注模生坯的制备方法,其特征在于,步骤(4)中,所述注模成型环境温度为25℃,引发剂与催化剂加入量之比为3:2,引发剂质量为步骤(2)中有机单体质量的1~5wt%。
7.根据权利要求1所述一种模量可调控凝胶注模生坯的制备方法,其特征在于,步骤(5)中,干燥环境具体为无阳光直射,温度25℃,湿度95%,干燥后的生坯,以模量大小表征其二次加工能力的强弱。
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