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 PDF

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CN108164269A
CN108164269A CN201711475577.8A CN201711475577A CN108164269A CN 108164269 A CN108164269 A CN 108164269A CN 201711475577 A CN201711475577 A CN 201711475577A CN 108164269 A CN108164269 A CN 108164269A
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李蔚
彭华庆
孙小曼
刘会娇
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East China University of Science and Technology
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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；阿拉伯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

一种模量可调控凝胶注模生坯的制作方法
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，乳化剂为阿拉伯树胶，分散剂为阿拉伯树胶，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，阿拉伯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阿拉伯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阿拉伯树胶、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阿拉伯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阿拉伯树胶、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阿拉伯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阿拉伯树胶、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，乳化剂为阿拉伯树胶，分散剂为阿拉伯树胶，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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* Cited by examiner, † Cited by third party
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CN112456978A (zh) * 2020-11-25 2021-03-09 上海三思电子工程有限公司 一种陶瓷浆料及其制备方法和用途
CN112500151A (zh) * 2020-11-30 2021-03-16 华南理工大学 一种具有复杂结构的生物活性陶瓷支架与柔性可调的三维生坯及其制备方法
CN116023124A (zh) * 2023-03-28 2023-04-28 成都超纯应用材料有限责任公司 一种基于注凝成型的氧化铝陶瓷及其制备方法
CN117303914A (zh) * 2023-11-30 2023-12-29 山东合创明业精细陶瓷有限公司 塑性陶瓷素坯的制备方法

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112456978A (zh) * 2020-11-25 2021-03-09 上海三思电子工程有限公司 一种陶瓷浆料及其制备方法和用途
CN112500151A (zh) * 2020-11-30 2021-03-16 华南理工大学 一种具有复杂结构的生物活性陶瓷支架与柔性可调的三维生坯及其制备方法
CN116023124A (zh) * 2023-03-28 2023-04-28 成都超纯应用材料有限责任公司 一种基于注凝成型的氧化铝陶瓷及其制备方法
CN117303914A (zh) * 2023-11-30 2023-12-29 山东合创明业精细陶瓷有限公司 塑性陶瓷素坯的制备方法
CN117303914B (zh) * 2023-11-30 2024-03-15 山东合创明业精细陶瓷有限公司 塑性陶瓷素坯的制备方法

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