CN111233488B - 表面改性的氧化锆注射成型溶剂脱脂喂料及其制备方法和应用 - Google Patents

表面改性的氧化锆注射成型溶剂脱脂喂料及其制备方法和应用 Download PDF

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CN111233488B
CN111233488B CN202010112736.3A CN202010112736A CN111233488B CN 111233488 B CN111233488 B CN 111233488B CN 202010112736 A CN202010112736 A CN 202010112736A CN 111233488 B CN111233488 B CN 111233488B
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CN111233488A (zh
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李志强
刘策
杨瑶刚
付珂
高笑
王德昌
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Changyu Holding Group Co ltd
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Abstract

本发明属于氧化锆陶瓷注射成型技术领域，具体涉及一种表面改性的氧化锆注射成型溶剂脱脂喂料及其制备方法和应用。所述的喂料由改性的氧化锆粉体与粘结剂制成，所述改性的氧化锆粉体与粘结剂的质量比为82～91:9～18；所述的粘结剂中表面活性剂、骨架树脂、弹性体树脂、润滑助剂和增塑剂的质量比为：3～6:25～35:8～15:38～61:3～6；氧化锆粉体经改性后表面呈碱性，可以与酸性的表面活性剂更好地结合。本发明采用的粘结剂之间相容性较好，且骨架粘结剂在高温下，对坯体强度的支撑性良好，且粘结剂采用多种不同的组分，可以满足不同产品的使用需求；同时提供的制备方法，更利于改性的氧化锆粉体与粘结剂的均匀混合。

Description

表面改性的氧化锆注射成型溶剂脱脂喂料及其制备方法和 应用
技术领域
本发明属于氧化锆陶瓷注射成型技术领域，具体涉及一种表面改性的氧化锆注射成型溶剂脱脂喂料及其制备方法和应用。
背景技术
结构陶瓷是指主要由离子键、共价键结合的一类先进陶瓷材料，具有高强度、高硬度、耐高温、耐磨损、耐腐蚀等优异性能。这类材料在国内外已经得到了广泛的应用，遍及化工、冶金、机械等领域和人们的日常生活。在最近的20年里，结构陶瓷在航空航天、通信电子、生物医学、国防军工等高科技领域也获得越来越多的应用，氧化锆作为其中的优异代表，更是受到了广泛的关注。
溶剂萃取脱脂是最新发展起来的一种新型脱脂工艺。溶剂脱脂的粘结剂范围两部分，一部分是易溶于某些溶剂的低分子物质，另一部分是不溶于溶剂的高分子。在脱脂过程中，低分子物质溶解后，高分子可起到支撑坯体强度的作用。残存的有机载体和溶剂可最后通过快速加热完全除去。
氧化锆陶瓷注射成型溶剂脱脂喂料对于粘结剂的选择很严格，且过程工艺复杂，易产生溶胀、裂纹等缺陷。
发明内容
本发明要解决的技术问题是：克服现有技术的不足，提供一种表面改性的氧化锆注射成型溶剂脱脂喂料，通过对氧化锆粉体的表面改性，同时本发明还提供其制备方法使得与粘结剂之间混合的更加均匀，科学合理，简单易操作，本发明粘结剂采用多种不同的组分，可以满足不同产品的使用需求。
本发明是采用以下技术方案实现的：
所述的表面改性的氧化锆注射成型溶剂脱脂喂料，由改性的氧化锆粉体与粘结剂制成，所述改性的氧化锆粉体与粘结剂的质量比为82～91:9～18；其中，所述的粘结剂包括表面活性剂、骨架树脂、弹性体树脂、润滑助剂和增塑剂；
所述的改性的氧化锆粉体的制备方法，包括以下步骤：
(1)将氧化锆与纯水进行混合，形成混合的氧化锆浆料；
(2)将氨水加入到步骤(1)中的氧化锆浆料中，调节pH值为8±0.5，形成碱性的氧化锆浆料；
(3)将步骤(2)得到碱性的氧化锆浆料烘干脱去水分后，得到改性的氧化锆粉体。
步骤(1)中所述的氧化锆与纯水的质量比为1:2～3。
所述的表面活性剂、骨架树脂、弹性体树脂、润滑助剂和增塑剂的质量比为3～6:25～35:8～15:38～61:3～6。
所述的表面活性剂为硬脂酸或聚山梨酯中的一种或两种。
所述的骨架树脂为聚丙烯、高密度聚乙烯、低密度聚乙烯、线性低密度聚乙烯或聚苯乙烯中的一种或多种。
所述的弹性体树脂为苯乙烯类热塑性弹性体、聚氨酯类热塑性弹性体或聚烯烃类热塑性弹性体中的一种或多种。
所述的润滑助剂为石蜡、微晶石蜡或巴西棕榈蜡中的一种或多种。
所述的增塑剂为二甘醇二苯甲酸酯。
本发明所述的表面改性的氧化锆注射成型溶剂脱脂喂料的制备方法，包括以下步骤：
(1)配料：按比例将改性的氧化锆粉体与粘结剂各组分称量后分别置于容器中；
(2)部分粘结剂的预混：将骨架树脂、弹性体树脂、润滑助剂在200℃～250℃混合20min～30min，然后冷却切块备用，得到预混后的粘结剂；
(3)喂料的密炼：密炼机温度设置为150℃～200℃，加入1/2质量的改性的氧化锆粉体，加入表面活性剂，设置转速10r/min～30r/min，混合40min～60min，然后加入步骤(2)得到的预混后的粘结剂，混合10min～15min，然后加入剩余1/2质量的改性的氧化锆粉体，混合10min～15min，然后加入增塑剂，混合120min～150min；
(4)喂料的造粒：将混合好的团状喂料置于造粒机中，设置温度140～150℃，挤出转速10～20r/min，切粒转速10～20r/min，得到造粒后的喂料，即得表面改性的氧化锆注射成型溶剂脱脂喂料。
本发明所述的表面改性的氧化锆注射成型溶剂脱脂喂料的应用，用于制作陶瓷注射成型坯件，制备方法包括以下步骤：
(1)生坯的溶剂脱脂：将所述的表面改性的氧化锆注射成型溶剂脱脂喂料造粒后，采用注射成型机成型为陶瓷生坯，然后在50～60℃煤油中浸泡40～50h，得到溶脱后的产品；
(2)热脱脂后烧结：将溶脱后的产品在脱脂炉进行脱脂，然后在烧结炉进行烧结，得到最终的陶瓷毛坯。
与现有技术相比，本发明的有益效果如下：
1、本发明通过对氧化锆粉体进行改性，使得氧化锆粉体经改性后表面呈碱性，可以与酸性的表面活性剂更好地结合。
2、本发明采用的粘结剂之间相容性较好，且骨架粘结剂在高温下，对坯体强度的支撑性良好。
3、本发明提供的制备方法，更利于改性的氧化锆粉体与粘结剂的均匀混合。
具体实施方式
下面结合实施例对本发明作进一步的说明。
实施例中用到的所有原料，若无特殊说明均为市购。
实施例1
将氧化锆粉体的表面进行改性，具体实施步骤是：
步骤1，将氧化锆与纯水按质量比1:3在容器中进行混合，形成混合的氧化锆浆料；
步骤2，将氨水加入到氧化锆浆料中，边加入边搅拌，调节pH值在8±0.5的范围内，形成碱性的氧化锆浆料；
步骤3，将氧化锆浆料在烘箱中烘干，脱去水分，得到改性的氧化锆粉体。
实施例2
将实施例1制备的改性的氧化锆粉体与粘结剂按质量比为82:18配料，其中，粘结剂中硬脂酸、聚丙烯、高密度聚乙烯、聚苯乙烯、苯乙烯类热塑性弹性体、全精炼石蜡、二甘醇二苯甲酸酯重量比为3:8:10:7:8:61:3，按照配比称量，得到本实施例的喂料组成。
实施例3
将实施例1制备的改性的氧化锆粉体与粘结剂比例为83:17，其中，粘结剂中聚山梨酯、低密度聚乙烯、线性低密度聚乙烯、聚氨酯类热塑性弹性体、微晶石蜡、巴西棕榈蜡、二甘醇二苯甲酸酯重量比为6:17:18:15:30:8:6，按照配比称量，得到本实施例的喂料组成。
实施例4
将实施例1制备的改性的氧化锆粉体与粘结剂比例为84:16，其中，粘结剂中硬脂酸、聚丙烯、聚苯乙烯、聚烯烃类热塑性弹性体、微晶石蜡、二甘醇二苯甲酸酯重量比为3:10:11:15:55:6，按照配比称量，得到本实施例的喂料组成。
实施例5
将实施例1制备的改性的氧化锆粉体与粘结剂比例为85:15，其中粘结剂中硬脂酸、聚山梨酯、高密度聚乙烯、线性低密度聚乙烯、苯乙烯类热塑性弹性体、聚氨酯类热塑性弹性体、巴西棕榈蜡、二甘醇二苯甲酸酯重量比为2:1:18:9:3:7:54:6，按照配比称量，得到本实施例的喂料组成。
实施例6
将实施例1制备的改性的氧化锆粉体与粘结剂比例为86:14，其中，粘结剂中聚山梨酯、聚丙烯、低密度聚乙烯、苯乙烯类热塑性弹性体、聚烯烃类热塑性弹性体、全精炼石蜡、巴西棕榈蜡、二甘醇二苯甲酸酯重量比为4:15:15:6:6:20:28:6，按照配比称量，得到本实施例的喂料组成。
实施例7
将实施例1制备的改性的氧化锆粉体与粘结剂比例为87:13，其中，粘结剂中硬脂酸、聚丙烯、高密度聚乙烯、聚氨酯类热塑性弹性体、聚烯烃类热塑性弹性体、全精炼石蜡、微晶石蜡、二甘醇二苯甲酸酯重量比为4:13:16:4:8:18:32:5，按照配比称量，得到本实施例的喂料组成。
实施例8
将实施例1制备的改性的氧化锆粉体与粘结剂比例为88:12，其中，粘结剂中聚山梨酯、聚丙烯、线性低密度聚乙烯、苯乙烯类热塑性弹性体、全精炼石蜡、微晶石蜡、巴西棕榈蜡、二甘醇二苯甲酸酯重量比为5:8:20:11:17:20:14:5，按照配比称量，得到本实施例的喂料组成。
实施例9
将实施例1制备的改性的氧化锆粉体与粘结剂比例为89:11，其中，粘结剂中硬脂酸、聚山梨酯、高密度聚乙烯、聚苯乙烯、聚氨酯类热塑性弹性体、全精炼石蜡、二甘醇二苯甲酸酯重量比为1:4:13:19:8:9:41:5，按照配比称量，得到本实施例的喂料组成。
实施例10
将实施例1制备的改性的氧化锆粉体与粘结剂比例为90:10，其中，粘结剂中硬脂酸、高密度聚乙烯、线性低密度聚乙烯、聚烯烃类热塑性弹性体、全精炼石蜡、二甘醇二苯甲酸酯重量比为6:7:9:14:60:4，按照配比称量，得到本实施例的喂料组成。
实施例11
将实施例1制备的改性的氧化锆粉体与粘结剂比例为91:9，其中，粘结剂中聚山梨酯、高密度聚乙烯、线性低密度聚乙烯、聚苯乙烯、苯乙烯类热塑性弹性体、聚烯烃类热塑性弹性体、巴西棕榈蜡、二甘醇二苯甲酸酯重量比为6:7:6:20:5:10:42:4，按照配比称量，得到本实施例的喂料组成。
实施例12
将实施例2、实施例3和实施例4配比的改性的氧化锆粉体与粘结剂喂料组成进行造粒并制成陶瓷坯体，具体实施步骤如下：
步骤1，粉体和粘结剂的称量；按比例将粉体与粘结剂称量后分别置于容器中；
步骤2，部分粘结剂的预混；将骨架树脂、弹性体树脂、润滑助剂在200℃混合20min；
步骤3，喂料的密炼；密炼机温度设置为150℃，加入1/2的氧化锆粉体，加入表面活性剂，设置转速10r/min，混合40min，然后加入预混后的粘结剂，混合10min，然后加入剩余3/4氧化锆粉体，混合10min，然后加入增塑剂，混合120min；
步骤4，喂料的造粒；将混合好的团装喂料置于造粒机中，设置温度150℃，挤出转速10r/min，切粒转速10r/min，得到造粒后的喂料。
步骤5，生坯的溶剂脱脂；将喂料在注射成型机成型为陶瓷生坯，然后在50℃煤油中浸泡40h，得到溶脱后的产品；
步骤6，热脱脂烧结；将溶脱后的产品在脱脂炉进行脱脂，然后在烧结炉进行烧结，得到最终的陶瓷毛坯。
实施例13
将实施例5、实施例6和实施例7配比的改性的氧化锆粉体与粘结剂喂料组成进行造粒并制成陶瓷坯体，具体实施步骤如下：
步骤1，粉体和粘结剂的称量；按比例将粉体与粘结剂称量后分别置于容器中；
步骤2，部分粘结剂的预混；将骨架树脂、弹性体树脂在225℃混合25min；
步骤3，喂料的密炼；密炼机温度设置为200℃，加入1/2的氧化锆粉体，加入表面活性剂，设置转速30r/min，混合60min，然后加入预混后的粘结剂，混合15min，然后加入剩余1/2氧化锆粉体，混合15min，然后加入增塑剂，混合150min；
步骤4，喂料的造粒；将混合好的团装喂料置于造粒机中，设置温度140℃，挤出转速10r/min，切粒转速10r/min，得到造粒后的喂料。
步骤5，生坯的溶剂脱脂；将喂料在注射成型机成型为陶瓷生坯，然后在50℃煤油中浸泡40h，得到溶脱后的产品；
步骤6，热脱脂烧结；将溶脱后的产品在脱脂炉进行脱脂，然后在烧结炉进行烧结，得到最终的陶瓷毛坯。
实施例14
将按实施例8、实施例9、实施例10和实施例11配比的氧化锆粉体与粘结剂喂料组成进行造粒并制成陶瓷坯体，具体实施步骤如下：
步骤1，粉体和粘结剂的称量；按比例将粉体与粘结剂称量后分别置于容器中；
步骤2，部分粘结剂的预混；将骨架树脂、弹性体树脂在180℃混合25min；
步骤3，喂料的密炼；密炼机温度设置为170℃，加入1/2的氧化锆粉体，加入表面活性剂，设置转速20r/min，混合50min，然后加入预混后的粘结剂，混合12min，然后加入剩余1/2氧化锆粉体，混合12min，然后加入增塑剂，混合130min；
步骤4，喂料的造粒；将混合好的团装喂料置于造粒机中，设置温度150℃，挤出转速20r/min，切粒转速20r/min，得到造粒后的喂料。
步骤5，生坯的溶剂脱脂；将喂料在注射成型机成型为陶瓷生坯，然后在60℃煤油中浸泡50h，得到溶脱后的产品；
步骤6，热脱脂烧结；将溶脱后的产品在脱脂炉进行脱脂，然后在烧结炉进行烧结，得到最终的陶瓷毛坯。
将实施例2～11用于制备相同的氧化锆陶瓷产品，对比产品的性能，结果如表1所示。结果表明，依本专利工艺流程制作的陶瓷产品结构致密，性能优异。
表1实施例2～11制备的氧化锆陶瓷产品性能测试结果
实施例 密度(g/cm3) 强度(MPa) 韧性(MPa·m1/2) 硬度
2 6.04 1267 8.6 1375
3 6.04 1292 8.3 1409
4 6.05 1223 8.5 1298
5 6.03 1197 8.6 1305
6 6.04 1390 8.9 1285
7 6.03 1362 9.2 1429
8 6.03 1099 8.4 1402
9 6.05 1183 8.8 1359
10 6.04 1263 9.0 1292
11 6.04 1206 8.4 1396
当然，上述内容仅为本发明的较佳实施例，不能被认为用于限定对本发明的实施例范围。本发明也并不仅限于上述举例，本技术领域的普通技术人员在本发明的实质范围内所做出的均等变化与改进等，均应归属于本发明的专利涵盖范围内。

Claims (3)

1.一种表面改性的氧化锆注射成型溶剂脱脂喂料，其特征在于：由改性的氧化锆粉体与粘结剂制成，所述改性的氧化锆粉体与粘结剂的质量比为82～91:9～18；其中，所述的粘结剂包括表面活性剂、骨架树脂、弹性体树脂、润滑助剂和增塑剂；
所述的改性的氧化锆粉体的制备方法，包括以下步骤：
(1)将氧化锆与纯水进行混合，形成混合的氧化锆浆料；
(2)将氨水加入到步骤(1)中的氧化锆浆料中，调节pH值为8±0.5，形成碱性的氧化锆浆料；
(3)将步骤(2)得到碱性的氧化锆浆料烘干脱去水分后，得到改性的氧化锆粉体；
步骤(1)中所述的氧化锆与纯水的质量比为1:2～3；
所述的表面活性剂、骨架树脂、弹性体树脂、润滑助剂和增塑剂的质量比为3～6:25～35:8～15:38～61:3～6；
所述的弹性体树脂为苯乙烯类热塑性弹性体、聚氨酯类热塑性弹性体或聚烯烃类热塑性弹性体中的一种或多种；
所述的增塑剂为二甘醇二苯甲酸酯；
所述的表面改性的氧化锆注射成型溶剂脱脂喂料的制备方法，包括以下步骤：
(1)配料：将改性的氧化锆粉体与粘结剂各组分称量后分别置于容器中；
(2)部分粘结剂的预混：将骨架树脂、弹性体树脂、润滑助剂在200℃～250℃混合20min～30min，然后冷却切块备用，得到预混后的粘结剂；
(3)喂料的密炼：密炼机温度设置为150℃～200℃，加入1/2质量的改性的氧化锆粉体，加入表面活性剂，设置转速10r/min～30r/min，混合40min～60min，然后加入步骤(2)得到的预混后的粘结剂，混合10min～15min，然后加入剩余1/2质量的改性的氧化锆粉体，混合10min～15min，然后加入增塑剂，混合120min～150min；
(4)喂料的造粒：将混合好的团状喂料置于造粒机中，设置温度140～150℃，挤出转速10～20r/min，切粒转速10～20r/min，得到造粒后的喂料，即得表面改性的氧化锆注射成型溶剂脱脂喂料；
所述的表面改性的氧化锆注射成型溶剂脱脂喂料的应用，用于制作陶瓷注射成型坯件，包括以下步骤：
(1)生坯的溶剂脱脂：将所述的表面改性的氧化锆注射成型溶剂脱脂喂料造粒后，采用注射成型机成型为陶瓷生坯，然后在50～60℃煤油中浸泡40～50h，得到溶脱后的产品；
(2)热脱脂后烧结：将溶脱后的产品在脱脂炉进行脱脂，然后在烧结炉进行烧结，得到最终的陶瓷毛坯；
所述的表面活性剂为硬脂酸或聚山梨酯中的一种或两种。
2.根据权利要求1所述的表面改性的氧化锆注射成型溶剂脱脂喂料，其特征在于：所述的骨架树脂为聚丙烯、高密度聚乙烯、低密度聚乙烯、线性低密度聚乙烯或聚苯乙烯中的一种或多种。
3.根据权利要求1所述的表面改性的氧化锆注射成型溶剂脱脂喂料，其特征在于：所述的润滑助剂为石蜡、微晶石蜡或巴西棕榈蜡中的一种或多种。
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