CN114736009B - 一种注射成型氧化铝基陶瓷件复合物料及其制备方法 - Google Patents
一种注射成型氧化铝基陶瓷件复合物料及其制备方法 Download PDFInfo
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Abstract
本发明涉及氧化铝材料技术领域,尤其涉及一种注射成型氧化铝基陶瓷件复合物料及其制备方法。所述复合物料由以下原料组成:氧化铝200~250份、硅烷偶联剂10~20份、钛酸脂偶联剂5~10份、钛酸金属8~15份、助烧剂15~28份、增塑剂10~20份、分散剂5~7份、粘结剂10~20份、脱模剂1~3份、有机溶剂18~25份。本发明通过在对氧化铝使用硅烷偶联剂以及钛酸脂偶联剂进行改性,不仅能改善陶瓷件的抗弯强度、断裂韧性、硬度、体积密度等力学性能,还能进一步提高陶瓷件的抗热震性,提高了陶瓷件在复杂温度环境下的整体可靠性。
Description
技术领域
本发明涉及氧化铝材料技术领域,尤其涉及一种注射成型氧化铝基陶瓷件复合物料及其制备方法。
背景技术
氧化铝陶瓷是一种性能优异的高温结构陶瓷,由于具有硬度大,耐磨损、耐化学腐蚀,原料便宜等特点,成为目前应用最为广泛的结构陶瓷之一。但是由于氧化铝陶瓷硬度高,脆性大,难以加工,在精密结构陶瓷成型技术中,传统的干压、热压铸等陶瓷成型工艺中,制备的陶瓷具有尺寸精度低、气孔多,致密度不高,只适合于生产结构简单,精度要求不高,低附加值的陶瓷制品,难以满足高性能氧化铝陶瓷零部件的生产要求。由于陶瓷注射成型具有自动化程度高,可生产形状复杂,成型的产品无需机加工或少加工,制成的产品具有极高的尺寸精度及表面光洁度,在氧化铝陶瓷成型工艺中得到广泛应用。
目前的氧化铝陶瓷注射成型技术,根据粘结剂体系的不同主要分为蜡基体系、水基体系、塑基体系等。其脱脂方式也不尽相同。其中,蜡基体系可单独进行直接热脱脂,也可以溶剂和热脱脂两者相结合的方式进行脱脂。其中,溶剂脱脂和热脱脂两者相结合的方式进行脱脂,具有脱脂效率高,脱脂时间短等优点,但是溶剂脱脂使用的有机溶剂如正庚烷、四氯乙烷等存在有毒、环保等问题。而直接热脱脂具有工艺简单,操作方便环保等优点,缺点是脱脂时间长,效率低,容易引起变形鼓包等缺陷。并且该材料体系成型的陶瓷生坯在排胶过程中易变形、致密度低,不易成型脱模。
基于上述情况,本发明提出了一种注射成型氧化铝基陶瓷件复合物料及其制备方法,可有效解决以上问题。
发明内容
本发明的目的在于提供一种注射成型氧化铝基陶瓷件复合物料及其制备方法。
为实现上述目的,本发明提供了一种注射成型氧化铝基陶瓷件复合物料,所述复合物料由以下原料组成:氧化铝200~250份、硅烷偶联剂10~20份、钛酸脂偶联剂5~10份、钛酸金属8~15份、助烧剂15~28份、增塑剂10~20份、分散剂5~7份、粘结剂10~20份、脱模剂1~3份、有机溶剂18~25份。
优选地,所述钛酸脂偶联剂包括三硬脂酸钛酸异丙酯、异丙基三油酸酰氧基钛酸酯、二异丙氧基二乙酰丙酮钛酸酯、双(二辛氧基焦磷酸酯基)乙撑钛酸酯的其中一种或两种以上的组合。
优选地,所述硅烷偶联剂包括KH550、KH560、KH570、KH590的其中一种或两种以上的组合。
优选地,所述钛酸金属为钛酸锶与钛酸铋的组合。
优选地,所述助烧剂为稀土氧化物,包括氧化钇、氧化钙、氧化铌、氧化铈、氧化钐、氧化镧中的至少一种或两种以上的组合。
优选地,所述增塑剂包括邻苯二甲酸二丁酯、邻苯二甲酸二辛酯、乙二醇、丙三醇的至少一种或两种以上的组合。
优选地,所述分散剂包括硬脂酸、油酸、羧基硬脂酸中的至少一种或两种以上的组合。
优选地,所述粘结剂为聚乙烯醇缩丁醛、聚乙二醇、聚甲基丙烯酸甲酯、聚甲基丙烯酸乙酯中的至少一种或两种以上的组合。
优选地,所述脱模剂包括乙撑双硬脂酰胺、石蜡、棕榈蜡的至少一种或两种以上的组合。
优选地,所述有机溶剂包括甲基乙基酮、无水乙醇、丙酮、异丙醇、乙酸乙酯、正己烷、环己烷的至少一种或两种以上的组合。
优选地,所述复合物料由以下原料组成:氧化铝200份、硅烷偶联剂10份、钛酸脂偶联剂5份、钛酸金属8份、助烧剂15份、增塑剂10份、分散剂5份、粘结剂10份、脱模剂1份、有机溶剂18份。
优选地,所述复合物料由以下原料组成:氧化铝250份、硅烷偶联剂20份、钛酸脂偶联剂10份、钛酸金属15份、助烧剂28份、增塑剂20份、分散剂7份、粘结剂20份、脱模剂3份、有机溶剂25份。
本发明还提供一种注射成型氧化铝基陶瓷件复合物料的制备方法,所述制备方法包括以下步骤:
(1)将氧化铝加入球磨机球磨,待粉体粒度达到1~5μm时,加入硅烷偶联剂继续球磨1~2h,随后加入钛酸脂偶联剂继续球磨1~2h,得到浆料A;
(2)将钛酸金属、助烧剂、粘结剂、增塑剂、有机溶剂加入到浆料A中,继续球磨1~2h得到浆料B;
(3)将浆料B、分散剂、脱模剂放入混炼机中,在180℃~220℃下均匀混炼3~4次,每次混炼30~40min,转速为50~60rpm,即得所述复合物料。
与现有技术相比,本发明具有如下有益效果:
1.本发明通过在对氧化铝使用硅烷偶联剂以及钛酸脂偶联剂进行改性,不仅能改善陶瓷件的抗弯强度、断裂韧性、硬度、体积密级等力学性能,还能进一步提高陶瓷件的抗热震性,提高了陶瓷件在复杂温度环境下的整体可靠性。
2.本发明原材料在国内充足,价格适宜,使其规模化生产没有太高的成本限制;其次,本发明组合适用范围广,可满足注射成型氧化铝基陶瓷件复合物料背胶层的生产要求;同时,制备工艺方法简单,总体生产成本不高,有利于工业的大规模生产。
具体实施方式
实施例1
按表1称量具体原料,其余步骤制备步骤如下:
(1)将氧化铝加入球磨机球磨,待粉体粒度达到1~5μm时,加入KH590继续球磨1h,随后加入异丙基三油酸酰氧基钛酸酯继续球磨1h,得到浆料A;
(2)将钛酸锶、钛酸铋、氧化钇、氧化镧、聚甲基丙烯酸乙酯、邻苯二甲酸二丁酯、异丙醇、甲醇加入到浆料A中,继续球磨2h得到浆料B;
(3)将浆料B、硬脂酸、乙撑双硬脂酰胺放入混炼机中,在180℃下均匀混炼4次,每次混炼30min,转速为50rpm,即得所述复合物料。
实施例2
按表1称量具体原料,其余步骤制备步骤如下:
(1)将氧化铝加入球磨机球磨,待粉体粒度达到1~5μm时,加入KH590继续球磨2h,随后加入异丙基三油酸酰氧基钛酸酯继续球磨2h,得到浆料A;
(2)将钛酸锶、钛酸铋、氧化钇、氧化镧、聚甲基丙烯酸乙酯、邻苯二甲酸二丁酯、异丙醇、甲醇加入到浆料A中,继续球磨1h得到浆料B;
(3)将浆料B、硬脂酸、乙撑双硬脂酰胺放入混炼机中,在220℃下均匀混炼3次,每次混炼40min,转速为60rpm,即得所述复合物料。
实施例3
按表1称量具体原料,其余步骤制备步骤如下:
(1)将氧化铝加入球磨机球磨,待粉体粒度达到1~5μm时,加入KH590继续球磨2h,随后加入异丙基三油酸酰氧基钛酸酯继续球磨2h,得到浆料A;
(2)将钛酸锶、钛酸铋、氧化钇、氧化镧、聚甲基丙烯酸乙酯、邻苯二甲酸二丁酯、异丙醇、甲醇加入到浆料A中,继续球磨2h得到浆料B;
(3)将浆料B、硬脂酸、乙撑双硬脂酰胺放入混炼机中,在220℃下均匀混炼4次,每次混炼40min,转速为60rpm,即得所述复合物料。
对比例1
按表1称量具体原料,其余步骤制备步骤如下:
(1)将氧化铝加入球磨机球磨,待粉体粒度达到1~5μm时,加入异丙基三油酸酰氧基钛酸酯继续球磨2h,得到浆料A;
(2)将钛酸锶、钛酸铋、氧化钇、氧化镧、聚甲基丙烯酸乙酯、邻苯二甲酸二丁酯、异丙醇、甲醇加入到浆料A中,继续球磨2h得到浆料B;
(3)将浆料B、硬脂酸、乙撑双硬脂酰胺放入混炼机中,在220℃下均匀混炼4次,每次混炼40min,转速为60rpm,即得所述复合物料。
对比例2
按表1称量具体原料,其余步骤制备步骤如下:
(1)将氧化铝加入球磨机球磨,待粉体粒度达到1~5μm时,加入KH590继续球磨2h,得到浆料A;
(2)将钛酸锶、钛酸铋、氧化钇、氧化镧、聚甲基丙烯酸乙酯、邻苯二甲酸二丁酯、异丙醇、甲醇加入到浆料A中,继续球磨2h得到浆料B;
(3)将浆料B、硬脂酸、乙撑双硬脂酰胺放入混炼机中,在220℃下均匀混炼4次,每次混炼40min,转速为60rpm,即得所述复合物料。
对比例3
按表1称量具体原料,其余步骤制备步骤如下:
(1)将氧化铝加入球磨机球磨,待粉体粒度达到1~5μm时,得到浆料A;
(2)将钛酸锶、钛酸铋、氧化钇、氧化镧、聚甲基丙烯酸乙酯、邻苯二甲酸二丁酯、异丙醇、甲醇加入到浆料A中,继续球磨2h得到浆料B;
(3)将浆料B、硬脂酸、乙撑双硬脂酰胺放入混炼机中,在220℃下均匀混炼4次,每次混炼40min,转速为60rpm,即得所述复合物料。
表1
物料组成 | 实施例1 | 实施例2 | 实施例3 | 对比例1 | 对比例2 | 对比例3 |
氧化铝 | 200 | 220 | 250 | 250 | 250 | 250 |
KH590 | 10 | 15 | 20 | / | 20 | / |
异丙基三油酸酰氧基钛酸酯 | 5 | 6 | 10 | 10 | / | / |
钛酸锶 | 3 | 4 | 5 | 5 | 5 | 5 |
钛酸铋 | 5 | 7 | 10 | 10 | 10 | 10 |
氧化钇 | 6 | 8 | 12 | 12 | 12 | 12 |
氧化镧 | 9 | 12 | 16 | 16 | 16 | 16 |
邻苯二甲酸二丁酯 | 10 | 15 | 20 | 20 | 20 | 20 |
硬脂酸 | 5 | 6 | 7 | 7 | 7 | 7 |
聚甲基丙烯酸乙酯 | 10 | 15 | 20 | 20 | 20 | 20 |
乙撑双硬脂酰胺 | 1 | 2 | 3 | 3 | 3 | 3 |
异丙醇 | 10 | 12 | 15 | 15 | 15 | 15 |
甲醇 | 8 | 8 | 10 | 10 | 10 | 10 |
实施例 4性能测试
将实施例1~3以及对比例1~3制备得到的复合物料按以下方法制备陶瓷件:将混炼后的原料在切粒机中造粒成直径3mm、高度5mm的陶瓷喂料后,通过自动上料机将喂料送入高压注射成型机料斗中,在注射压力为40MPa,注射温度为150℃的条件下,将陶瓷喂料注入精密模具,开模后得到陶瓷毛坯;在温度70℃、湿度60%恒温恒湿条件下进行脱脂处理;在100℃温度下烘干后,通过机械臂将其放入推板窑中,陶瓷毛坯在650℃保温2小时排胶处理,升温速率为20℃/h,然后升温至1500℃~1550℃进行烧结,升温速率为120-180℃/h,保温时间为16h,即得陶瓷件。
将使用实施例1~3以及对比例1~3的复合物料制备得到的陶瓷件进行硬度、抗弯强度、断裂韧性、体积密度、抗热震性测试。测试结果见表2。
表2性能测试结果
实施例1 | 实施例2 | 实施例3 | 对比例1 | 对比例2 | 对比例3 | |
硬度(GPa) | 19.2 | 18.9 | 18.7 | 17.5 | 16.6 | 17.4 |
抗弯强度 (MPa) | 778 | 792 | 783 | 772 | 742 | 785 |
断裂韧性 (MPa·m1/2) | 9.5 | 9.4 | 9.7 | 7.1 | 6.3 | 6.8 |
体积密度(g•cm3) | 4.10 | 4.14 | 4.11 | 3.95 | 3.62 | 4.12 |
抗热震性(1200℃~25℃最大热交换次数) | 33 | 34 | 36 | 19 | 25 | 11 |
前述对本发明的具体示例性实施方案的描述是为了说明和例证的目的。这些描述并非想将本发明限定为所公开的精确形式,并且很显然,根据上述教导,可以进行很多改变和变化。对示例性实施例进行选择和描述的目的在于解释本发明的特定原理及其实际应用,从而使得本领域的技术人员能够实现并利用本发明的各种不同的示例性实施方案以及各种不同的选择和改变。本发明的范围意在由权利要求书及其等同形式所限定。
Claims (1)
1.一种注射成型氧化铝基陶瓷件的制备方法,其特征在于,所述氧化铝基陶瓷件由以下复合物料制备组成:氧化铝250份、硅烷偶联剂KH590 20份、异丙基三油酸酰氧基钛酸酯10份、钛酸锶5份、钛酸铋10份、氧化钇12份、氧化镧16份、邻苯二甲酸二丁酯20份、硬脂酸7份、聚甲基丙烯酸乙酯20份、乙撑双硬脂酰胺3份、异丙醇15份、甲醇10份;
所述复合物料的制备方法为:(1)将氧化铝加入球磨机球磨,待粉体粒度达到1~5μm时,得到浆料A;(2)将钛酸锶、钛酸铋、氧化钇、氧化镧、聚甲基丙烯酸乙酯、邻苯二甲酸二丁酯、异丙醇、甲醇加入到浆料A中,继续球磨2h得到浆料B;(3)将浆料B、硬脂酸、乙撑双硬脂酰胺放入混炼机中,在220℃下均匀混炼4次,每次混炼40min,转速为60rpm,即得所述复合物料;
所述陶瓷件的制备方法为:将混炼后的复合物料在切粒机中造粒成直径3mm、高度5mm的陶瓷喂料后,通过自动上料机将喂料送入高压注射成型机料斗中,在注射压力为40MPa,注射温度为150℃的条件下,将陶瓷喂料注入精密模具,开模后得到陶瓷毛坯;在温度℃、湿度60%恒温恒湿条件下进行脱脂处理;在100℃温度下烘干后,通过机械臂将其放入推板窑中,陶瓷毛坯在650℃保温2小时排胶处理,升温速率为20℃/h,然后升温至1500℃~1550℃进行烧结,升温速率为120-180℃/h,保温时间为16h,即得。
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