CN104844198B - 手持终端产品外观陶瓷薄型件及其制备方法 - Google Patents

手持终端产品外观陶瓷薄型件及其制备方法 Download PDF

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CN104844198B
CN104844198B CN201410054368.6A CN201410054368A CN104844198B CN 104844198 B CN104844198 B CN 104844198B CN 201410054368 A CN201410054368 A CN 201410054368A CN 104844198 B CN104844198 B CN 104844198B
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thin type
preparation
outward appearance
biscuit
solvent
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CN104844198A (zh
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谢志鹏
颜宏艳
廖语茜
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Tsinghua University
Hongfujin Precision Industry Shenzhen Co Ltd
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Tsinghua University
Hongfujin Precision Industry Shenzhen Co Ltd
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Abstract

本发明涉及一种手持终端产品外观陶瓷薄型件的制备方法，包括：制备流延浆料，该流延浆料包括陶瓷粉料、分散剂、溶剂、粘结剂及增塑剂，各组分的重量百分比是：陶瓷粉料为50~60wt%，分散剂为0.5~1.5wt%，溶剂为30~40wt%，粘结剂为3~7wt%，增塑剂为3~9wt%；将该流延浆料在流延机上进行流延，得到单层素坯；层叠该单层素坯，包括将该单层素坯表面涂覆该流延浆料，将两个或多个该单层素坯层叠，形成素坯叠片，以及将该素坯叠片干压；干燥该素坯叠片，去除素坯叠片中的溶剂；将该素坯叠片冲压或裁剪成所需形状和尺寸；将该成形后的素坯叠片放入加热炉中进行热脱脂；以及将脱脂后的坯体在高温炉中进行烧结。

Description

手持终端产品外观陶瓷薄型件及其制备方法
技术领域
本发明涉及陶瓷产品制造领域，尤其涉及一种手持终端产品外观陶瓷薄型件的制备方法。
背景技术
手持终端产品，如智能手机、掌上电脑、平板电脑等的外观件通常选用塑料或金属制造。ABS工程塑料重量轻且价格低廉，钛合金轻薄坚硬，铝合金强度高，耐腐蚀，耐热性高。但由于手持式终端产品使用的频繁性，且大都在室外使用，周围的湿度、温度等环境因素对手持终端的操作影响比较大。ABS材料的热变形温度较低，可燃，耐候性较差，金属材料化学稳定性差，比重大。这些都影响了手持式终端产品的外观甚至寿命。
陶瓷材料强度高，化学稳定性好，耐磨损，作为手持终端产品外观件比传统的塑料和金属材质更加耐磨和拥有玉质感。目前制造手持式终端产品外观件的常用方法有干压、注浆成型及热压铸。陶瓷干压成型虽然效率较高，但成型产品存在密度差异、显微结构不均匀的现象。陶瓷注浆虽可成型，但成型坯体易产生密度不均和成分偏析，成型尺寸精度低和产品可靠性下降等问题，并且成型为手工操作且干燥效率低。热压铸成型最大的问题是生产周期长，效率低下，排除石蜡周期较长，且排蜡过程中容易产生气孔、开裂等缺陷。
流延法是一种形成薄型陶瓷件的方法，主要用于制备厚度在微米级的小尺寸的电子元器件，如传感器、压电元件、陶瓷电容器及片式微波元器件，可以制备出尺寸精度较高的产品。然而电子元器件主要利用陶瓷的压电、介电等特殊性能，将流延法用于大尺寸产品的制备则较少。目前还未有报道将流延法用于制备手持终端产品的外观件。
发明内容
本发明的目的在于提供一种新的手持终端产品外观陶瓷薄型件的制备方法。
一种手持终端产品外观陶瓷薄型件的制备方法，包括：制备流延浆料，该流延浆料包括陶瓷粉料、分散剂、溶剂、粘结剂及增塑剂，各组分的重量百分比是：陶瓷粉料为50~60wt%，分散剂为0.5~1.5wt%，溶剂为30~40wt%，粘结剂为3~7wt%，增塑剂为3~9wt%；将该流延浆料在流延机上进行流延，得到单层素坯；层叠该单层素坯，包括将该单层素坯表面涂覆该流延浆料，将两个以上该单层素坯层叠，形成素坯叠片，以及将该素坯叠片干压；干燥该素坯叠片，去除素坯叠片中的溶剂；将该素坯叠片冲压或裁剪成所需形状和尺寸；将该成形后的素坯叠片放入加热炉中进行热脱脂；以及将脱脂后的坯体在高温炉中进行烧结。
本方法通过层叠得到的素坯表面平整，柔韧性好，并且素坯整体厚度不受流延机刀口高度的限制，可方便调节。通过该方法制备的陶瓷薄型件厚度为0.6~1.5mm，可适用于大多数手持式终端产品外观所需的陶瓷薄型件。而普通的单层流延只能制备厚度在0.8 mm以下的素坯片，烧结后的厚度在0.6mm以下，难以应用于大尺寸产品，尤其是手持终端产品外观陶瓷薄型件。
附图说明
图1为本发明实施例手持终端产品外观陶瓷薄型件的制备方法的流程图。
如下具体实施方式将结合上述附图进一步说明本发明。
具体实施方式
下面将结合附图及具体实施例对本发明提供的一种手持终端产品外观陶瓷薄型件的制备方法做进一步的详细说明。
请参阅图1，本发明提供一种流延成型法制备手持式终端产品外观陶瓷薄型件的方法，包括以下步骤：
（1）制备流延浆料：
该流延浆料包括陶瓷粉料、分散剂、溶剂、粘结剂及增塑剂，各组分的重量百分比是：陶瓷粉料为50~60wt%，分散剂为0.5~1.5wt%，溶剂为30~40wt%，粘结剂为3~7wt%，增塑剂为3~9wt%。该流延浆料中还可加入少量的除泡剂，质量百分比可以为0.5~1.5wt%。
在一实施例中，该流延浆料的制备方法，可包括以下步骤：
称取上述比例的陶瓷粉料、分散剂、溶剂、粘结剂及增塑剂；
将陶瓷粉料、分散剂及一部分溶剂加入球磨罐中，进行第一次球磨，时间为12~20小时，获得均匀的初始浆料；
将粘结剂、增塑剂及剩余的溶剂加入该球磨罐中，与该初始浆料混合，进行第二次球磨，时间为10~20小时，即得到所需的流延浆料。
该流延浆料具适宜的粘度，利于流延形成均匀稳定的薄型件素坯。该流延浆料的粘度可以为5~30Pa﹒s。
所述陶瓷粉料可以为氧化锆、氧化铝或氧化锆增韧氧化铝复合粉体，平均粒径为0.1微米~1微米。该陶瓷粉料可以比金属材料具有更好的耐磨性。所述分散剂可以为非离子型表面活性剂，如三油甘油酯酸、油酸、蓖麻油及鱼油中的至少一种。所述溶剂可以为两种溶剂的混合溶剂，主溶剂为乙醇或正丁醇，助溶剂选用丙酮或乙二醇。所述粘结剂可以为聚乙烯醇缩丁醛或聚甲基丙烯酸甲脂。所述增塑剂可以为聚乙二醇或邻苯二甲酸二丁酯。除泡剂可以为正丁醇及乙二醇中的至少一种。
优选地，所述第一次球磨时各组分的重量百分比为：60~80%陶瓷粉料，20~30%溶剂，0.1~0.3%分散剂。所述第二次球磨时加入的增塑剂、粘结剂及剩余溶剂之间的重量百分比为：35~45%增塑剂，25~35%粘结剂，25~35%溶剂。
在制备该流延浆料后，还可进一步包括将该流延浆料除泡的步骤。现有的浆料除泡都是采用抽真空方式，但真空除泡时会导致溶剂蒸发，使浆料粘度大幅度提高而不利于流延成型。为解决该问题，在本实施例中，该除泡的步骤具体是将流延浆料置于密闭环境中高速旋转脱泡，转速可以为1500r/min~2500r/min。利用高速旋转产生的离心力，可以使气泡从流延浆料中上升并破裂，达到除泡的目的，避免抽真空带来的溶剂损失，同时密闭环境可以减少溶剂挥发，可有效保证固相含量，稳定浆料粘度。该旋转除泡的时间可以为5min~30min。
另外，也可使用高能球磨机，通过调整球磨时的转速及时间，将浆料制备及除泡的步骤一体化。该高能球磨机的转速可以为800r/min~2200r/min，时间可以为20min~30min。该高能球磨机的球磨混合及除泡步骤可以分低速-高速-低速三个阶段，在一实施例中，首先在800r/min球磨1分钟之后以1000r/min除泡1分钟；其次在2000r/min球磨15分钟之后以2200r/min除泡2分钟；最后以1000r/min球磨2分钟。
通过高能球磨机将浆料制备和除泡一体化，不但可以简化工艺，节约时间，并且由于处理时间较短，还保证了在整个混料的过程中溶剂量的基本恒定，使得各组分能更好的在溶剂中溶解，同时，这种工艺有效的提高了固相含量，避免了传统工艺中由于溶剂挥发带来的粘度增大。
（2）将该流延浆料在流延机上进行流延，得到单层素坯。
流延速率为0.08 m/s ~0.12m/s，流延机刀口高度可以为1000微米~3000微米。流延带可以选用聚酯膜，其化学性稳定，耐腐蚀，耐高温，并且不易变形。在流延层中大部分溶剂挥发后，单层素坯的厚度(t)为0.2mm≤t<0.8mm，素坯的宽度可以达到5cm以上，如5 cm ~15cm。
（3）层叠该单层素坯，包括将该单层素坯表面涂覆流延浆料；将多个单层素坯层叠，形成素坯叠片；以及将素坯叠片干压。
干压素坯叠片的压力可以为6 MPa ~10MPa，优选为8MPa，时间可以为3min~10min，优选为4min。
该流延浆料的涂覆的方式不限，可以为机涂或手涂，所用流延浆料为步骤（1）中的流延浆料。流延浆料的涂覆厚度可以为0.1mm~0.2mm。优选为将两个单层素坯层叠。成型的素坯叠片素坯由于具有很好柔韧性，可后期进行冲压、剪裁等加工。
（4）干燥素坯叠片，去除素坯叠片中的溶剂。干燥温度可以为20~60℃，干燥时间为1~2小时。优选为在溶剂气氛中进行干燥，可以使溶剂蒸发速度不致过快。溶剂蒸发速度过快容易导致素坯叠片形成开裂和气孔。例如，当所用溶剂为3:2的乙醇和丁酮时，可以在干燥箱中放入同样比例的溶剂，形成溶剂气氛。更为优选地，步骤（2）、（3）、（4）均在溶剂气氛中进行，可以避免溶剂在流延和层叠过程中挥发造成的开裂和气孔。
单层流延得到的干燥后的素坯片的厚度小于0.8mm，通过层叠单层素坯片，干燥后可得到0.8~1.6mm的素坯叠片。
（5）将具有柔韧性的素坯叠片冲压或裁剪成所需形状和尺寸。例如可以是利用冲压装置将该素坯叠片进行成形。
（6）将该素坯叠片放入加热炉中加热至250~600°C，进行热脱脂，脱除有机添加剂，如粘结剂、增塑剂、分散剂和除泡剂，得到坯体。优选以0.5~1.0℃/min速率升温至600°C，保温0.5~2小时。
（7）脱脂后的坯体在高温炉中进行烧结，烧结温度1400~1600℃之间，保温1~3小时，随炉冷却，得到薄型陶瓷部件。烧结成致密陶瓷后的薄型件厚度为0.6~1.5mm。烧结后两层素坯叠片结合成一体，完整无分层。
本发明的有益效果为：可以制备出比现有的金属或塑料的手持式终端产品外观薄型件更加耐磨，性能更加稳定的氧化锆或氧化锆增韧氧化铝陶瓷薄型件，有效保证了外观薄型件的寿命，即便频繁使用，也很少或几乎无磨损。由于流延法本身带来的限制，在浆料粘度适用流延的条件下，即使提升刀口高度，浆料在流延带上也会自行摊开，因此传统的流延素坯厚度小于0.8mm，烧结后的厚度更小，通常只用于生产厚度为微米级的电子元件。采用本发明的方法得到的素坯厚度可大于0.8 mm，且素坯叠片无变形和开裂缺陷，烧结平整、致密。通过本方法可以使陶瓷薄型件的厚度不受流延法限制，可以将流延法用于制备大尺寸陶瓷片制造领域，拓展了流延法的应用范围。提出了改善流延工艺中气泡脱出的方法，即采用的密闭空间的高速旋转除泡工艺，有效减少了溶剂蒸发。
实施例1
本实施例中，陶瓷粉体选用氧化锆陶瓷粉，粉体平均粒径0.2~0.3微米，比表面积11 m2/g。
（1）流延浆料制备及除泡
将96.8g氧化锆陶瓷粉体，60ml乙醇和丙酮的混合物，1.6ml三油酸甘油酯，2ml正丁醇和乙二醇混合液（体积比1:1），加入球磨罐中进行第一次球磨，时间为16小时；将8.3g聚乙烯醇缩丁醛，9.4ml聚乙二醇和邻苯二甲酸二丁酯的混合液，10ml乙醇和丁酮的混合物，加入该球磨罐中，进行第二次球磨，时间为13小时，得到流延浆料。
将流延浆料置于密闭容器中，高速旋转10min，转速2200r/min，使浆料内的气泡浮在浆料表面破裂。
（2）流延
该流延速率为0.12m/s，在溶剂气氛保护下进行流延，形成单层素坯片，厚度约为0.5mm，宽度约为10cm。
（3）层叠
将该单层素坯片表面涂覆原先的流延浆料，涂覆厚度为0.1mm~0.2mm，覆盖另一层相同的单层素坯片，将该两层的素坯叠片在干压机中压合，压力为8MPa，时间为4min。
（4）干燥
将该素坯叠片在保护气氛中50°C放置1小时，使溶剂挥发，得到厚度约为1毫米的叠片。
（5）冲压裁片
利用冲压装置，将流延膜带冲裁成所需样品形状，可在生坯上按照需要冲孔。
（6）脱脂
将冲裁好的坯片放入加热炉中，进行热脱脂，脱除有机添加剂，以0.5℃/min升温至600℃速率，保温1小时。
（7）烧结
脱脂后的坯体在硅钼棒烧结炉中进行烧结，烧结温度1480℃，保温1小时，随炉冷却，得到厚度为0.8mm的陶瓷部件。
经实验测试，该陶瓷薄型件的密度可以达到6.05g/cm3。
实施例2
本实施例中，陶瓷粉体选用氧化锆增韧氧化铝陶瓷复合粉，粉体平均粒径0.3~0.5微米，比表面积8 m2/g。
（1）流延浆料制备与除泡
分别将87.8g氧化锆陶瓷粉体和氧化锆/氧化铝复合粉体（其中氧化铝质量分数10%），与55ml乙醇和丙酮的混合物，1.4ml三油酸甘油酯，1.5ml正丁醇和乙二醇混合液（体积比1:1），加入球磨罐中进行第一次球磨，时间为13小时；将7.5g聚乙烯醇缩丁醛，8.7ml邻苯二甲酸二丁酯的溶液，9.5ml乙醇和丙酮的混合物，加入球磨罐中，进行第二次球磨，时间为11小时，得到流延浆料。
将该氧化锆/氧化铝（10wt%氧化铝）复合粉流延浆料置于密闭容器中，高速旋转5min，转速2500r/min，使浆料内的气泡浮在浆料表面破裂。
（2）流延
该流延速率为0.11 m/s，在溶剂气氛保护下进行流延，形成单层素坯片，厚度约为0.7mm，宽度约为10cm。
（3）层叠
将该单层素坯片表面涂覆原先的流延浆料，涂覆厚度为0.1mm~0.2mm，覆盖另一层相同的单层素坯片，将该两层的素坯叠片在干压机中压合，压力为8MPa，时间为4min。
（4）干燥
将该素坯叠片在保护气氛中40°C放置2小时，得到厚度约为1.4mm的素坯叠片。
（5）冲压裁片
利用冲压装置，将流延坯片冲裁成所需样品形状，可在生坯上按照需要冲孔。
（6）脱脂
将冲裁好的膜带放入加热炉中，进行热脱脂，脱除有机添加剂，以1℃/min升温至600℃速率，保温0.5小时。
（7）烧结
脱脂后的在硅钼棒烧结炉中坯体进行烧结，烧结温度1530℃，保温1.5小时，随炉冷却，得到厚度为1.2毫米的陶瓷薄型件。经实验测试，该陶瓷薄型件的密度可以达到5.60g/cm3。
另外，本领域技术人员还可在本发明精神内做其他变化，当然，这些依据本发明精神所做的变化，都应包含在本发明所要求保护的范围之内。

Claims (18)

1.一种手持终端产品外观陶瓷薄型件的制备方法，包括：
制备流延浆料，该流延浆料包括陶瓷粉料、分散剂、溶剂、粘结剂及增塑剂，各组分的重量百分比是：陶瓷粉料为50~60wt%，分散剂为0.5~1.5wt%，溶剂为30~40wt%，粘结剂为3~7wt%，增塑剂为3~9wt%；
将该流延浆料在流延机上进行流延，得到单层素坯；
层叠该单层素坯，包括将该单层素坯表面涂覆该流延浆料，将至少两个单层素坯层叠，形成素坯叠片，以及将该素坯叠片干压；
干燥该素坯叠片，去除素坯叠片中的溶剂；
将该素坯叠片冲压或裁剪成所需形状和尺寸；
将该成形后的素坯叠片放入加热炉中进行热脱脂；以及
将脱脂后的坯体在高温炉中进行烧结。
2.如权利要求1所述的手持终端产品外观陶瓷薄型件的制备方法，其特征在于，制备该流延浆料的步骤包括：
按比例称取陶瓷粉料、分散剂、溶剂、粘结剂及增塑剂；
将陶瓷粉料、分散剂及一部分溶剂加入球磨罐中，进行第一次球磨，获得均匀的初始浆料；以及
将粘结剂、增塑剂及剩余的溶剂加入该球磨罐中，与该初始浆料混合，进行第二次球磨，即得到所需的流延浆料。
3.如权利要求2所述的手持终端产品外观陶瓷薄型件的制备方法，其特征在于，所述第一次球磨时各组分的重量百分比为：60~80%陶瓷粉料，20~30%溶剂，0.1~0.3%分散剂。
4.如权利要求2所述的手持终端产品外观陶瓷薄型件的制备方法，其特征在于，所述第二次球磨时加入的增塑剂、粘结剂及剩余溶剂之间的重量百分比为：35~45%增塑剂，25~35%粘结剂，25~35%溶剂。
5.如权利要求2所述的手持终端产品外观陶瓷薄型件的制备方法，其特征在于，所述第一次球磨的时间为12小时~20小时，所述第二次球磨的时间为10小时~20小时。
6.如权利要求1所述的手持终端产品外观陶瓷薄型件的制备方法，其特征在于，所述浆料中的陶瓷粉料为氧化锆、氧化铝、氧化锆增韧氧化铝复合粉体，平均粒径为0.1微米~1微米。
7.如权利要求1所述的手持终端产品外观陶瓷薄型件的制备方法，其特征在于，所述的分散剂为三油甘油酯酸、油酸、蓖麻油及鱼油中的至少一种。
8.如权利要求1所述的手持终端产品外观陶瓷薄型件的制备方法，其特征在于，所述溶剂为两种溶剂的混合溶剂，主溶剂为乙醇或正丁醇，助溶剂为丙酮或乙二醇。
9.如权利要求1所述的手持终端产品外观陶瓷薄型件的制备方法，其特征在于，所述粘结剂为聚乙烯醇缩丁醛或聚甲基丙烯酸甲脂。
10.如权利要求1所述的手持终端产品外观陶瓷薄型件的制备方法，其特征在于，所述增塑剂为聚乙二醇或邻苯二甲酸二丁酯。
11.如权利要求1所述的手持终端产品外观陶瓷薄型件的制备方法，其特征在于，进一步包括将流延浆料置于密闭环境中高速旋转脱泡的步骤，转速为1500r/min~2500r/min。
12.如权利要求1所述的手持终端产品外观陶瓷薄型件的制备方法，其特征在于，使用高能球磨机制备该流延浆料，该高能球磨机的转速为800r/min~2200r/min。
13.如权利要求1所述的手持终端产品外观陶瓷薄型件的制备方法，其特征在于，该流延浆料的粘度为5 Pa﹒s ~30Pa﹒s。
14.如权利要求1所述的手持终端产品外观陶瓷薄型件的制备方法，其特征在于，该干燥的步骤为在该流延浆料所用的溶剂的气氛中进行。
15.如权利要求1所述的手持终端产品外观陶瓷薄型件的制备方法，其特征在于，该流延、层叠及干燥的步骤均在该流延浆料所用的溶剂的气氛中进行。
16.如权利要求1所述的手持终端产品外观陶瓷薄型件的制备方法，其特征在于，该干压素坯叠片的压力为6 MPa ~10MPa。
17.如权利要求1所述的手持终端产品外观陶瓷薄型件的制备方法，其特征在于，该热脱脂的步骤为以0.5℃/min~1.0℃/min速率升温至600°C，保温0.5~2小时。
18.如权利要求1所述的手持终端产品外观陶瓷薄型件的制备方法，其特征在于，该烧结步骤的烧结温度为1400℃~1600℃之间，保温1~3小时。
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