CN106747458A - 制作碳化硅陶瓷微珠的生产工艺 - Google Patents

制作碳化硅陶瓷微珠的生产工艺 Download PDF

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CN106747458A
CN106747458A CN201710048635.2A CN201710048635A CN106747458A CN 106747458 A CN106747458 A CN 106747458A CN 201710048635 A CN201710048635 A CN 201710048635A CN 106747458 A CN106747458 A CN 106747458A
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grinding agent
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silicon carbide
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CN106747458B (zh
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于利学
李正闯
于娜
倪赫隆
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Weihai Ring Advanced Ceramic Co Ltd
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Abstract

本发明涉及一种制作碳化硅陶瓷微珠的生产工艺，属于粉体研磨领域。陶瓷原料的制备按照质量百分比，由如下组分组成：α‑SiC粉75%‑90%,SiO２3%‑7%,Al2O35%‑7%，TiN0.1%‑3%，酚醛树脂0.5%‑1%，HT树脂0.4%‑5%，油酸0.1%‑1%,B4C0.9%‑1%；在同一个转盘中将粘合剂PVA注入陶瓷原料，利用粘合剂PVA在介质中成球并固化，直接成型致密的粒径在0.1—2mm的坯珠；对填入海绵中的坯珠进行冷等静压，时间2‑10分钟；将冷等静压后的坯珠置于脱胶炉中完成脱胶工序；真空高温烧结炉中，将所得坯珠置于坩埚中进行烧结，生产陶瓷微珠坯球；将所得陶瓷微珠坯球进行研磨和抛光生产陶瓷微珠。

Description

制作碳化硅陶瓷微珠的生产工艺
技术领域
本发明涉及粉体研磨领域，详细地讲是一种制作碳化硅陶瓷微珠的生产工艺。
背景技术
目前，熔融法对陶瓷材料体系下，主要用于碳化钨和硅酸锆材料体系，不能用于碳化硅陶瓷微珠的成型；滚动成型采用“行星式”旋转装置，将粘合剂PVA和陶瓷粉放入特定的旋转盘中，转动得到粒径在0.1mm—2mm的微珠，这种方法工艺简单，但所制备的陶瓷微珠圆度较差，容易出现脱皮和破裂现象；注模成型需要将陶瓷浆料注入模具中，虽然可以克服滚动法带来的空心，分层，致密性差等缺点，提高了产品质量，但是对于1mm以下的陶瓷微珠，生产效率低。
发明内容
为了克服现有技术的不足，本发明提出一种制作碳化硅陶瓷微珠的生产工艺, 该陶瓷微珠具有低密度、高硬度、低摩擦系数，耐磨、自润滑及刚性好等，广泛地用于粉体磨介球。
本发明解决其技术问题所采用的技术方案是：一种制作碳化硅陶瓷微珠的生产工艺，其特征在于：
1）陶瓷原料的制备：将陶瓷原料过130目筛后，按照比例配成浆料混合均匀，置于砂磨机中球磨7h，经过喷雾造粒干燥后过筛；
其中，所述的陶瓷原料按照质量百分比计，由如下组分组成：
α-SiC粉 75%-90%
SiO２ 3%-7%
Al2O3 5%-7%
TiN 0.1%-3%
酚醛树脂 0.5%-1%
HT树脂 0.4%-5%
油酸 0.1%-1%
B4C 0.9%-1%；
2）注浆滚动成型：采用“行星式”旋转装置，在同一个转盘中将粘合剂PVA注入陶瓷原料，利用粘合剂PVA在介质中成球并固化，直接成型致密的粒径在0.1—2mm的坯珠；
3）冷等静压：在200兆帕压力下，对填入海绵中的坯珠进行冷等静压，时间2-10分钟；
4）脱胶工序：将冷等静压后的坯珠置于脱胶炉中，升温至1200℃时逐渐降温至室温，其中在450℃—1100℃之间保温1小时，12小时可以完成脱胶工序；
5）烧结：真空高温烧结炉中，将所得坯珠置于坩埚中，以15℃/min的升温速度进行烧结，其中烧结温度1050～1150℃，烧结时间3～4小时，继续升温至1350℃，其中在1150℃-1350℃保温2-6小时，停止加热，冷却至室温, 生产陶瓷微珠坯球；
6）研磨抛光：将所得陶瓷微珠坯球进行研磨和抛光生产陶瓷微珠，陶瓷微珠的球度不超过0.08微米，表面粗糙度不超过0.008微米，方法如下：
a.粗磨：载荷压力3—20N/珠，所用粗磨研磨剂中，金刚石颗粒的粒度为20—100um，金刚石颗粒圆度为0.2—0.6；
b.精磨：载荷压力0.5—3N/珠，所用精磨研磨剂中，金刚石颗粒的粒度为1—10um，金刚石颗粒圆度为0.6—0.7；
c.抛光磨：载荷压力0.1—0.5N/珠，所用抛光磨研磨剂中，金刚石颗粒的粒度为0.01-1um，金刚石颗粒圆度为0.70—0.85。
所述的粗磨研磨剂、精磨研磨剂和抛光磨研磨剂与研磨基质的质量比例均为1：1—1：6，所述研磨基质为水。
所述的粗磨研磨剂、精磨研磨剂和抛光磨研磨剂按质量百分比组成都为：
金刚石颗粒 25%
分散剂 70%
氧化铈 0.5%
三聚磷酸钠 0.5%
硅酸钠 3.5%
十二烷基磺酸钠 0.5%。
所述的分散剂为柠檬酸铵。
本发明的有益效果是，该工艺包括：配方料的制备、碳化硅陶瓷微珠成型、冷等静压、脱胶、烧结和研磨六个步骤。成型步骤；烧结步骤可以实现在常压下烧结碳化硅陶瓷微珠，在真空烧结碳化硅陶瓷微珠；研磨步骤包括各个阶段的研磨剂，含有粗磨研磨剂、精磨研磨剂和抛光磨研磨剂。这些研磨剂在研磨的各个阶段中配合使用，可达到研磨效率高、对陶瓷体污染少、减少研磨时间的效果。该陶瓷微珠具有低密度、高硬度、低摩擦系数，耐磨、自润滑及刚性好等，广泛地用于粉体磨介球。
下面结合实施例对本发明进一步说明。
具体实施方式
实施例一：
1）陶瓷原料的制备：将陶瓷原料过130目筛后，按照比例配成浆料混合均匀，置于砂磨机中球磨7h，经过喷雾造粒干燥后过筛；
其中，所述的陶瓷原料按照质量百分比计，由如下组分组成：
α-SiC粉 75%
SiO２ 7%
Al2O3 7%
TiN 3%
酚醛树脂 1%
HT树脂 5%
油酸 1%
B4C 1%。
2）注浆滚动成型：采用“行星式”旋转装置，在同一个转盘中将粘合剂PVA注入陶瓷原料，利用粘合剂PVA在介质中成球并固化，直接成型致密的粒径在0.1—2mm的坯珠。
3）冷等静压：在200兆帕压力下，对填入海绵中的坯珠进行冷等静压，时间2分钟。
4）脱胶工序：将冷等静压后的坯珠置于脱胶炉中，升温至1200℃时逐渐降温至室温，其中在450℃—1100℃之间保温1小时，12小时可以完成脱胶工序。
5）烧结：真空高温烧结炉中，将所得坯珠置于坩埚中，以15℃/min的升温速度进行烧结，其中烧结温度1050～1150℃，烧结时间3小时，继续升温至1350℃，其中在1150℃-1350℃保温2小时，停止加热，冷却至室温, 生产陶瓷微珠坯球。
6）研磨抛光：将所得陶瓷微珠坯球进行研磨和抛光生产陶瓷微珠，陶瓷微珠的球度不超过0.08微米，表面粗糙度不超过0.008微米，方法如下：
a.粗磨：载荷压力3N/珠，所用粗磨研磨剂中，金刚石颗粒的粒度为20um，金刚石颗粒圆度为0.2；
b.精磨：载荷压力0.5N/珠，所用精磨研磨剂中，金刚石颗粒的粒度为1um，金刚石颗粒圆度为0.6；
c.抛光磨：载荷压力0.1N/珠，所用抛光磨研磨剂中，金刚石颗粒的粒度为0.01um，金刚石颗粒圆度为0.70。
所述的粗磨研磨剂、精磨研磨剂和抛光磨研磨剂与研磨基质的质量比例均为1：1，所述研磨基质为水。
所述的粗磨研磨剂、精磨研磨剂和抛光磨研磨剂按质量百分比组成都为：
金刚石颗粒 25%
分散剂 70%
氧化铈 0.5%
三聚磷酸钠 0.5%
硅酸钠 3.5%
十二烷基磺酸钠 0.5%
所述的分散剂为柠檬酸铵。
实施例二：
1）陶瓷原料的制备：将陶瓷原料过130目筛后，按照比例配成浆料混合均匀，置于砂磨机中球磨7h，经过喷雾造粒干燥后过筛；
其中，所述的陶瓷原料按照质量百分比计，由如下组分组成：
α-SiC粉 90%
SiO２ 3%
Al2O3 5%
TiN 0.1%
酚醛树脂 0.5%
HT树脂 0.4%
油酸 0.1%
B4C 0.9%。
2）注浆滚动成型：采用“行星式”旋转装置，在同一个转盘中将粘合剂PVA注入陶瓷原料，利用粘合剂PVA在介质中成球并固化，直接成型致密的粒径在0.1—2mm的坯珠。
3）冷等静压：在200兆帕压力下，对填入海绵中的坯珠进行冷等静压，时间10分钟。
4）脱胶工序：将冷等静压后的坯珠置于脱胶炉中，升温至1200℃时逐渐降温至室温，其中在450℃—1100℃之间保温1小时，12小时可以完成脱胶工序。
5）烧结：真空高温烧结炉中，将所得坯珠置于坩埚中，以15℃/min的升温速度进行烧结，其中烧结温度1050～1150℃，烧结时间4小时，继续升温至1350℃，其中在1150℃-1350℃保温6小时，停止加热，冷却至室温, 生产陶瓷微珠坯球。
6）研磨抛光：将所得陶瓷微珠坯球进行研磨和抛光生产陶瓷微珠，陶瓷微珠的球度不超过0.08微米，表面粗糙度不超过0.008微米，方法如下：
a.粗磨：载荷压力20N/珠，所用粗磨研磨剂中，金刚石颗粒的粒度为100um，金刚石颗粒圆度为0.6；
b.精磨：载荷压力3N/珠，所用精磨研磨剂中，金刚石颗粒的粒度为10um，金刚石颗粒圆度为0.7；
c.抛光磨：载荷压力0.5N/珠，所用抛光磨研磨剂中，金刚石颗粒的粒度为1um，金刚石颗粒圆度为0.85。
所述的粗磨研磨剂、精磨研磨剂和抛光磨研磨剂与研磨基质的质量比例均为1：6，所述研磨基质为水。
所述的粗磨研磨剂、精磨研磨剂和抛光磨研磨剂按质量百分比组成都为：
金刚石颗粒 25%
分散剂 70%
氧化铈 0.5%
三聚磷酸钠 0.5%
硅酸钠 3.5%
十二烷基磺酸钠 0.5%
所述的分散剂为柠檬酸铵。
实施例三：
1）陶瓷原料的制备：将陶瓷原料过130目筛后，按照比例配成浆料混合均匀，置于砂磨机中球磨7h，经过喷雾造粒干燥后过筛；
其中，所述的陶瓷原料按照质量百分比计，由如下组分组成：
α-SiC粉 80%
SiO２ 6%
Al2O3 6%
TiN 2%
酚醛树脂 0.6%
HT树脂 4%
油酸 0.5%
B4C 0.9%。
2）注浆滚动成型：采用“行星式”旋转装置，在同一个转盘中将粘合剂PVA注入陶瓷原料，利用粘合剂PVA在介质中成球并固化，直接成型致密的粒径在0.1—2mm的坯珠。
3）冷等静压：在200兆帕压力下，对填入海绵中的坯珠进行冷等静压，时间8分钟。
4）脱胶工序：将冷等静压后的坯珠置于脱胶炉中，升温至1200℃时逐渐降温至室温，其中在450℃—1100℃之间保温1小时，12小时可以完成脱胶工序。
5）烧结：真空高温烧结炉中，将所得坯珠置于坩埚中，以15℃/min的升温速度进行烧结，其中烧结温度1050～1150℃，烧结时间4小时，继续升温至1350℃，其中在1150℃-1350℃保温4小时，停止加热，冷却至室温, 生产陶瓷微珠坯球。
6）研磨抛光：将所得陶瓷微珠坯球进行研磨和抛光生产陶瓷微珠，陶瓷微珠的球度不超过0.08微米，表面粗糙度不超过0.008微米，方法如下：
a.粗磨：载荷压力15N/珠，所用粗磨研磨剂中，金刚石颗粒的粒度为50um，金刚石颗粒圆度为0.4；
b.精磨：载荷压力2N/珠，所用精磨研磨剂中，金刚石颗粒的粒度为6um，金刚石颗粒圆度为0.6；
c.抛光磨：载荷压力0.3N/珠，所用抛光磨研磨剂中，金刚石颗粒的粒度为0.1um，金刚石颗粒圆度为0.75。
所述的粗磨研磨剂、精磨研磨剂和抛光磨研磨剂与研磨基质的质量比例均为1：4，所述研磨基质为水。
所述的粗磨研磨剂、精磨研磨剂和抛光磨研磨剂按质量百分比组成都为：
金刚石颗粒 25%
分散剂 70%
氧化铈 0.5%
三聚磷酸钠 0.5%
硅酸钠 3.5%
十二烷基磺酸钠 0.5%
所述的分散剂为柠檬酸铵。

Claims (5)

1.一种制作碳化硅陶瓷微珠的生产工艺，其特征在于：
1）陶瓷原料的制备：将陶瓷原料过130目筛后，按照比例配成浆料混合均匀，置于砂磨机中球磨7h，经过喷雾造粒干燥后过筛；
其中，所述的陶瓷原料按照质量百分比计，由如下组分组成：
α-SiC粉 75%-90%
SiO２ 3%-7%
Al2O3 5%-7%
TiN 0.1%-3%
酚醛树脂 0.5%-1%
HT树脂 0.4%-5%
油酸 0.1%-1%
B4C 0.9%-1%；
2）注浆滚动成型：采用“行星式”旋转装置，在同一个转盘中将粘合剂PVA注入陶瓷原料，利用粘合剂PVA在介质中成球并固化，直接成型致密的粒径在0.1—2mm的坯珠；
3）冷等静压：在200兆帕压力下，对填入海绵中的坯珠进行冷等静压，时间2-10分钟；
4）脱胶工序：将冷等静压后的坯珠置于脱胶炉中，升温至1200℃时逐渐降温至室温，其中在450℃—1100℃之间保温1小时，12小时可以完成脱胶工序；
5）烧结：真空高温烧结炉中，将所得坯珠置于坩埚中，以15℃/min的升温速度进行烧结，其中烧结温度1050～1150℃，烧结时间3～4小时，继续升温至1350℃，其中在1150℃-1350℃保温2-6小时，停止加热，冷却至室温, 生产陶瓷微珠坯球；
6）研磨抛光：将所得陶瓷微珠坯球进行研磨和抛光生产陶瓷微珠，陶瓷微珠的球度不超过0.08微米，表面粗糙度不超过0.008微米。
2.根据权利要求1所述制作碳化硅陶瓷微珠的生产工艺，其特征在于所述的研磨抛光方法如下：
a.粗磨：载荷压力3—20N/珠，所用粗磨研磨剂中，金刚石颗粒的粒度为20—100um，金刚石颗粒圆度为0.2—0.6；
b.精磨：载荷压力0.5—3N/珠，所用精磨研磨剂中，金刚石颗粒的粒度为1—10um，金刚石颗粒圆度为0.6—0.7；
c.抛光磨：载荷压力0.1—0.5N/珠，所用抛光磨研磨剂中，金刚石颗粒的粒度为0.01-1um，金刚石颗粒圆度为0.70—0.85。
3.根据权利要求2所述制作碳化硅陶瓷微珠的生产工艺，其特征在于所述的粗磨研磨剂、精磨研磨剂和抛光磨研磨剂与研磨基质的质量比例均为1：1—1：6，所述研磨基质为水。
4.根据权利要求2所述制作碳化硅陶瓷微珠的生产工艺，其特征在于所述的粗磨研磨剂、精磨研磨剂和抛光磨研磨剂按质量百分比组成都为：
金刚石颗粒 25%
分散剂 70%
氧化铈 0.5%
三聚磷酸钠 0.5%
硅酸钠 3.5%
十二烷基磺酸钠 0.5%。
5.根据权利要求4所述制作碳化硅陶瓷微珠的生产工艺，其特征在于所述的分散剂为柠檬酸铵。
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