CN106431394A - 黑色氧化锆烧结体及其制备方法与应用 - Google Patents

黑色氧化锆烧结体及其制备方法与应用 Download PDF

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Publication number
CN106431394A
CN106431394A CN201610792397.1A CN201610792397A CN106431394A CN 106431394 A CN106431394 A CN 106431394A CN 201610792397 A CN201610792397 A CN 201610792397A CN 106431394 A CN106431394 A CN 106431394A
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Prior art keywords
sintered body
powder
oxide
oxide sintered
black zirconia
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CN201610792397.1A
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Inventor
杨爱民
莫学魁
宋锡滨
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Shandong Sinocera Functional Material Co Ltd
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Shandong Sinocera Functional Material Co Ltd
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Priority to CN201610792397.1A priority Critical patent/CN106431394A/zh
Publication of CN106431394A publication Critical patent/CN106431394A/zh
Priority to US16/329,519 priority patent/US10737983B2/en
Priority to PCT/CN2017/095745 priority patent/WO2018040833A1/zh
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Abstract

本发明提供一种新型的黑色氧化锆烧结体，其是将黑色氧化锆烧结体用粉末加工成型，然后在常压大气中进行高温烧结制得的。所述黑色氧化锆烧结体用粉末是以可溶性锆盐、可溶性钇盐和发色剂为原料，经水热合成法制得；其中可溶性锆盐和钇盐以及发色剂的摩尔比为90‑95：1‑5：1‑9。本发明的黑色氧化锆烧结体可用于陶瓷工艺。利用本发明提供的氧化锆粉末可制作黑色氧化锆烧结体，且工艺简单，烧结过程无需保护气氛、无需热压烧结，烧结体质地均匀，强度高，三点抗弯强度≥1100MPa，烧结无污染。

Description

黑色氧化锆烧结体及其制备方法与应用
技术领域
本发明涉及化工领域，具体地说，涉及一种黑色氧化锆烧结体及其制备方法与应用。
背景技术
现有黑色氧化锆陶瓷包括两种加工工艺，一种是使用白色氧化锆制成坯体后进行渗碳处理。这种方法制作黑色氧化锆烧结体工艺繁琐，而且需在保护气氛下烧结，对设备要求高，另外在烧结过程中色料挥发性很强，设备污染严重。另一种是在氧化锆粉体中添加金属氧化物发色剂，但由于金属氧化物易出现大颗粒、分布不均匀等问题，导致氧化锆陶瓷烧结体强度低、开裂、颜色不均匀、颜色发暗等。
CN1566021公开了一种黑色氧化锆陶瓷的制造方法，其工件坯脱蜡、脱脂后，需真空或保护气氛烧结，对烧结设备要求高，烧结温度高(1550-1650℃)；制作工艺复杂，其烧结过程中需使用石墨进行渗碳染色处理；该工艺烧结对设备污染严重。
发明内容
本发明的目的是提供一种新型的黑色氧化锆烧结体及其制备方法。
本发明的另一目的是提供所述黑色氧化锆烧结体在陶瓷工艺中的应用。
为了实现本发明目的，本发明首先提供一种黑色氧化锆烧结体用粉末，所述粉末按如下步骤制备：
S1、将可溶性锆盐和钇盐按照比例混合溶于水，加入发色剂，搅拌条件下缓慢加入氨水，用氨水调浆料pH至8-10；
S2、将上述浆料转移至反应釜中，于140-200℃水热合成10-72h；
S3、将上述所得反应溶液经水洗、干燥得粉体；
S4、上述粉体经800-1200℃热处理2-5h后进行研磨分散；
S5、将分散好的颗粒进行造粒，即得黑色氧化锆烧结体用粉末；
S1中，可溶性锆盐和钇盐以及发色剂的摩尔比为90-95：1-5：1-9，优选92：3：5。
本发明的黑色氧化锆烧结体用粉末具有比表面积BET为10-16m2/g，平均粒径为0.1-0.3μm。
所述可溶性锆盐包括氧氯化锆、硝酸锆、硫酸锆等；所述可溶性钇盐包括氯化钇、硝酸钇、硫酸钇等。
所述发色剂包括氧化钴、氧化锰、氧化铁、氧化钛、氧化铝、氧化镍、氧化铜、氧化铒、氧化硅、氧化锌、氧化铬等中的至少一种。
本发明还提供由所述粉末制备的黑色氧化锆烧结体。其中，所述烧结体的L值≤3，a值为-1～1，b值为-1～1，瓷体密度≥6.0g/cm3，三点抗弯强度≥1100MPa。其中，L表示明度(Luminosity)，a表示从洋红色至绿色的范围，b表示从黄色至蓝色的范围。L的值域从0到100，a和b的值域均从+127至-128，可用分光测色计测试。
本发明的黑色氧化锆烧结体可采用以下方法制备得到：将所述粉末加工成型，然后在常压大气中进行高温烧结，即得。例如，可采用干压成型的方式将所述粉末加工成工件坯，成型压力150-250MPa。
前述方法中，高温烧结时的温度保持在1400-1550℃，时间为1-4h。
本发明中，将所述粉末加工成型可以采用压制或注射成形法。
本发明还提供所述黑色氧化锆烧结体在陶瓷工艺中的应用。例如，用于陶瓷刀、手表外壳、手机外壳、磨具、饰品及其它结构件。
本发明进一步提供含有所述黑色氧化锆烧结体的陶瓷材料。
本发明具有以下优点：
利用本发明提供黑色氧化锆烧结体用粉末可制作黑色氧化锆烧结体，且工艺简单，脱脂后直接烧结即可，无需其它处理，烧结温度低(1400-1550℃)；烧结过程无需保护气氛、无需热压烧结，烧结体质地均匀，强度高，三点抗弯强度≥1100MPa，烧结无污染，对设备要求低。
具体实施方式
以下实施例用于说明本发明，但不用来限制本发明的范围。若未特别指明，实施例中所用的技术手段为本领域技术人员所熟知的常规手段，所用原料均为市售商品。
本发明中涉及到的百分号“％”，若未特别说明，是指质量百分比；但溶液的百分比，除另有规定外。
实施例1-5黑色氧化锆烧结体用粉末
所述黑色氧化锆烧结体用粉末是以可溶性锆盐、可溶性钇盐和发色剂为原料，经水热合成法制得(表1)。
表1黑色氧化锆烧结体用粉末
具体工艺如下：
S1、将硝酸锆和硝酸钇按照比例混合溶于水，加入发色剂，搅拌条件下缓慢加入氨水，用氨水调浆料pH至8-10；
S2、将上述浆料转移至反应釜中，于140-200℃水热合成10-72h；
S3、将上述所得反应溶液经水洗、干燥得粉体；
S4、上述粉体经800-1200℃热处理2-5h后进行研磨分散；
S5、将分散好的颗粒进行造粒，即得黑色氧化锆烧结体用粉末。
实施例6-10黑色氧化锆烧结体及其制备方法
实施例1-5制备的粉末经干压成型(成型压力150-250MPa)后，在常压大气中，于1400-1550℃进行烧结1-4h制得黑色氧化锆烧结体。
所得烧结体产品的各项指标见表2。
表2黑色氧化锆烧结体产品指标
L值 a值 b值 瓷体密度，g/cm3 三点抗弯强度，MPa
实施例1 2.3 -0.03 -0.02 6.001 1337.3
实施例2 2.5 -0.01 0.01 5.999 1298.3
实施例3 2.2 0.01 -0.03 5.998 1468.9
实施例4 2.3 -0.02 -0.04 5.999 1489.0
实施例5 2.9 -0.03 0.02 6.000 1231.3
本发明提供的黑色氧化锆烧结体可用于制作陶瓷刀、手表外壳、手机外壳、磨具、饰品及其它结构件。
虽然，上文中已经用一般性说明及具体实施方案对本发明作了详尽的描述，但在本发明基础上，可以对之作一些修改或改进，这对本领域技术人员而言是显而易见的。因此，在不偏离本发明精神的基础上所做的这些修改或改进，均属于本发明要求保护的范围。

Claims (10)

1.黑色氧化锆烧结体用粉末，其特征在于，所述粉末按如下步骤制备：
S1、将可溶性锆盐和钇盐按照比例混合溶于水，加入发色剂，搅拌条件下用氨水调浆料pH至8-10；
S2、将上述浆料于140-200℃水热合成10-72h；
S3、将上述所得反应溶液经水洗、干燥得粉体；
S4、上述粉体经800-1200℃热处理2-5h后进行研磨分散；
S5、将分散好的颗粒进行造粒，即得黑色氧化锆烧结体用粉末；
S1中，可溶性锆盐和钇盐以及发色剂的摩尔比为90-95：1-5：1-9，优选92：3：5。
2.根据权利要求1所述的粉末，其特征在于，所述粉末的比表面积BET为10-16m2/g，平均粒径为0.1-0.3μm。
3.根据权利要求1或2所述的粉末，其特征在于，其特征在于，S1中所述发色剂包括氧化钴、氧化锰、氧化铁、氧化钛、氧化铝、氧化镍、氧化铜、氧化铒、氧化硅、氧化锌、氧化铬中的至少一种。
4.由权利要求1-3任一项所述粉末制备的黑色氧化锆烧结体。
5.根据权利要求4所述的烧结体，其特征在于，所述烧结体的L值≤3，a值为-1～1，b值为-1～1，瓷体密度≥6.0g/cm3，三点抗弯强度≥1100MPa。
6.权利要求4或5所述烧结体的制备方法，其特征在于，将所述粉末加工成型，然后在常压大气中进行高温烧结，即得。
7.根据权利要求6所述的方法，其特征在于，高温烧结时的温度保持在1400-1550℃，时间为1-4h。
8.根据权利要求6或7所述的方法，其特征在于，将所述粉末加工成型可以采用压制或注射成形法。
9.权利要求4或5所述烧结体在陶瓷工艺中的应用。
10.含有权利要求4或5所述烧结体的陶瓷材料。
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