CN106083001B - 一种纳米晶蓝色陶瓷刚玉磨料及其制备方法 - Google Patents

一种纳米晶蓝色陶瓷刚玉磨料及其制备方法 Download PDF

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CN106083001B
CN106083001B CN201610446675.8A CN201610446675A CN106083001B CN 106083001 B CN106083001 B CN 106083001B CN 201610446675 A CN201610446675 A CN 201610446675A CN 106083001 B CN106083001 B CN 106083001B
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李志宏
王津松
朱玉梅
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Abstract

本发明公开了一种纳米晶蓝色陶瓷刚玉磨料及其制备方法，采用溶胶‑凝胶法制备含铝前驱体，引入添加剂，再经造粒、筛分、锻烧等工艺获得陶瓷刚玉磨料。本发明以Al2(SO4)3·18H2O或Al(NO3)3·9H2O为原料，外加添加剂占原料的质量百分比为0.15％～0.8％，添加剂的原料组成及其占添加剂的质量百分比含量为Co(NO3)2·6H2O5％～25％，(NH4)3AlF6 5％～20％，C16H36O4Ti 0％～65％，Si(OC2H5)4 0％～40％，Mg(NO3)2·6H2O0％～50％，Ca(NO3)2·4H2O 0～20％。本发明改变了刚玉磨料的显色特征，与电熔法相比降低了400℃～800℃的生产温度，优化了刚玉磨料内部显微结构，单颗粒抗压强度最高可达58.6N，冲击韧性比现有的陶瓷刚玉磨料提高15％～25％，制成的陶瓷刚玉砂轮磨削效率比普通刚玉砂轮提高55％以上，使用寿命也得到相应延长。

Description

一种纳米晶蓝色陶瓷刚玉磨料及其制备方法
技术领域
本发明是关于磨削加工磨料的，尤其涉及一种纳米晶蓝色陶瓷刚玉磨料及其制备方法。
背景技术
人造刚玉磨料自从19世纪末首次研制成功以来，取得了极快的发展，由于其具有良好的机械性能和高温磨削稳定性，以及加工对象的广泛性，获得了广泛的应用。人造刚玉依据其杂质离子含量和晶型分为：棕刚玉、黑刚玉、白刚玉、铬刚玉、锆刚玉、镨钕刚玉、矾土烧结刚玉、单晶刚玉等品种。此类刚玉磨料由于没有从根本上改变电熔融的制备方法，不仅能耗高，而且晶粒尺寸大，磨削性能较差，因此在加工领域的应用受到了诸多限制。
陶瓷刚玉磨料诞生于20世纪80年代，是一种新型刚玉磨料，主要通过溶胶-凝胶法来制备含铝前驱体，再经过合适的煅烧工艺处理得到。这一制备手段与传统的电熔融法相比有很多显著的优点，其制备的刚玉磨料内部晶粒尺寸可以达到纳米级别，磨粒内部微观形貌可控，使其在强度、韧性、自锐性、磨削效率、加工精度及使用寿命等方面与传统刚玉磨料相比都有了显著提升，主要应用于高档材料的磨削加工领域，如加工宇航材料、飞机发动机和汽轮机部件的高温合金。
由于现代制造业水平的提高，对加工产品的质量和效率要求越来越高，从而对于磨料的要求也随之越高，使刚玉磨料在向着能满足高速、重负荷、强力磨削和精密磨削的方向发展。但由于纯氧化铝的烧结扩散活化能较高，低温下难以烧结，高温下又易引起晶粒异常长大，影响其显微结构，进而损害磨料强度、韧性和自锐性等一系列的机械性能。因此，如何降低生产过程中的能源消耗，优化磨粒内部显微结构尤其是有效细化内部晶粒，提高磨料磨削性能及使用寿命以适应国内及国际市场的需要，一直以来都是是刚玉磨料研究开发领域的热点。
发明内容
本发明的目的是，通过一种新的添加剂体系降低产品烧成温度和优化显微结构，提供一种能源消耗小，性能优异的纳米晶蓝色陶瓷刚玉磨料及其制备方法。
本发明通过如下技术方案予以实现：
一种纳米晶蓝色陶瓷刚玉磨料，以Al2(SO4)3·18H2O或Al(NO3)3·9H2O为原料，外加添加剂占原料的质量百分比含量为0.15％～0.8％；
所述添加剂的原料组成及其质量百分比含量为：Co(NO3)2·6H2O 5％～25％，(NH4)3AlF65％～20％，C16H36O4Ti 0％～65％，Si(OC2H5)4 0％～40％，Mg(NO3)2·6H2O 0％～50％，Ca(NO3)2·4H2O 0～20％。
上述纳米晶蓝色陶瓷刚玉磨料的制备方法，具有如下步骤：
(1)采用Al2(SO4)3·18H2O或Al(NO3)3·9H2O为原料，溶解于水配成Al3+浓度为0.3～0.6mol/L的溶液；
(2)向步骤(1)的溶液中加入浓度为1mol/L氨水，在常温下进行磁力搅拌，控制pH为9.0～9.8，使其持续反应直至完全凝胶化，然后经抽滤，反复洗涤得到Al(OH)3凝胶前驱体；
(3)按照质量百分比含量为：5％～25％的Co(NO3)2·6H2O，5％～20％的(NH4)3AlF6，0％～65％的C16H36O4Ti，0％～40％的Si(OC2H5)4，0％～50％的Mg(NO3)2·6H2O，0～20％的Ca(NO3)2·4H2O配置添加剂，再将添加剂加入到步骤(2)所得凝胶前驱体中，以水为介质，采用刚玉磨球，湿法球磨使其充分混匀后，再于80℃干燥，得到干凝胶，然后经过造粒、筛分得到前驱体颗粒；
(4)将步骤(3)所得前驱体颗粒于1200℃～1300℃煅烧0.5～2h，或者将前驱体颗粒先加热到1300℃～1400℃，再迅速降到1050℃～1150℃，并保温1～3h，再进一步筛分、分级，得到不同粒度的纳米晶蓝色陶瓷刚玉磨料。
所述步骤(3)的造粒筛分后的前驱体颗粒为尖片型、等积型或长柱型，最终得到形貌可控的磨料颗粒。
所述步骤(4)的蓝色陶瓷刚玉磨料显微结构均匀致密，磨料颗粒内部晶粒呈等轴状或片状，晶粒平均尺寸在80nm～300nm之间。
本发明的有益效果如下：
拓宽了陶瓷刚玉磨料添加剂体系的选择范围，改变了刚玉磨料的显色特征；降低了陶瓷刚玉磨料的烧成温度，与电熔法相比降低了400℃～800℃的生产温度，大幅减少了生产过程中的能源消耗；刚玉磨料内部显微结构均匀致密，细化了晶粒，磨粒内部晶粒尺寸为80nm～300nm；改善了刚玉磨料的强度、韧性和自锐性等机械性能，单颗粒抗压强度最高可达58.6N，冲击韧性比现有的陶瓷刚玉磨料提高15％～25％，制成的陶瓷刚玉砂轮磨削效率比普通刚玉砂轮提高55％以上，使用寿命也得到相应延长。
具体实施方式
下面结合具体实施例进一步说明本发明的技术方案。
本发明原料及添加剂均采用市售分析纯原料，各实施例以制备5g的刚玉磨料为基准称量Al2(SO4)3·18H2O或Al(NO3)3·9H2O原料，外加添加剂占原料的质量百分比含量的范围为0.15％～0.8％。
实施例1
取32.67gAl2(SO4)3·18H2O溶解于水，配成Al3+浓度为0.4mol/L的溶液；
向上述溶液中加入浓度为1mol/L的氨水，不断搅拌，控制pH为9.2，使其持续反应直至完全凝胶化，然后经抽滤、反复洗涤得到Al(OH)3凝胶前驱体；
将0.2wt％的外加添加剂加入Al(OH)3凝胶前驱体中，以水为介质，采用刚玉磨球，湿法球磨使其充分混匀；所述添加剂的组成及其质量百分比含量为：8％Co(NO3)2·6H2O，59％C16H36O4Ti，23％Si(OC2H5)4，10％(NH4)3AlF6；
将球磨后的湿凝胶在80℃干燥得到干凝胶，然后经过造粒、筛分得到前驱体颗粒；
将前驱体颗粒在1200℃煅烧1.5h，再经筛分、分级得到不同粒度的陶瓷刚玉磨料；
所得陶瓷刚玉磨料为浅蓝色，磨料颗粒内部晶粒呈等轴状，晶粒平均尺寸为180nm。
实施例2
取36.76gAl(NO3)3·9H2O溶解于水，配成Al3+浓度为0.5mol/L溶液；
向上述溶液中加入浓度为1mol/L的氨水，不断搅拌，控制pH为9.8，使其持续反应直至完全凝胶化，然后经抽滤、反复洗涤得到Al(OH)3凝胶前驱体；
将0.8wt％的外加添加剂加入Al(OH)3凝胶前驱体中，以水为介质，采用刚玉磨球，湿法球磨使其充分混匀；所述添加剂的组成及其质量百分比含量为：19％Co(NO3)2·6H2O，46％C16H36O4Ti，24％Si(OC2H5)4，11％(NH4)3AlF6；
将球磨后的湿凝胶在80℃干燥得到干凝胶，然后经过造粒、筛分得到前驱体颗粒；
将前驱体颗粒在1300℃煅烧1h，再经筛分、分级得到不同粒度的陶瓷刚玉磨料；
所得陶瓷刚玉磨料为深蓝色，磨料颗粒内部晶粒呈等轴状，晶粒平均尺寸为280nm。
实施例3
取32.67gAl2(SO4)3·18H2O溶解于水，配成Al3+浓度为0.6mol/L溶液；
向上述溶液中加入浓度为1mol/L的氨水，不断搅拌，控制pH为9.2，使其持续反应直至完全凝胶化，然后经抽滤、反复洗涤得到Al(OH)3凝胶前驱体；
将0.54wt％的外加添加剂加入Al(OH)3凝胶前驱体中，以水为介质，采用刚玉磨球，湿法球磨使其充分混匀；所述添加剂的组成及其质量百分比含量为：18％Co(NO3)2·6H2O，50％C16H36O4Ti，24％Mg(NO3)2·6H2O，8％(NH4)3AlF6 0～30％；
将球磨后的湿凝胶在80℃干燥得到干凝胶，然后经过造粒、筛分得到前驱体颗粒；
将前驱体颗粒在1300℃煅烧2h，再经筛分、分级得到不同粒度的陶瓷刚玉磨料；
所得陶瓷刚玉磨料为天蓝色，磨料颗粒内部晶粒呈片状，晶粒平均尺寸为240nm。
实施例4
取36.76gAl(NO3)3·9H2O溶解于水，配成Al3+浓度为0.5mol/L溶液；
向上述溶液中加入浓度为1mol/L的氨水，不断搅拌，控制pH为9.4，使其持续反应直至完全凝胶化，然后经抽滤、反复洗涤得到Al(OH)3凝胶前驱体；
将0.37wt％的外加添加剂加入Al(OH)3凝胶前驱体中，以水为介质，采用刚玉磨球，湿法球磨使其充分混匀；所述添加剂的组成及其质量百分比含量为：16％Co(NO3)2·6H2O，40％Mg(NO3)2·6H2O，30％Si(OC2H5)4，6％(NH4)3AlF6，8％Ca(NO3)2·4H2O；
将球磨后的湿凝胶在80℃干燥得到干凝胶，然后经过造粒、筛分得到前驱体颗粒；
将前驱体颗粒加热到1350℃，然后迅速降到1150℃保温1.5h，再经筛分、分级得到不同粒度的陶瓷刚玉磨料；
所得陶瓷刚玉磨料颗粒为天蓝色，磨料颗粒内部晶粒呈等轴状，晶粒平均尺寸为80nm。
以上对本发明做了实例性的描述，应该说明的是，本发明并不局限于上述实施例，很多细节的变化是可能的，并不因此违背本发明的精神。

Claims (3)

1.一种纳米晶蓝色陶瓷刚玉磨料，以Al2(SO4)3·18H2O或Al(NO3)3·9H2O为原料，外加添加剂占原料的质量百分比含量为0.15％～0.8％；
所述添加剂的原料组成及其质量百分比含量为：Co(NO3)2·6H2O 5％～25％，(NH4)3AlF6 5％～20％，C16H36O4Ti 0％～65％，Si(OC2H5)4 0％～40％，Mg(NO3)2·6H2O 0％～50％，Ca(NO3)2·4H2O 0～20％，其中，C16H36O4Ti、Si(OC2H5)4、Mg(NO3)2·6H2O和Ca(NO3)2·4H2O的两种以上组分不能同时为0；
上述纳米晶蓝色陶瓷刚玉磨料的制备方法，具有如下步骤：
(1)采用Al2(SO4)3·18H2O或Al(NO3)3·9H2O为原料，溶解于水配成Al3+浓度为0.3～0.6mol/L的溶液；
(2)向步骤(1)的溶液中加入浓度为1mol/L氨水，在常温下进行磁力搅拌，控制pH为9～9.8，使其持续反应直至完全凝胶化，然后经抽滤，反复洗涤得到Al(OH)3凝胶前驱体；
(3)按照质量百分比含量为：5％～25％的Co(NO3)2·6H2O，5％～20％的(NH4)3AlF6，0％～65％的C16H36O4Ti，0％～40％的Si(OC2H5)4，0％～50％的Mg(NO3)2·6H2O，0～20％的Ca(NO3)2·4H2O配置添加剂，再将添加剂加入到步骤(2)所得凝胶前驱体中，以水为介质，采用刚玉磨球，湿法球磨使其充分混匀后，再于80℃干燥，得到干凝胶，然后经过造粒、筛分得到前驱体颗粒；
(4)将步骤(3)所得前驱体颗粒于1200℃～1300℃煅烧0.5～2h，或者将前驱体颗粒先加热到1300℃～1400℃，再迅速降到1050℃～1150℃，并保温1～3h，再进一步筛分、分级，得到不同粒度的纳米晶蓝色陶瓷刚玉磨料。
2.根据权利要求1的纳米晶蓝色陶瓷刚玉磨料，其特征在于，所述步骤(3)的造粒筛分后的前驱体颗粒为尖片型、等积型或长柱型，最终得到形貌可控的磨料颗粒。
3.根据权利要求1的纳米晶蓝色陶瓷刚玉磨料，其特征在于，所述步骤(4)的蓝色陶瓷刚玉磨料显微结构均匀致密，磨料颗粒内部晶粒呈等轴状或片状，晶粒平均尺寸在80nm～300nm之间。
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