CN109485392A - 一种微观片状互锁结构陶瓷刚玉磨料 - Google Patents
一种微观片状互锁结构陶瓷刚玉磨料 Download PDFInfo
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Abstract
本发明公开了一种微观片状互锁结构陶瓷刚玉磨料,以拟薄水铝石原料,硝酸为胶凝剂,外加添加剂为原料质量百分比含量的1%~8%;所述添加剂原料组成及其质量百分比含量为(NH4)6Mo7O24 1%~25%,Sr(NO3)2 10%~30%,H3BO3 9%~45%,Mg(NO3)2 10%~45%,KNO3 5%~20%。先以拟薄水铝石为原料,配制成固含量为10%~30%的溶胶;再配制添加剂,于溶胶中外加1%~8%的添加剂,进行搅拌,用硝酸溶液控制溶胶PH值1.5~3.0;再将湿凝胶于60~80℃下干燥,制得干凝胶,再破碎造粒,得到磨料烧结前驱体颗粒,烧结前驱体颗粒于1200℃~1550℃煅烧,得到陶瓷刚玉磨料。本发明显微结构致密,晶粒径长平均尺寸在120nm~200nm之间,晶粒片层厚度在10~60nm之间,细化了磨料晶粒,提高了磨料的单颗粒抗压强度(34N)。
Description
技术领域
本发明属于一种以成分为特征的陶瓷组合物,特别涉及一种拟薄水铝石制备微观片状互锁结构陶瓷刚玉磨料及其制备方法。
背景技术
磨料是指在磨削、研磨和抛光中起切削作用的材料。传统的磨料根据硬度的高低划分为普通磨料和超硬磨料。普通刚玉磨料中的刚玉磨料因其良好的机械性能、稳定的切削性能及其低廉的工艺成本,受到广泛的青睐。随着人造刚玉磨料技术的进步,刚玉磨料按其所含杂质离子的种类和晶型可分为:棕刚玉、白刚玉、单晶刚玉、微晶刚玉、锆刚玉、铬刚玉、陶瓷刚玉等。传统的刚玉磨料主要以电弧炉高温炉熔炼原料,通过还原和分离氧化物,从而得到刚玉磨料。但是这种传统的生产方法存在高能耗、大晶粒尺寸和磨削性能差等特点。电熔刚玉磨料在砂轮中使用时,磨粒等沿着晶粒的解理面碎裂,在磨料破碎时可能损失的磨削表面积达五分之一之多,通常用来制作低档次的磨料用品。
陶瓷刚玉磨料于20世纪80年代诞生,晶粒为亚微米级的刚玉晶体,一般采用溶胶-凝胶工艺合成并进一步烧结而得。陶瓷刚玉磨料砂轮的加工性能高于电熔刚玉磨料砂轮,在合成耗能方面远低于电熔刚玉磨料的生产方法,受到广大用户的欢迎。陶瓷刚玉磨料具有韧性好、自锐性好、磨粒锋利、切削能力强、磨削效率高等特点,符合行业内对磨料的高速、重负荷、精密磨削等要求。因而,如何通过控制磨料的微观形貌,降低生产工艺能耗,制备高磨削性能、高使用寿命的刚玉磨料成为了刚玉磨料开发的热点。
发明内容
本发明的目的,是在现有技术的基础上,克服刚玉磨料微观形貌过于单一和韧性较低的缺点,通过使用一种新的原料和添加剂体系和改善制备工艺,降低刚玉磨料的烧成温度、控制其微观形貌,从而提升磨料的产品性能。提供一种低能耗生产,微观结构均匀的片状互锁结构陶瓷刚玉磨料及其制备方法。
本发明通过如下技术方案得以实现。
一种微观片状互锁结构陶瓷刚玉磨料,以拟薄水铝石即水合氧化铝为原料,硝酸为胶凝剂,外加添加剂为原料质量百分比含量的1%~8%;
所述添加剂的原料组成及其质量百分比含量为:
(NH4)6Mo7O24 1%~25%,
Sr(NO3)2 10%~30%,
H3BO3 9%~45%,
Mg(NO3)2 10%~45%,
KNO3 5%~20%;
上述微观片状互锁结构陶瓷刚玉磨料的制备方法,具体步骤如下:
(1)以拟薄水铝石为原料,加入去离子水并搅拌,配制成固含量为10%~30%的溶胶;
(2)按照原料质量百分比含量为:1%~25%的(NH4)6Mo7O24,10%~30%的Sr(NO3)2,9%~45%的H3BO3,10%~45%的Mg(NO3)2,5%~20%的KNO3配制添加剂;再于步骤(1)所得溶胶中外加1%~8%的添加剂,同时用磁力搅拌器对溶胶进行搅拌;
(3)将硝酸用去离子水稀释,向步骤(2)的溶胶中缓慢滴加稀释后的硝酸,常温下进行搅拌,控制PH值在1.5~3.0,使其反应完全,停止加硝酸后继续搅拌1h,使添加剂均匀分散在溶胶中直至完全凝胶化;再将制得的湿凝胶于60~80℃下干燥,制得干凝胶;再对干凝胶进行破碎造粒、筛分后得到磨料烧结前驱体颗粒;
(4)对步骤(3)所得的烧结前驱体于1200℃~1550℃下进行煅烧,保温2h,并进一步的筛分和分级,得到不同粒度的微观片状互锁结构陶瓷刚玉磨料。
所述步骤(1)的拟薄水铝石粒径为60nm;
所述步骤(3)的稀释的硝酸溶液浓度为0.01~0.04mol/L;
所述步骤(3)的烧结前驱体之前的“筛分”是过40目筛;
所述步骤(4)得到的的微观片状互锁陶瓷刚玉磨料得显微结构致密,磨料颗粒呈片状晶粒相互穿插,即片状晶粒之间呈“互锁”,晶粒径长平均尺寸在120nm~200nm之间,晶粒片层厚度在10~60nm之间。
本发明通过改变添加剂的配比,控制刚玉磨料的微观结构,省去传统刚玉磨料中的球磨工序,降低了烧结温度。另外,生产过程中的干凝胶废料可循环利用,与传统的电熔法相比大幅度减少了生产过程中的能耗。微观片状互锁结构陶瓷刚玉磨料显微结构致密,磨料颗粒呈片状晶粒相互穿插,即晶粒之间“互锁”,晶粒径长平均尺寸在120nm~200nm之间,晶粒片层厚度在10~60nm之间。通过控制添加剂比例及烧结制度,细化了磨料晶粒,提高了刚玉磨料的单颗粒抗压强度、断裂韧性及自锐性等机械性能,其中磨料单颗粒抗压强度为34N。
附图说明
图1为实施例3的扫描电镜微观形貌图。
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。
本发明使用原料为纳米级拟薄水铝石的工业纯原料,添加剂和硝酸均采用分析纯原料,各实施例均以制备10g的刚玉磨料为基准称量拟薄水铝石原料,拟薄水铝石粒径为60nm。引入的添加剂为在拟薄水铝石原料基础上外加质量百分比含量的1%~8%。
实施例1
(1)取15g拟薄水铝石,溶解于45mL去离子水,配置成固含量为25%的溶胶。
(2)再于步骤(1)所得溶胶中外加3%的添加剂,常温下以恒定速度同一方向搅拌,使添加剂在溶胶均匀分散。所述添加剂的组成及其质量百分比含量为10.4%(NH4)6Mo7O24,18.3%Sr(NO3)2,10.3%H3BO3,45%Mg(NO3)2,16%KNO3。
(3)将硝酸用去离子水稀释,稀释后的硝酸溶液浓度为0.04mol/L,向步骤(2)的溶胶中缓慢滴加稀释后的硝酸水溶液,常温下进行搅拌,控制PH值在2.5,使其反应完全,停止加硝酸后继续搅1h,使添加剂均匀分散在溶胶中直至完全凝胶化;再将制得的湿凝胶于60℃下干燥,制得干凝胶;再对干凝胶进行破碎造粒、过40目筛,得到磨料烧结前驱体颗粒。
(4)对步骤(3)所得的烧结前驱体于1200℃进行煅烧,保温2h,筛分后得到微观片状互锁结构陶瓷刚玉磨料。
所得微观片状互锁纳米晶陶瓷刚玉磨料平均晶粒径长为130nm,片状厚度为34nm,单颗粒抗压强度为30N。
实施例2
(1)取15g拟薄水铝石,溶解于45mL去离子水,配置成固含量为25%的溶胶。
(2)再于步骤(1)所得溶胶中外加4%的添加剂,常温下以恒定速度同一方向搅拌,使添加剂在溶胶均匀分散。所述添加剂的组成及其质量百分比含量为15.2%(NH4)6Mo7O24,20.1%Sr(NO3)2,15%H3BO3,30%Mg(NO3)2,19.7%KNO3。
(3)将硝酸用去离子水稀释,稀释后的硝酸溶液浓度为0.04mol/L,向步骤(2)的溶胶中缓慢滴加稀释后的硝酸水溶液,常温下进行搅拌,控制PH值在3,使其反应完全,停止加硝酸后继续搅拌1h,使添加剂均匀分散在溶胶中直至完全凝胶化;再将制得的湿凝胶于60℃下干燥,制得干凝胶;再对干凝胶进行破碎造粒、过40目筛,得到磨料烧结前驱体颗粒。
(4)对步骤(3)所得的烧结前驱体于1300℃进行煅烧,保温2h,筛分后得到微观片状互锁结构陶瓷刚玉磨料。
所得微观片状互锁纳米晶陶瓷刚玉磨料平均晶粒径长为170nm,片状厚度为40nm,单颗粒抗压强度为32N。
实施例3
(1)取15g拟薄水铝石,溶解于45mL去离子水,配置成固含量为25%的溶胶。
(2)再于步骤(1)所得溶胶中外加6%的添加剂,常温下以恒定速度同一方向搅拌,使添加剂在溶胶均匀分散。所述添加剂的组成及其质量百分比含量为18.7%(NH4)6Mo7O24,26%Sr(NO3)2,30.3%H3BO3,18.9%Mg(NO3)2,6.1%KNO3。
(3)将硝酸用去离子水稀释,稀释后的硝酸溶液浓度为0.03mol/L,向步骤(2)的溶胶中缓慢滴加稀释后的硝酸水溶液,常温下进行搅拌,控制PH值在3,使其反应完全,停止加硝酸后继续搅拌1h,使添加剂均匀分散在溶胶中直至完全凝胶化;再将制得的湿凝胶于60℃下干燥,制得干凝胶;再对干凝胶进行破碎造粒、过40目筛,得到磨料烧结前驱体颗粒;
(4)对步骤(3)所得的烧结前驱体于1400℃进行煅烧,保温2h,筛分后得到微观片状互锁结构陶瓷刚玉磨料。
所得微观片状互锁纳米晶陶瓷刚玉磨料平均晶粒径长为180nm,片状厚度为42nm,单颗粒抗压强度为33.3N。
图1是实施例3的扫描电镜微观形貌图,由图中可以看出,微观片状晶粒之间相互穿插,均匀地呈“互锁”状态,片状晶粒形貌均匀,利于提高磨料的韧性。
实施例4
(1)取15g拟薄水铝石,溶解于60mL去离子水,配置成固含量为20%的溶胶。
(2)再于步骤(1)所得溶胶中外加6%的添加剂,常温下以恒定速度同一方向搅拌,使添加剂在溶胶均匀分散。所述添加剂的组成及其质量百分比含量为23%(NH4)6Mo7O24,27.9%Sr(NO3)2,29.2%H3BO3,10.9%Mg(NO3)2,9%KNO3。
(3)将硝酸用去离子水稀释,稀释后的硝酸溶液浓度为0.04mol/L,向步骤(2)的溶胶中缓慢滴加稀释后的硝酸水溶液,常温下进行搅拌,控制PH值在3,使其反应完全,停止加硝酸后继续搅拌1h,使添加剂均匀分散在溶胶中直至完全凝胶化;再将制得的湿凝胶于60℃下干燥,制得干凝胶;再对干凝胶进行破碎造粒、过40目筛,得到磨料烧结前驱体颗粒。
(4)对步骤(3)所得的烧结前驱体于1550℃进行煅烧,保温2h,筛分后得到微观片状互锁结构陶瓷刚玉磨料。所得微观片状互锁纳米晶陶瓷刚玉磨料平均晶粒径长为200nm,片状厚度为43nm,单颗粒抗压强度为34N。
本发明并不局限于上述实例,很多细节的变化是可能的,但这不违背本发明的范围和创新精神。
以上实例仅是对本发明做出的示例性描述,在不脱离本发明核心方法的前提下,对烧结温度、PH值等方面做的简单变形或其他本领域技术人员能够不花费创造力的等同替换均落入本发明的范围。
Claims (5)
1.一种微观片状互锁结构陶瓷刚玉磨料,以拟薄水铝石即水合氧化铝为原料,硝酸为胶凝剂,外加添加剂为原料质量百分比含量的1%~8%;
所述添加剂的原料组成及其质量百分比含量为:
(NH4)6Mo7O24 1%~25%,
Sr(NO3)2 10%~30%,
H3BO3 9%~45%,
Mg(NO3)2 10%~45%,
KNO3 5%~20%;
上述微观片状互锁结构陶瓷刚玉磨料的制备方法,具体步骤如下:
(1)以拟薄水铝石为原料,加入去离子水并搅拌,配制成固含量为10%~30%的溶胶;
(2)按照原料质量百分比含量为:1%~25%的(NH4)6Mo7O24,10%~30%的Sr(NO3)2,9%~45%的H3BO3,10%~45%的Mg(NO3)2,5%~20%的KNO3配制添加剂;再于步骤(1)所得溶胶中外加1%~8%的添加剂,同时用磁力搅拌器对溶胶进行搅拌;
(3)将硝酸用去离子水稀释,向步骤(2)的溶胶中缓慢滴加稀释后的硝酸,常温下进行搅拌,控制PH值在1.5~3.0,使其反应完全,停止加硝酸后继续搅拌1h,使添加剂均匀分散在溶胶中直至完全凝胶化;再将制得的湿凝胶于60~80℃下干燥,制得干凝胶;再对干凝胶进行破碎造粒、筛分后得到磨料烧结前驱体颗粒;
(4)对步骤(3)所得的烧结前驱体于1200℃~1550℃下进行煅烧,保温2h,并进一步的筛分和分级,得到不同粒度的微观片状互锁结构陶瓷刚玉磨料。
2.根据权利要求1所述的一种微观片状互锁结构陶瓷刚玉磨料,其特征在于,所述步骤(1)的拟薄水铝石粒径为60nm。
3.根据权利要求1所述的一种微观片状互锁结构陶瓷刚玉磨料,其特征在于,所述步骤(3)的稀释的硝酸溶液浓度为0.01~0.04mol/L。
4.根据权利要求1所述的一种微观片状互锁结构陶瓷刚玉磨料,其特征在于,所述步骤(3)的烧结前驱体之前的“筛分”是过40目筛。
5.根据权利要求1所述的一种微观片状互锁结构陶瓷刚玉磨料,其特征在于,所述步骤(4)得到的的微观片状互锁陶瓷刚玉磨料得显微结构致密,磨料颗粒呈片状晶粒相互穿插,即片状晶粒之间呈“互锁”,晶粒径长平均尺寸在120nm~200nm之间,晶粒片层厚度在10~60nm之间。
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