CN113603493B - 一种耐磨氮化硅陶瓷刀具材料及其制备方法 - Google Patents

一种耐磨氮化硅陶瓷刀具材料及其制备方法 Download PDF

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CN113603493B
CN113603493B CN202110759757.9A CN202110759757A CN113603493B CN 113603493 B CN113603493 B CN 113603493B CN 202110759757 A CN202110759757 A CN 202110759757A CN 113603493 B CN113603493 B CN 113603493B
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silicon nitride
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CN113603493A (zh
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杨文伍
陈祯祯
任莉
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Ningbo Silver Porcelain New Material Co ltd
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Abstract

本发明提供了一种耐磨氮化硅陶瓷刀具材料，由以下重量百分比的组分制备而成：氧化铝2～3％，氧化镧4～5％，氧化镝1～2％，耐磨助剂1～1.5％，其余为氮化硅，各组分的重量百分比之和为100％。本发明还提供了该耐磨氮化硅陶瓷刀具材料的制备方法。本发明所提供的耐磨氮化硅陶瓷刀具材料具有较强的耐磨性能和较高的硬度、抗弯强度、致密度。

Description

一种耐磨氮化硅陶瓷刀具材料及其制备方法
技术领域
本发明涉及一种刀具材料，特别是涉及一种耐磨氮化硅陶瓷刀具材料及其制备方法。
背景技术
氮化硅陶瓷由于具有优异的耐高温性能、耐磨损、耐腐蚀以及高硬度等优点，在切削刀具、轴承、高压柱塞、密封环、耐磨元件等方面得到了广泛运用。目前氮化硅陶瓷的主要研究方向包括：烧结助剂选择，烧结工艺参数控制，微观结构(包括晶粒尺寸，α-氮化硅向β-氮化硅转化的晶相转化率)，力学性能，热学性能，电性能等。氮化硅陶瓷的摩擦因数较低，适用于大进给量或断续切削铸铁、高温合金、镍基合金等的切削刀具，但是在高速切削过程中，氮化硅陶瓷刀具的化学稳定性下降，导致其表面产生磨损，甚至会产生严重的月牙洼磨损。
发明内容
本发明要解决的技术问题是提供一种耐磨氮化硅陶瓷刀具材料，其具有较强的耐磨性能和较高的硬度、抗弯强度、致密度。
为解决上述技术问题，本发明的技术方案是：
一种耐磨氮化硅陶瓷刀具材料，由以下重量百分比的组分制备而成：氧化铝2～3％，氧化镧4～5％，氧化镝1～2％，耐磨助剂1～1.5％，其余为氮化硅，各组分的重量百分比之和为100％。
进一步地，本发明所述耐磨助剂由以下步骤制成：
A1.将硝酸锆加入去离子水中混合均匀得到硝酸锆溶液，将硫酸钛加入去离子水中混合均匀得到硫酸钛溶液，将硝酸锆溶液、硫酸钛溶液混合后滴加入氨水直至pH值为9得到沉淀，室温老化3小时后将沉淀抽滤得到固体物，将固体物水洗至中性后100℃下干燥24小时，转入箱式炉中400℃下煅烧3小时得到钛锆复合氧化物；
A2.将炭黑、步骤A1所得钛锆复合氧化物混合均匀，转入管式炉中，通氩气保护下升温至1500℃后保温反应3小时，随炉冷却至室温后得到耐磨助剂。
进一步地，本发明所述耐磨助剂的制备步骤A1中，硝酸锆溶液的浓度为0.4mol/L，硫酸钛溶液的浓度为0.4mol/L，硝酸锆溶液、硫酸钛溶液的体积比为2:3。
进一步地，本发明所述耐磨助剂的制备步骤A2中，炭黑、钛锆复合氧化物的重量比为1:2，管式炉的升温速度为10℃/分。
进一步地，本发明所述氮化硅中α-氮化硅的含量为96wt％，β-氮化硅的含量为4wt％。
本发明要解决的另一技术问题提供上述耐磨氮化硅陶瓷刀具材料的制备方法。
为解决上述技术问题，技术方案是：
一种耐磨氮化硅陶瓷刀具材料的制备方法，包括以下步骤：
B1.按重量百分比称取各组分后混合均匀得到混合粉，将混合粉加入无水乙醇中超声分散30～40分钟得到混合液；
B2.将步骤B1所得混合液、磨球加入球磨罐中，球磨18～24小时后得到混合浆料；
B3.将步骤B2所得混合浆料旋转蒸发干燥后转入真空烘箱中100℃下烘干，取出后研磨过100目筛得到混合粉料；
B4.将步骤B3所得混合粉料装入模具中干压成型，然后冷等静压保压2分钟得到坯料；
B5.将步骤B4所得压坯置于通氮气保护的烧结炉中，真空热压烧结后随炉冷却至室温得到耐磨氮化硅陶瓷刀具材料。
进一步地，本发明所述步骤B1中，混合粉、无水乙醇的重量比为1:1.5。
进一步地，本发明所述步骤B2中，磨球为氮化硅球，混合液、磨球的重量比为1:7。
进一步地，本发明所述步骤B4中，冷等静压保压时的压力为300MPa。
进一步地，本发明所述步骤B5中，真空热压烧结的压力为30MPa，温度为1700～1800℃，升温速度为10℃/分，保温时间为1～1.5小时。
与现有技术相比，本发明具有以下有益效果：
本发明将硝酸锆与硫酸钛通过共沉淀法制得钛锆复合氧化物，然后将其与炭黑通过碳热还原法原位还原得到耐磨助剂，该耐磨助剂具有较高的硬度和优异的耐磨性能，能有效提高氮化硅陶瓷刀具材料的硬度和耐磨性能；此外，本发明使用的氧化镝能起到较好的助烧结作用，有效促进氮化硅液相形成和致密化，进而提高氮化硅陶瓷刀具材料的致密度和抗弯强度。
具体实施方式
下面将结合具体实施例来详细说明本发明，在此本发明的示意性实施例及其说明用来解释本发明，但并不作为对本发明的限定。
实施例1
耐磨氮化硅陶瓷刀具材料，由以下重量百分比的组分制备而成：氧化铝2.5％，氧化镧4.4％，氧化镝1.5％，耐磨助剂1.4％，其余为氮化硅，各组分的重量百分比之和为100％，氮化硅中α-氮化硅的含量为96wt％，β-氮化硅的含量为4wt％。
耐磨助剂由以下步骤制成：
A1.将硝酸锆加入去离子水中混合均匀得到浓度为0.4mol/L的硝酸锆溶液，将硫酸钛加入去离子水中混合均匀得到浓度为0.4mol/L的硫酸钛溶液，将体积比为2:3的硝酸锆溶液、硫酸钛溶液混合后滴加入氨水直至pH值为9得到沉淀，室温老化3小时后将沉淀抽滤得到固体物，将固体物水洗至中性后100℃下干燥24小时，转入箱式炉中400℃下煅烧3小时得到钛锆复合氧化物；
A2.将重量比为1:2的炭黑、步骤A1所得钛锆复合氧化物混合均匀，转入管式炉中，通氩气保护下以10℃/分的升温速度升温至1500℃后保温反应3小时，随炉冷却至室温后得到耐磨助剂。
该耐磨氮化硅陶瓷刀具材料的制备方法包括以下步骤：
B1.按重量百分比称取各组分后混合均匀得到混合粉，按1:1.5的重量比将混合粉加入无水乙醇中超声分散35分钟得到混合液；
B2.将重量比为1:7的步骤B1所得混合液、氮化硅球加入球磨罐中，球磨21小时后得到混合浆料；
B3.将步骤B2所得混合浆料旋转蒸发干燥后转入真空烘箱中100℃下烘干，取出后研磨过100目筛得到混合粉料；
B4.将步骤B3所得混合粉料装入模具中干压成型，然后300MPa压力下冷等静压保压2分钟得到坯料；
B5.将步骤B4所得压坯置于通氮气保护的烧结炉中，真空热压烧结后随炉冷却至室温得到耐磨氮化硅陶瓷刀具材料，真空热压烧结的压力为30MPa，温度为1750℃，升温速度为10℃/分，保温时间为1.2小时。
实施例2
耐磨氮化硅陶瓷刀具材料，由以下重量百分比的组分制备而成：氧化铝2.8％，氧化镧4.5％，氧化镝2％，耐磨助剂1％，其余为氮化硅，各组分的重量百分比之和为100％，氮化硅中α-氮化硅的含量为96wt％，β-氮化硅的含量为4wt％。
耐磨助剂的制备步骤与实施例1一样。
该耐磨氮化硅陶瓷刀具材料的制备方法包括以下步骤：
B1.按重量百分比称取各组分后混合均匀得到混合粉，按1:1.5的重量比将混合粉加入无水乙醇中超声分散40分钟得到混合液；
B2.将重量比为1:7的步骤B1所得混合液、氮化硅球加入球磨罐中，球磨18小时后得到混合浆料；
B3.将步骤B2所得混合浆料旋转蒸发干燥后转入真空烘箱中100℃下烘干，取出后研磨过100目筛得到混合粉料；
B4.将步骤B3所得混合粉料装入模具中干压成型，然后300MPa压力下冷等静压保压2分钟得到坯料；
B5.将步骤B4所得压坯置于通氮气保护的烧结炉中，真空热压烧结后随炉冷却至室温得到耐磨氮化硅陶瓷刀具材料，真空热压烧结的压力为30MPa，温度为1780℃，升温速度为10℃/分，保温时间为1.1小时。
实施例3
耐磨氮化硅陶瓷刀具材料，由以下重量百分比的组分制备而成：氧化铝2％，氧化镧5％，氧化镝1.8％，耐磨助剂1.5％，其余为氮化硅，各组分的重量百分比之和为100％，氮化硅中α-氮化硅的含量为96wt％，β-氮化硅的含量为4wt％。
耐磨助剂的制备步骤与实施例1一样。
该耐磨氮化硅陶瓷刀具材料的制备方法包括以下步骤：
B1.按重量百分比称取各组分后混合均匀得到混合粉，按1:1.5的重量比将混合粉加入无水乙醇中超声分散32分钟得到混合液；
B2.将重量比为1:7的步骤B1所得混合液、氮化硅球加入球磨罐中，球磨20小时后得到混合浆料；
B3.将步骤B2所得混合浆料旋转蒸发干燥后转入真空烘箱中100℃下烘干，取出后研磨过100目筛得到混合粉料；
B4.将步骤B3所得混合粉料装入模具中干压成型，然后300MPa压力下冷等静压保压2分钟得到坯料；
B5.将步骤B4所得压坯置于通氮气保护的烧结炉中，真空热压烧结后随炉冷却至室温得到耐磨氮化硅陶瓷刀具材料，真空热压烧结的压力为30MPa，温度为1800℃，升温速度为10℃/分，保温时间为1小时。
实施例4
耐磨氮化硅陶瓷刀具材料，由以下重量百分比的组分制备而成：氧化铝3％，氧化镧4％，氧化镝1％，耐磨助剂1.2％，其余为氮化硅，各组分的重量百分比之和为100％，氮化硅中α-氮化硅的含量为96wt％，β-氮化硅的含量为4wt％。
耐磨助剂的制备步骤与实施例1一样。
该耐磨氮化硅陶瓷刀具材料的制备方法包括以下步骤：
B1.按重量百分比称取各组分后混合均匀得到混合粉，按1:1.5的重量比将混合粉加入无水乙醇中超声分散30分钟得到混合液；
B2.将重量比为1:7的步骤B1所得混合液、氮化硅球加入球磨罐中，球磨24小时后得到混合浆料；
B3.将步骤B2所得混合浆料旋转蒸发干燥后转入真空烘箱中100℃下烘干，取出后研磨过100目筛得到混合粉料；
B4.将步骤B3所得混合粉料装入模具中干压成型，然后300MPa压力下冷等静压保压2分钟得到坯料；
B5.将步骤B4所得压坯置于通氮气保护的烧结炉中，真空热压烧结后随炉冷却至室温得到耐磨氮化硅陶瓷刀具材料，真空热压烧结的压力为30MPa，温度为1700℃，升温速度为10℃/分，保温时间为1.5小时。
对比例1：
与实施例1的不同之处在于：组分中不包括耐磨助剂，并省去耐磨助剂的制备步骤。
对比例2：
与实施例1的不同之处在于：组分中不包括氧化镝。
实验例1：耐磨性能测试
将实施例1～4、对比例1～2制得的氮化硅陶瓷材料制成10mm×3mm×3mm尺寸的试样，使用往复滑动式摩擦磨损试验机对试样进行磨损率测试，上对磨材料为φ10mm的氮化硅球，下对磨材料为前述试样。对试样进行打磨抛光处理后施加100N径向载荷，对磨时间为15分钟，线速度为6mm/秒，使用超景深三维显微镜测定试样表面的磨痕。
磨损率越低表明耐磨性能越好。测试结果如表1所示：
Figure BDA0003149094940000051
Figure BDA0003149094940000061
表1
由表1以看出，本发明实施例1～4的磨损率均较低，表面本发明制得的氮化硅陶瓷刀具材料具有较好的耐磨性能。对比例1～2的部分组分与实施例1不同，与实施例1相比，对比例1的磨损率明显升高，表明本发明使用的耐磨助剂能有效提高氮化硅陶瓷刀具材料的耐磨性能。
实验例2：硬度测试
采用压痕法分别测定实施例1～4、对比例1～2制得的氮化硅陶瓷刀具材料的维氏硬度，载荷为5kg，以在不同位置进行10次测试后计算出的平均值为准。
测试结果如表2所示：
维氏硬度(GPa)
实施例1 21.2
实施例2 20.3
实施例3 21.3
实施例4 20.6
对比例1 16.4
对比例2 21.0
表2
由表2可以看出，本发明实施例1～4制得的氮化硅陶瓷刀具材料的硬度均较高。对比例1～2的部分组分与实施例1不同，与实施例1相比，对比例1的硬度明显降低，表明本发明使用的耐磨助剂能有效提高氮化硅陶瓷刀具材料的硬度。
实验例3：抗弯强度测试
将实施例1～4、对比例1～2制得的氮化硅陶瓷刀具材料制成40mm×4mm×3mm尺寸的试样，使用拉力试验机采用三点弯曲法对试样进行抗弯强度测试，跨距为30mm，加载速度为0.5mm/分。
测试结果如表3所示：
抗弯强度(MPa)
实施例1 948
实施例2 956
实施例3 940
实施例4 932
对比例1 946
对比例2 877
表3
由表3可以看出，本发明实施例1～4制得的氮化硅陶瓷刀具材料的抗弯强度均较高。对比例1～2的部分组分与实施例1不同，与实施例1相比，对比例2的抗弯强度明显降低，表明本发明使用的氧化镝能有效提高氮化硅陶瓷刀具材料的抗弯强度。
实验例4：致密度测试
采用阿基米德法分别测定实施例1～4、对比例1～2制得的氮化硅陶瓷刀具材料的致密度，测试结果如表4所示：
致密度(％)
实施例1 97.28
实施例2 97.44
实施例3 97.36
实施例4 97.15
对比例1 97.25
对比例2 91.09
表4
由表4可以看出，本发明实施例1～4制得的氮化硅陶瓷刀具材料的致密度均较高。对比例1～2的部分组分与实施例1不同，与实施例1相比，对比例2的致密度明显降低，表明本发明使用的氧化镝能有效提高氮化硅陶瓷刀具材料的致密度。
上述实施例仅例示性说明本发明的原理及其功效，而非用于限制本发明。任何熟悉此技术的人士皆可在不违背本发明的精神及范畴下，对上述实施例进行修饰或改变。因此，举凡所属技术领域中具有通常知识者在未脱离本发明所揭示的精神与技术思想下所完成的一切等效修饰或改变，仍应由本发明的权利要求所涵盖。

Claims (9)

1.一种耐磨氮化硅陶瓷刀具材料，其特征在于：由以下重量百分比的组分制备而成：氧化铝2～3％，氧化镧4～5％，氧化镝1～2％，耐磨助剂1～1.5％，其余为氮化硅，各组分的重量百分比之和为100％；
所述耐磨助剂由以下步骤制成：
A1.将硝酸锆加入去离子水中混合均匀得到硝酸锆溶液，将硫酸钛加入去离子水中混合均匀得到硫酸钛溶液，将硝酸锆溶液、硫酸钛溶液混合后滴加入氨水直至pH值为9得到沉淀，室温老化3小时后将沉淀抽滤得到固体物，将固体物水洗至中性后100℃下干燥24小时，转入箱式炉中400℃下煅烧3小时得到钛锆复合氧化物；
A2.将炭黑、步骤A1所得钛锆复合氧化物混合均匀，转入管式炉中，通氩气保护下升温至1500℃后保温反应3小时，随炉冷却至室温后得到耐磨助剂。
2.根据权利要求1所述的一种耐磨氮化硅陶瓷刀具材料，其特征在于：所述耐磨助剂的制备步骤A1中，硝酸锆溶液的浓度为0.4mol/L，硫酸钛溶液的浓度为0.4mol/L，硝酸锆溶液、硫酸钛溶液的体积比为2:3。
3.根据权利要求1所述的一种耐磨氮化硅陶瓷刀具材料，其特征在于：所述耐磨助剂的制备步骤A2中，炭黑、钛锆复合氧化物的重量比为1:2，管式炉的升温速度为10℃/分。
4.根据权利要求1所述的一种耐磨氮化硅陶瓷刀具材料，其特征在于：所述氮化硅中α-氮化硅的含量为96wt％，β-氮化硅的含量为4wt％。
5.根据权利要求1～4任意一项所述的一种耐磨氮化硅陶瓷刀具材料的制备方法，其特征在于：包括以下步骤：
B1.按重量百分比称取各组分后混合均匀得到混合粉，将混合粉加入无水乙醇中超声分散30～40分钟得到混合液；
B2.将步骤B1所得混合液、磨球加入球磨罐中，球磨18～24小时后得到混合浆料；
B3.将步骤B2所得混合浆料旋转蒸发干燥后转入真空烘箱中100℃下烘干，取出后研磨过100目筛得到混合粉料；
B4.将步骤B3所得混合粉料装入模具中干压成型，然后冷等静压保压2分钟得到坯料；
B5.将步骤B4所得压坯置于通氮气保护的烧结炉中，真空热压烧结后随炉冷却至室温得到耐磨氮化硅陶瓷刀具材料。
6.根据权利要求5所述的一种耐磨氮化硅陶瓷刀具材料的制备方法，其特征在于：所述步骤B1中，混合粉、无水乙醇的重量比为1:1.5。
7.根据权利要求5所述的一种耐磨氮化硅陶瓷刀具材料的制备方法，其特征在于：所述步骤B2中，磨球为氮化硅球，混合液、磨球的重量比为1:7。
8.根据权利要求5所述的一种耐磨氮化硅陶瓷刀具材料的制备方法，其特征在于：所述步骤B4中，冷等静压保压时的压力为300MPa。
9.根据权利要求5所述的一种耐磨氮化硅陶瓷刀具材料的制备方法，其特征在于：所述步骤B5中，真空热压烧结的压力为30MPa，温度为1700～1800℃，升温速度为10℃/分，保温时间为1～1.5小时。
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