CN112174650A - 一种自润滑刀具用高韧性陶瓷材料的制备方法 - Google Patents
一种自润滑刀具用高韧性陶瓷材料的制备方法 Download PDFInfo
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Abstract
本发明涉及一种自润滑刀具用高韧性陶瓷材料的制备方法,属于陶瓷材料技术领域。本发明通过添加氧化锆晶须,制备一种自润滑刀具用高韧性陶瓷材料,氧化锆常温下为四方相氧化锆,当温度升高时,四方相氧化锆转变为单斜相,诱导表面产生压缩应力,从而阻止或延缓裂纹的继续扩展,陶瓷材料中添加氧化锆晶须,可以有效提高陶瓷材料的强度,当晶须受到外加作用力时,在陶瓷材料内部桥连的晶须会产生一个作用力迫使裂纹闭合,从而达到耗费一些外力所做功的效果,进而增加陶瓷材料的韧性和强度,当裂纹由陶瓷材料表面扩散到晶须时,裂纹的扩散方向就会发生改变,因为晶须和陶瓷材料的解离而导致了裂纹沿着晶须进行扩散,这不仅增大了所形成的新表面的面积,而且还可以使裂纹在其临界尺寸之内,进而加强陶瓷材料的韧性。
Description
技术领域
本发明涉及一种自润滑刀具用高韧性陶瓷材料的制备方法,属于陶瓷材料技术领域。
背景技术
切削加工是机械领域的重要组成部分,其中千切削能实现刀具在没有润滑液的条件下的切削加工,使环境效益得到保证,但是干切削条件下刀具与加工工件会发生剧烈摩擦,使得加工条件恶化,加工过程中高摩擦系数以及摩擦产生高热量,使得刀具的寿命大幅缩减,于此同时,难加工材料的涌现也对切削刀具提出了更高的要求,这就为自润滑陶瓷刀具材料的出现和发展提供了契机。陶瓷材料作为无机非金属材料中的最重要的组成之一,在国民经济中的各个领域中有着广阔的应用前景,切削加工作为机械加工技术中最重要的组成部分之一,随着绿色加工工业的兴起,寻找能实现加工工艺的高效、低成本、低污染一直是切削切加工发展重要内容,因此而对刀具材料的研宄成为机械学科发展的重要内容。
自润滑陶瓷刀具除了具有陶瓷刀具的高硬度、较好的化学稳定性,同时也有着良好的自润滑能力。通过以不同的形式添加固体润滑剂到陶瓷材料中,使最终设计、制备的自润滑陶瓷刀具能在整个切削过程中保持较低的摩擦系数,能较好地实现切削刀具的自润滑能力,提升刀具的切削性能。但是陶瓷材料主要是由共价键和离子键构成的,有着相对较高的缺陷敏感性,因此,陶瓷材料的脆性断裂成为限制陶瓷材料应用的最重要的原因之一。
发明内容
本发明所要解决的技术问题:针对陶瓷材料的脆性大,容易断裂的问题,提供了一种自润滑刀具用高韧性陶瓷材料的制备方法。
为解决上述技术问题,本发明采用的技术方案是:
(1)按重量份数计,分别称量60~80份刚玉粉、12~16份氧化锆晶须、18~24份氢氧化铝包覆氟化钙粉末、3~6份氧化镁粉末、0.6~0.8份硼酸、200~300份无水乙醇;
(2)将刚玉粉、氧化锆晶须、氢氧化铝包覆氟化钙粉末、氧化镁粉末、硼酸加入无水乙醇中,常温下以200~250r/min转速搅拌1~2h,得混合浆料;
(3)将混合浆料置于热压烧结炉内,在1200~1400℃、20~40MPa的条件下保温保压烧结2~4h,随炉冷却至室温,得自润滑刀具用高韧性陶瓷材料。
步骤(1)所述的刚玉粉的平均粒径为80~100μm,氧化镁粉末的平均粒径为50~60μm。
步骤(1)所述的氢氧化铝包覆氟化钙粉末的具体制备步骤为:
(1)按重量份数计,分别称量20~30份氟化钙粉末、30~45份硝酸铝、4~6份聚乙烯吡咯烷酮、120~180份无水乙醇、60~90份去离子水;
(2)将氟化钙粉末、聚乙烯吡咯烷酮加入无水乙醇中,常温下以300~400r/min转速搅拌20~30min,再置于超声波分散机中,常温下超声分散10~20min,得氟化钙分散液;
(3)将硝酸铝加入去离子水中,常温下以160~200r/min转速搅拌10~12min,得硝酸铝溶液;
(4)将硝酸铝溶液加入氟化钙分散液,调节pH至8~9,在40~60℃的水浴条件下以200~250r/min转速搅拌20~30min,常温冷却,过滤,取滤饼,置于60~80℃的烘箱中干燥1~2h,常温冷却,得氢氧化铝包覆氟化钙粉末;
步骤(1)所述的氟化钙粉末的平均粒度为40~60nm。
步骤(2)所述的超声分散的功率为300~400W。
步骤(4)所述的pH调节采用的是质量分数10%的氨水。
步骤(1)所述的氧化锆晶须的具体制备步骤为:
(1)按重量份数计,分别称量20~30份氧化锆干凝胶粉末、20~30份偏钒酸钠、2~3份氟化钠;
(2)将氧化锆干凝胶粉末、偏钒酸钠、氟化钠置于搅拌机中,常温下以300~400r/min转速搅拌混合20~30min,得干凝胶混合物;
(3)将干凝胶混合物置于微波烧结炉中,常温下以10℃/min的速率升温至400~500℃,保温烧结6~8h,随炉冷却至室温,用去离子水洗涤5~7次,置于80~100℃的烘箱中干燥1~2h,得氧化锆晶须。
步骤(1)所述的氧化锆干凝胶粉末的具体制备步骤为:
(1)按重量份数计,分别称量5~10份四氯化锆、25~50份无水乙醇;
(2)将四氯化锆加入无水乙醇中,置于110~120℃的油浴条件下以120~160r/min转速搅拌回流20~24h,常温冷却,得氧化锆溶胶;
(3)将氧化锆溶胶置于马弗炉中,常温下以5℃/min的速率升温至300~400℃,保温10~20min,再以10℃/min的速率升温至800~900℃,保温煅烧40~60min,随炉冷却至室温,得氧化锆干凝胶,研磨,过200目,得氧化锆干凝胶粉末。
本发明与其他方法相比,有益技术效果是:
本发明通过添加氧化锆晶须,制备一种自润滑刀具用高韧性陶瓷材料,氧化锆常温下为四方相氧化锆,四方相氧化锆能够稳定的存在于常温条件下,当温度升高时,在陶瓷材料的裂纹尖端处,由于拉应力的作用使得四方相氧化锆转变为单斜相,诱导表面产生压缩应力,从而阻止或延缓裂纹的继续扩展,这个相变过程伴随着体积膨胀和剪切应变,形成屏蔽效应,可以有效抑制陶瓷材料表面裂纹的扩展,并且当部分四方相氧化锆颗粒转变为单斜相时,伴随一定程度的体积膨胀,同时在陶瓷材料内部单斜相颗粒的周围会产生部分微裂纹,这样可以在裂纹扩展时,减少裂纹尖端的应力集中来达到增韧效果,提高陶瓷材料强度;陶瓷材料中添加氧化锆晶须,可以有效提高陶瓷材料的强度,当晶须受到外加作用力时,在陶瓷材料内部桥连的晶须会产生一个作用力迫使裂纹闭合,从而达到耗费一些外力所做功的效果,进而增加陶瓷材料的韧性和强度,当裂纹由陶瓷材料表面扩散到晶须时,裂纹的扩散方向就会发生改变,因为晶须和陶瓷材料的解离而导致了裂纹沿着晶须进行扩散,这不仅增大了所形成的新表面的面积,而且还可以使裂纹在其临界尺寸之内,进而加强陶瓷材料的韧性。
具体实施方式
按重量份数计,分别称量5~10份四氯化锆、25~50份无水乙醇,将四氯化锆加入无水乙醇中,置于110~120℃的油浴条件下以120~160r/min转速搅拌回流20~24h,常温冷却,得氧化锆溶胶,将氧化锆溶胶置于马弗炉中,常温下以5℃/min的速率升温至300~400℃,保温10~20min,再以10℃/min的速率升温至800~900℃,保温煅烧40~60min,随炉冷却至室温,得氧化锆干凝胶,研磨,过200目,得氧化锆干凝胶粉末; 再按重量份数计,分别称量20~30份氧化锆干凝胶粉末、20~30份偏钒酸钠、2~3份氟化钠,将氧化锆干凝胶粉末、偏钒酸钠、氟化钠置于搅拌机中,常温下以300~400r/min转速搅拌混合20~30min,得干凝胶混合物,将干凝胶混合物置于微波烧结炉中,常温下以10℃/min的速率升温至400~500℃,保温烧结6~8h,随炉冷却至室温,用去离子水洗涤5~7次,置于80~100℃的烘箱中干燥1~2h,得氧化锆晶须;
再按重量份数计,分别称量20~30份平均粒度40~60nm的氟化钙粉末、30~45份硝酸铝、4~6份聚乙烯吡咯烷酮、120~180份无水乙醇、60~90份去离子水,将氟化钙粉末、聚乙烯吡咯烷酮加入无水乙醇中,常温下以300~400r/min转速搅拌20~30min,再置于超声波分散机中,常温下以300~400W的功率超声分散10~20min,得氟化钙分散液,将硝酸铝加入去离子水中,常温下以160~200r/min转速搅拌10~12min,得硝酸铝溶液,将硝酸铝溶液加入氟化钙分散液,滴加质量分数10%的氨水调节pH至8~9,在40~60℃的水浴条件下以200~250r/min转速搅拌20~30min,常温冷却,过滤,取滤饼,置于60~80℃的烘箱中干燥1~2h,常温冷却,得氢氧化铝包覆氟化钙粉末;
再按重量份数计,分别称量60~80份平均粒径80~100μm的刚玉粉、12~16份氧化锆晶须、18~24份氢氧化铝包覆氟化钙粉末、3~6份平均粒径50~60μm的氧化镁粉末、0.6~0.8份硼酸、200~300份无水乙醇,将刚玉粉、氧化锆晶须、氢氧化铝包覆氟化钙粉末、氧化镁粉末、硼酸加入无水乙醇中,常温下以200~250r/min转速搅拌1~2h,得混合浆料,将混合浆料置于热压烧结炉内,在1200~1400℃、20~40MPa的条件下保温保压烧结2~4h,随炉冷却至室温,得自润滑刀具用高韧性陶瓷材料。
实施例1
按重量份数计,分别称量5份四氯化锆、25份无水乙醇,将四氯化锆加入无水乙醇中,置于110℃的油浴条件下以120r/min转速搅拌回流20h,常温冷却,得氧化锆溶胶,将氧化锆溶胶置于马弗炉中,常温下以5℃/min的速率升温至300℃,保温10min,再以10℃/min的速率升温至800℃,保温煅烧40min,随炉冷却至室温,得氧化锆干凝胶,研磨,过200目,得氧化锆干凝胶粉末; 再按重量份数计,分别称量20份氧化锆干凝胶粉末、20份偏钒酸钠、2份氟化钠,将氧化锆干凝胶粉末、偏钒酸钠、氟化钠置于搅拌机中,常温下以300r/min转速搅拌混合20min,得干凝胶混合物,将干凝胶混合物置于微波烧结炉中,常温下以10℃/min的速率升温至400℃,保温烧结6h,随炉冷却至室温,用去离子水洗涤5次,置于80℃的烘箱中干燥1h,得氧化锆晶须;
再按重量份数计,分别称量20份平均粒度40nm的氟化钙粉末、30份硝酸铝、4份聚乙烯吡咯烷酮、120份无水乙醇、60份去离子水,将氟化钙粉末、聚乙烯吡咯烷酮加入无水乙醇中,常温下以300r/min转速搅拌20min,再置于超声波分散机中,常温下以300W的功率超声分散10min,得氟化钙分散液,将硝酸铝加入去离子水中,常温下以160r/min转速搅拌10min,得硝酸铝溶液,将硝酸铝溶液加入氟化钙分散液,滴加质量分数10%的氨水调节pH至8,在40℃的水浴条件下以200r/min转速搅拌20min,常温冷却,过滤,取滤饼,置于60℃的烘箱中干燥1h,常温冷却,得氢氧化铝包覆氟化钙粉末;
再按重量份数计,分别称量60份平均粒径80μm的刚玉粉、12份氧化锆晶须、18份氢氧化铝包覆氟化钙粉末、3份平均粒径50μm的氧化镁粉末、0.6份硼酸、200份无水乙醇,将刚玉粉、氧化锆晶须、氢氧化铝包覆氟化钙粉末、氧化镁粉末、硼酸加入无水乙醇中,常温下以200r/min转速搅拌1h,得混合浆料,将混合浆料置于热压烧结炉内,在1200℃、20MPa的条件下保温保压烧结2h,随炉冷却至室温,得自润滑刀具用高韧性陶瓷材料。
实施例2
按重量份数计,分别称量7份四氯化锆、36份无水乙醇,将四氯化锆加入无水乙醇中,置于115℃的油浴条件下以140r/min转速搅拌回流22h,常温冷却,得氧化锆溶胶,将氧化锆溶胶置于马弗炉中,常温下以5℃/min的速率升温至350℃,保温15min,再以10℃/min的速率升温至850℃,保温煅烧50min,随炉冷却至室温,得氧化锆干凝胶,研磨,过200目,得氧化锆干凝胶粉末; 再按重量份数计,分别称量25份氧化锆干凝胶粉末、25份偏钒酸钠、2.5份氟化钠,将氧化锆干凝胶粉末、偏钒酸钠、氟化钠置于搅拌机中,常温下以350r/min转速搅拌混合25min,得干凝胶混合物,将干凝胶混合物置于微波烧结炉中,常温下以10℃/min的速率升温至450℃,保温烧结7h,随炉冷却至室温,用去离子水洗涤6次,置于90℃的烘箱中干燥1.5h,得氧化锆晶须;
再按重量份数计,分别称量25份平均粒度50nm的氟化钙粉末、38份硝酸铝、5份聚乙烯吡咯烷酮、150份无水乙醇、75份去离子水,将氟化钙粉末、聚乙烯吡咯烷酮加入无水乙醇中,常温下以350r/min转速搅拌25min,再置于超声波分散机中,常温下以350W的功率超声分散15min,得氟化钙分散液,将硝酸铝加入去离子水中,常温下以180r/min转速搅拌11min,得硝酸铝溶液,将硝酸铝溶液加入氟化钙分散液,滴加质量分数10%的氨水调节pH至8.5,在50℃的水浴条件下以225r/min转速搅拌25min,常温冷却,过滤,取滤饼,置于70℃的烘箱中干燥1.5h,常温冷却,得氢氧化铝包覆氟化钙粉末;
再按重量份数计,分别称量70份平均粒径900μm的刚玉粉、14份氧化锆晶须、21份氢氧化铝包覆氟化钙粉末、4.5份平均粒径54μm的氧化镁粉末、0.7份硼酸、250份无水乙醇,将刚玉粉、氧化锆晶须、氢氧化铝包覆氟化钙粉末、氧化镁粉末、硼酸加入无水乙醇中,常温下以225r/min转速搅拌1.5h,得混合浆料,将混合浆料置于热压烧结炉内,在1300℃、30MPa的条件下保温保压烧结3h,随炉冷却至室温,得自润滑刀具用高韧性陶瓷材料。
实施例3
按重量份数计,分别称量10份四氯化锆50份无水乙醇,将四氯化锆加入无水乙醇中,置于120℃的油浴条件下以160r/min转速搅拌回流24h,常温冷却,得氧化锆溶胶,将氧化锆溶胶置于马弗炉中,常温下以5℃/min的速率升温至400℃,保温20min,再以10℃/min的速率升温至900℃,保温煅烧60min,随炉冷却至室温,得氧化锆干凝胶,研磨,过200目,得氧化锆干凝胶粉末; 再按重量份数计,分别称量30份氧化锆干凝胶粉末、30份偏钒酸钠、3份氟化钠,将氧化锆干凝胶粉末、偏钒酸钠、氟化钠置于搅拌机中,常温下以400r/min转速搅拌混合30min,得干凝胶混合物,将干凝胶混合物置于微波烧结炉中,常温下以10℃/min的速率升温至500℃,保温烧结8h,随炉冷却至室温,用去离子水洗涤7次,置于100℃的烘箱中干燥2h,得氧化锆晶须;
再按重量份数计,分别称量30份平均粒度60nm的氟化钙粉末、45份硝酸铝、6份聚乙烯吡咯烷酮、180份无水乙醇、90份去离子水,将氟化钙粉末、聚乙烯吡咯烷酮加入无水乙醇中,常温下以400r/min转速搅拌30min,再置于超声波分散机中,常温下以400W的功率超声分散20min,得氟化钙分散液,将硝酸铝加入去离子水中,常温下以200r/min转速搅拌12min,得硝酸铝溶液,将硝酸铝溶液加入氟化钙分散液,滴加质量分数10%的氨水调节pH至9,在60℃的水浴条件下以250r/min转速搅拌30min,常温冷却,过滤,取滤饼,置于80℃的烘箱中干燥2h,常温冷却,得氢氧化铝包覆氟化钙粉末;
再按重量份数计,分别称量80份平均粒径100μm的刚玉粉、16份氧化锆晶须、24份氢氧化铝包覆氟化钙粉末、6份平均粒径60μm的氧化镁粉末、0.8份硼酸、300份无水乙醇,将刚玉粉、氧化锆晶须、氢氧化铝包覆氟化钙粉末、氧化镁粉末、硼酸加入无水乙醇中,常温下以250r/min转速搅拌2h,得混合浆料,将混合浆料置于热压烧结炉内,在1400℃、40MPa的条件下保温保压烧结4h,随炉冷却至室温,得自润滑刀具用高韧性陶瓷材料。
Claims (8)
1.一种自润滑刀具用高韧性陶瓷材料的制备方法,其特征在于,具体制备步骤为:
(1)按重量份数计,分别称量60~80份刚玉粉、12~16份氧化锆晶须、18~24份氢氧化铝包覆氟化钙粉末、3~6份氧化镁粉末、0.6~0.8份硼酸、200~300份无水乙醇;
(2)将刚玉粉、氧化锆晶须、氢氧化铝包覆氟化钙粉末、氧化镁粉末、硼酸加入无水乙醇中,常温下以200~250r/min转速搅拌1~2h,得混合浆料;
(3)将混合浆料置于热压烧结炉内,在1200~1400℃、20~40MPa的条件下保温保压烧结2~4h,随炉冷却至室温,得自润滑刀具用高韧性陶瓷材料。
2.根据权利要求1所述的一种自润滑刀具用高韧性陶瓷材料的制备方法,其特征在于,步骤(1)所述的刚玉粉的平均粒径为80~100μm,氧化镁粉末的平均粒径为50~60μm。
3.根据权利要求1所述的一种自润滑刀具用高韧性陶瓷材料的制备方法,其特征在于,步骤(1)所述的氢氧化铝包覆氟化钙粉末的具体制备步骤为:
(1)按重量份数计,分别称量20~30份氟化钙粉末、30~45份硝酸铝、4~6份聚乙烯吡咯烷酮、120~180份无水乙醇、60~90份去离子水;
(2)将氟化钙粉末、聚乙烯吡咯烷酮加入无水乙醇中,常温下以300~400r/min转速搅拌20~30min,再置于超声波分散机中,常温下超声分散10~20min,得氟化钙分散液;
(3)将硝酸铝加入去离子水中,常温下以160~200r/min转速搅拌10~12min,得硝酸铝溶液;
(4)将硝酸铝溶液加入氟化钙分散液,调节pH至8~9,在40~60℃的水浴条件下以200~250r/min转速搅拌20~30min,常温冷却,过滤,取滤饼,置于60~80℃的烘箱中干燥1~2h,常温冷却,得氢氧化铝包覆氟化钙粉末。
4.根据权利要求3所述的一种自润滑刀具用高韧性陶瓷材料的制备方法,其特征在于,步骤(1)所述的氟化钙粉末的平均粒度为40~60nm。
5.根据权利要求3所述的一种自润滑刀具用高韧性陶瓷材料的制备方法,其特征在于,步骤(2)所述的超声分散的功率为300~400W。
6.根据权利要求3所述的一种自润滑刀具用高韧性陶瓷材料的制备方法,其特征在于,步骤(4)所述的pH调节采用的是质量分数10%的氨水。
7.根据权利要求1所述的一种自润滑刀具用高韧性陶瓷材料的制备方法,其特征在于,步骤(1)所述的氧化锆晶须的具体制备步骤为:
(1)按重量份数计,分别称量20~30份氧化锆干凝胶粉末、20~30份偏钒酸钠、2~3份氟化钠;
(2)将氧化锆干凝胶粉末、偏钒酸钠、氟化钠置于搅拌机中,常温下以300~400r/min转速搅拌混合20~30min,得干凝胶混合物;
(3)将干凝胶混合物置于微波烧结炉中,常温下以10℃/min的速率升温至400~500℃,保温烧结6~8h,随炉冷却至室温,用去离子水洗涤5~7次,置于80~100℃的烘箱中干燥1~2h,得氧化锆晶须。
8.根据权利要求7所述的一种自润滑刀具用高韧性陶瓷材料的制备方法,其特征在于,步骤(1)所述的氧化锆干凝胶粉末的具体制备步骤为:
(1)按重量份数计,分别称量5~10份四氯化锆、25~50份无水乙醇;
(2)将四氯化锆加入无水乙醇中,置于110~120℃的油浴条件下以120~160r/min转速搅拌回流20~24h,常温冷却,得氧化锆溶胶;
(3)将氧化锆溶胶置于马弗炉中,常温下以5℃/min的速率升温至300~400℃,保温10~20min,再以10℃/min的速率升温至800~900℃,保温煅烧40~60min,随炉冷却至室温,得氧化锆干凝胶,研磨,过200目,得氧化锆干凝胶粉末。
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CN113087529A (zh) * | 2021-04-06 | 2021-07-09 | 湖南泰鑫瓷业有限公司 | 一种高韧性陶瓷刀具的生产工艺 |
CN115321991A (zh) * | 2021-05-11 | 2022-11-11 | 中国科学院过程工程研究所 | 一种利用铝灰制备自润滑材料的方法 |
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN113087529A (zh) * | 2021-04-06 | 2021-07-09 | 湖南泰鑫瓷业有限公司 | 一种高韧性陶瓷刀具的生产工艺 |
CN113087529B (zh) * | 2021-04-06 | 2021-10-26 | 湖南泰鑫瓷业有限公司 | 一种高韧性陶瓷刀具的生产工艺 |
CN115321991A (zh) * | 2021-05-11 | 2022-11-11 | 中国科学院过程工程研究所 | 一种利用铝灰制备自润滑材料的方法 |
CN115321991B (zh) * | 2021-05-11 | 2023-05-05 | 中国科学院过程工程研究所 | 一种利用铝灰制备自润滑材料的方法 |
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