CN105729328A - 一种超硬金刚石砂轮的制备方法 - Google Patents
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Abstract
本发明涉及金刚石砂轮,具体说是一种超硬金刚石砂轮的制备方法;其包括制备二氧化钛溶胶;清洗金刚石颗粒,加热烘干后冷却;然后置于马弗炉炉内进行热处理;将金刚石磨料、氧化硅粉、氧化铝粉、氧化硼粉、氧化钾粉、氧化锂粉和碳酸氢钠粉混合球磨;然后将混合球磨后的物料筛分,再置于模具中冷压成型后进行烘干;然后置于炉内进行烧结,待冷却后卸模,得到金刚石砂轮片。本发明将金刚石浸泡在二氧化钛溶胶中,从而在金刚石颗粒表面涂覆二氧化钛薄膜,大大改善了金刚石的性能,同时采用氧化硅粉、氧化铝粉、氧化硼粉、氧化钾粉和氧化锂粉混合作为结合剂,辅以碳酸氢钠,制备的金刚石砂轮片与同类的工艺相比质量较好,有利于工业化生产。
Description
技术领域
本发明涉及金刚石砂轮,具体说是一种超硬金刚石砂轮的制备方法。
背景技术
近年来,随着科技的进步,人们对生产工具的要求向着高效率、高寿命高、高经济性的方向发展,在很多领域普通材料的工具已经不能满足劳动者日益提高的要求,所以以金刚石为代表的金刚石磨削工具发展迅速,其应用已经渗透到机械加工、汽车制造、航空航天、生物、医疗器具、电子信息、建筑、交通、地质采矿等领域。
目前,绝大部分人工合成的金刚石都为粉末状或细小的颗粒状,为了利用金刚石进行高精度,高效率磨削加工,通常采用结合剂将金刚石磨粒粘结起来并制成具有一定强度和形状的模具,以便于安装在各种磨床上进行磨削加工。与其他磨料如刚玉、碳化硅相比,用金刚石模具进行磨削时,其具有磨削效率高、使用寿命长、磨削力小,磨削温度低、磨削精度高等优点。但,现有的以金属材料为结合剂制备金刚石砂轮磨料的硬度不够强,不能适合高硬度材料的磨削。
发明内容
针对上述技术问题,本发明提供一种超硬金刚石砂轮的制备方法。
本发明采用的技术方案为:一种超硬金刚石砂轮的制备方法,其包括以下步骤:
(1)制备二氧化钛溶胶;
(2)清洗金刚石颗粒;
(3)将清洗后的金刚石颗粒浸泡于上述二氧化钛溶胶中,静置后捞出,并加热烘干后冷却;
(4)然后置于马弗炉炉内进行热处理,得到表面涂覆有二氧化钛薄膜的金刚石磨料;
(5)将上述金刚石磨料、氧化硅粉、氧化铝粉、氧化硼粉、氧化钾粉、氧化锂粉和碳酸氢钠粉混合球磨;
(6)然后将混合球磨后的物料筛分,得到混合料;再将混合料置于模具中冷压成型后进行烘干;
(7)然后置于炉内进行烧结,待冷却后卸模,得到金刚石砂轮片。
作为优选,在搅拌下将钛酸丁酯溶于无水乙醇中,接着加入二乙醇胺,待溶液混合均匀后,再滴加乙醇水溶液,继续搅拌,然后室温陈化,得到二氧化钛溶胶。
作为优选,所述二氧化钛溶胶中钛酸丁酯、水、二乙醇胺、乙醇的物质的量之比为1:1:1:(25—28)。
作为优选,清洗金刚石颗粒时,将金刚石颗粒先用盐酸溶液浸泡,再用去离子水冲洗并烘干,然后用丙酮超声清洗,接着用去离子水冲洗后干燥。
作为优选,金刚石颗粒用盐酸溶液浸泡后用去离子水冲洗至冲洗液的pH值为7。
作为优选,金刚石颗粒浸泡于二氧化钛溶胶中静置捞出后,再置于70—90℃的烘箱中干燥4—6min,然后冷却;并重复上述步骤3—5次。
作为优选,热处理时,先将马弗炉升温至90—100℃后保温20—30min,然后以4—7℃/min的升温速率升温至600—800℃,并保温50—60min后随炉冷却。
作为优选,混合料中金刚石磨料占70—80wt%,氧化硅粉占14—17wt%、氧化铝粉占2—3wt%、氧化硼粉占1—2wt%、氧化钾粉占1—2wt%、氧化锂粉占1—3wt%,碳酸氢钠粉占1—3wt%。
作为优选,所述模具采用石墨模具;冷压成型后以80℃的温度烘干5—10min。
作为优选,烧结在真空下进行;烧结时先以4—7℃/min的升温速率升温至950—1100℃,然后保温30—50min,最后随炉冷却。
从以上技术方案可知,本发明将金刚石浸泡在二氧化钛溶胶中,从而在金刚石颗粒表面涂覆二氧化钛薄膜,大大改善了金刚石的性能,提高了其强度,可以作为超硬金刚石砂轮的磨料,适合磨削超硬材料;同时采用氧化硅粉、氧化铝粉、氧化硼粉、氧化钾粉和氧化锂粉混合作为结合剂,辅以碳酸氢钠,并在真空条件制备金刚石砂轮片,其工艺流程较短,设备成本低,且制备的金刚石砂轮片与同类的工艺相比质量较好,有利于工业化生产。
具体实施方式
下面将详细说明本发明,在此本发明的示意性实施例以及说明用来解释本发明,但并不作为对本发明的限定。
超硬金刚石砂轮的制备方法,其包括以下步骤:
(1)制备二氧化钛溶胶;制备二氧化钛溶胶时,先在搅拌下将钛酸丁酯溶于无水乙醇中,接着加入二乙醇胺,待溶液混合均匀后,再滴加乙醇水溶液,继续搅拌,然后室温陈化,得到二氧化钛溶胶;在二氧化钛溶胶中钛酸丁酯、水、二乙醇胺、乙醇的物质的量之比为1:1:1:(25—28)。本发明采用钛酸丁酯为有机前驱体,以乙醇为有机溶剂,通过醇解、水解和缩聚反应制得二氧化钛溶胶。
(2)清洗金刚石颗粒;清洗金刚石颗粒时,将金刚石颗粒先用盐酸溶液浸泡,再用去离子水冲洗至冲洗液的pH值为7,并烘干,然后用丙酮超声清洗,接着用去离子水冲洗后干燥,可避免涂膜时引入杂质,降低金刚石的性能。
(3)将清洗后的金刚石颗粒浸泡于上述二氧化钛溶胶中,静置后捞出,并加热烘干后冷却;金刚石颗粒浸泡于二氧化钛溶胶中静置捞出后,再置于70—90℃的烘箱中干燥4—6min,然后冷却;并重复上述步骤3—5次,使得涂膜的质量更好,涂层均匀。金刚石浸泡在溶胶后,其表面会形成一层二氧化钛溶胶薄膜,溶胶薄膜在后继的干燥和热处理过程中会在金刚石表面产生进一步缩聚,形成三维网络结构的二氧化钛凝胶薄膜。由于溶胶凝胶成膜的厚度较薄,因此需要3—5次成膜,提高金刚石磨料的性能。
(4)然后置于马弗炉炉内进行热处理,得到表面涂覆有二氧化钛薄膜的金刚石磨料;热处理时,先将马弗炉升温至90—100℃后保温20—30min,然后以4—7℃/min的升温速率升温至600—800℃,并保温50—60min后随炉冷却。经过热处理后,薄膜致密度较高,附着力较强。
(5)将氧化硅粉、氧化铝粉、氧化硼粉、氧化钾粉、氧化锂粉和碳酸氢钠粉混合球磨,使物料混合均匀,且达到符合要求的粒度;本发明中氧化硅粉、氧化铝粉、氧化硼粉、氧化钾粉、氧化锂粉混合作为结合剂,其中氧化钾和氧化锂有利于抑制结合剂中析出方石英晶体,获得均匀的玻璃相结合剂,从而改善砂轮性能;碳酸氢钠在加工工程中由于加热而发生分解,产生二氧化碳气体,该气体在砂轮内部无法逸出,形成气孔,气孔可容纳磨削过程中产生的碎屑,从而提高磨削效率。
(6)物料混合球磨后,采用300目筛子进行分筛,去除较大的颗粒,保证制备砂轮的质量,在混合料中应保证金刚石磨料占70—80wt%,青铜粉占15—25wt%,碳化硅粉占3—8wt%,碳酸氢钠粉占1—3wt%,这样才能制备较高质量的砂轮片。得到混合料后,将其置于石墨模具中进行冷压成型,然后以80℃的温度烘干5—10min,保证混合料的质量成分;同时,由于石墨线膨胀系数小,耐热冲击性好,在高温下模具的几何尺寸稳定,易获得较高精度的成型制品;且石墨是一种非金属导电材料,具有低的摩擦系数,具有自润滑效果,易于脱模。
(7)物料装模烘干以后,置于炉内进行真空烧结,烧结时先以4—7℃/min的升温速率升温至950—1100℃,然后保温30—50min,再随炉冷却;待冷却后卸模,得到金刚石砂轮片。
实施例1
先在搅拌下将钛酸丁酯溶于无水乙醇中,接着加入二乙醇胺,待溶液混合均匀后,再滴加乙醇水溶液,继续搅拌,然后室温陈化1h,得到二氧化钛溶胶,其中钛酸丁酯、水、二乙醇胺、乙醇的物质的量之比为1:1:1:25;同时将金刚石颗粒先用盐酸溶液浸泡,再用去离子水冲洗至冲洗液的pH值为7,并烘干,然后用丙酮超声清洗,接着用去离子水冲洗后干燥,接着将清洗后的金刚石颗粒浸泡于上述二氧化钛溶胶中,静置后捞出,再置于70℃的烘箱中干燥6min,然后冷却;并重复上述步骤3次;然后置于马弗炉炉内,并将马弗炉升温至90℃后保温30min,然后以4℃/min的升温速率升温至600℃,并保温60min后随炉冷却,接着将金刚石磨料、氧化硅粉、氧化铝粉、氧化硼粉、氧化钾粉、氧化锂粉和碳酸氢钠粉混合球磨,再采用300目筛子进行分筛,保证分筛的混合料中金刚石磨料占70wt%,氧化硅粉占17wt%、氧化铝粉占3wt%、氧化硼粉占2wt%、氧化钾粉占2wt%、氧化锂粉占3wt%,碳酸氢钠粉占3wt%;再将混合料置于石墨模具中以80℃的温度烘干5min,然后置于炉内进行真空烧结,烧结时先以4℃/min的升温速率升温至1100℃,然后保温30min,再随炉冷却;待冷却后卸模,得到高精密切割金刚石砂轮片。测试该砂轮片得到:抗弯强度为72.6MPa,硬度为56HV;在nw=1000rpm、ns=150rpm、Vf=0.002mm/min、纯水磨削液的条件下,磨削比为48。
实施例2
先在搅拌下将钛酸丁酯溶于无水乙醇中,接着加入二乙醇胺,待溶液混合均匀后,再滴加乙醇水溶液,继续搅拌,然后室温陈化1h,得到二氧化钛溶胶,其中钛酸丁酯、水、二乙醇胺、乙醇的物质的量之比为1:1:1:26.5;同时将金刚石颗粒先用盐酸溶液浸泡,再用去离子水冲洗至冲洗液的pH值为7,并烘干,然后用丙酮超声清洗,接着用去离子水冲洗后干燥,接着将清洗后的金刚石颗粒浸泡于上述二氧化钛溶胶中,静置后捞出,再置于80℃的烘箱中干燥5min,然后冷却;并重复上述步骤4次;然后置于马弗炉炉内,并将马弗炉升温至95℃后保温25min,然后以5℃/min的升温速率升温至700℃,并保温55min后随炉冷却;接着将金刚石磨料、氧化硅粉、氧化铝粉、氧化硼粉、氧化钾粉、氧化锂粉和碳酸氢钠粉混合球磨,再采用300目筛子进行分筛,保证分筛的混合料中金刚石磨料占75wt%,氧化硅粉占15.5wt%、氧化铝粉占2.5wt%、氧化硼粉占1.5wt%、氧化钾粉占1.5wt%、氧化锂粉占2wt%,碳酸氢钠粉占2wt%;再将混合料置于石墨模具中以80℃的温度烘干8min,然后置于炉内进行真空烧结,烧结时先以5℃/min的升温速率升温至1100℃,然后保温40min,再随炉冷却;待冷却后卸模,得到高精密切割金刚石砂轮片。测试该砂轮片得到:抗弯强度为89.5MPa,硬度为77HV;在nw=1000rpm、ns=150rpm、Vf=0.002mm/min、纯水磨削液的条件下,磨削比为59。
实施例3
先在搅拌下将钛酸丁酯溶于无水乙醇中,接着加入二乙醇胺,待溶液混合均匀后,再滴加乙醇水溶液,继续搅拌,然后室温陈化1h,得到二氧化钛溶胶,其中钛酸丁酯、水、二乙醇胺、乙醇的物质的量之比为1:1:1:28;同时将金刚石颗粒先用盐酸溶液浸泡,再用去离子水冲洗至冲洗液的pH值为7,并烘干,然后用丙酮超声清洗,接着用去离子水冲洗后干燥,接着将清洗后的金刚石颗粒浸泡于上述二氧化钛溶胶中,静置后捞出,再置于90℃的烘箱中干燥4min,然后冷却;并重复上述步骤5次;然后置于马弗炉炉内,并将马弗炉升温至100℃后保温20min,然后以7℃/min的升温速率升温至800℃,并保温50min后随炉冷却;接着将金刚石磨料、氧化硅粉、氧化铝粉、氧化硼粉、氧化钾粉、氧化锂粉和碳酸氢钠粉混合球磨,再采用300目筛子进行分筛,保证分筛的混合料中金刚石磨料占80wt%,氧化硅粉占14wt%、氧化铝粉占2wt%、氧化硼粉占1wt%、氧化钾粉占1wt%、氧化锂粉占1wt%,碳酸氢钠粉占1wt%;再将混合料置于石墨模具中以80℃的温度烘干10min,然后置于炉内进行真空烧结,烧结时先以7℃/min的升温速率升温至1000℃,然后保温50min,再随炉冷却;待冷却后卸模,得到高精密切割金刚石砂轮片。测试该砂轮片得到:抗弯强度为72.6MPa,硬度为62HV;在nw=1000rpm、ns=150rpm、Vf=0.002mm/min、纯水磨削液的条件下,磨削比为53。
以上对本发明实施例所提供的技术方案进行了详细介绍,本文中应用了具体个例对本发明实施例的原理以及实施方式进行了阐述,以上实施例的说明只适用于帮助理解本发明实施例的原理;同时,对于本领域的一般技术人员,依据本发明实施例,在具体实施方式以及应用范围上均会有改变之处,综上所述,本说明书内容不应理解为对本发明的限制。
Claims (10)
1.一种超硬金刚石砂轮的制备方法,其包括以下步骤:
(1)制备二氧化钛溶胶;
(2)清洗金刚石颗粒;
(3)将清洗后的金刚石颗粒浸泡于上述二氧化钛溶胶中,静置后捞出,并加热烘干后冷却;
(4)然后置于马弗炉炉内进行热处理,得到表面涂覆有二氧化钛薄膜的金刚石磨料;
(5)将上述金刚石磨料、氧化硅粉、氧化铝粉、氧化硼粉、氧化钾粉、氧化锂粉和碳酸氢钠粉混合球磨;
(6)然后将混合球磨后的物料筛分,得到混合料;再将混合料置于模具中冷压成型后进行烘干;
(7)然后置于炉内进行烧结,待冷却后卸模,得到金刚石砂轮片。
2.根据权利要求1所述超硬金刚石砂轮的制备方法,其特征在于:在搅拌下将钛酸丁酯溶于无水乙醇中,接着加入二乙醇胺,待溶液混合均匀后,再滴加乙醇水溶液,继续搅拌,然后室温陈化,得到二氧化钛溶胶。
3.如权利要求1所述超硬金刚石砂轮的制备方法,其特征在于:所述二氧化钛溶胶中钛酸丁酯、水、二乙醇胺、乙醇的物质的量之比为1:1:1:(25—28)。
4.如权利要求1或2或3所述超硬金刚石砂轮的制备方法,其特征在于:清洗金刚石颗粒时,将金刚石颗粒先用盐酸溶液浸泡,再用去离子水冲洗并烘干,然后用丙酮超声清洗,接着用去离子水冲洗后干燥。
5.如权利要求4所述超硬金刚石砂轮的制备方法,其特征在于:金刚石颗粒用盐酸溶液浸泡后用去离子水冲洗至冲洗液的pH值为7。
6.如权利要求1所述超硬金刚石砂轮的制备方法,其特征在于:金刚石颗粒浸泡于二氧化钛溶胶中静置捞出后,再置于70—90℃的烘箱中干燥4—6min,然后冷却;并重复上述步骤3—5次。
7.如权利要求1所述超硬金刚石砂轮的制备方法,其特征在于:热处理时,先将马弗炉升温至90—100℃后保温20—30min,然后以4—7℃/min的升温速率升温至600—800℃,并保温50—60min后随炉冷却。
8.如权利要求1所述超硬金刚石砂轮的制备方法,其特征在于:混合料中金刚石磨料占70—80wt%,氧化硅粉占14—17wt%、氧化铝粉占2—3wt%、氧化硼粉占1—2wt%、氧化钾粉占1—2wt%、氧化锂粉占1—3wt%,碳酸氢钠粉占1—3wt%。
9.如权利要求1所述超硬金刚石砂轮的制备方法,其特征在于:所述模具采用石墨模具;冷压成型后以80℃的温度烘干5—10min。
10.如权利要求1所述超硬金刚石砂轮的制备方法,其特征在于:烧结在真空下进行;烧结时先以4—7℃/min的升温速率升温至950—1100℃,然后保温30—50min,最后随炉冷却。
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