CN114833733A - 一种金刚石树脂砂轮及其制备方法 - Google Patents
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Abstract
本发明公开了一种金刚石树脂砂轮及其制备方法,先将纳米金属氧化物加入聚酰胺酸溶液中分散均匀,后加入金刚石磨料混合均匀,经过冷冻干燥、热亚胺化,得到聚酰亚胺复合气凝胶包覆金刚石磨料,然后采用硅烷偶联剂对其进行改性,再与无机填料、热固性聚酰亚胺树脂混合均匀,热压成型后,将得到的毛坯加热固化即得。本发明的金刚石树脂砂轮对金刚石磨料的把持能力得到显著提升,从而有效提高了金刚石磨料的利用率,延长了金刚石树脂砂轮的使用寿命,有利于节约磨削加工的成本。
Description
技术领域
本发明涉及金刚石砂轮技术领域,尤其涉及一种金刚石树脂砂轮及其制备方法。
背景技术
金刚石砂轮是以金刚石为磨料,以金属粉、树脂、陶瓷等作为结合剂制成的一种广泛应用于磨削加工领域的磨具。其中,金刚石树脂砂轮所采用的的结合剂为树脂,是将原料经过混合、热压成型、固化等工艺制成,其不仅硬度高、研磨能力强,而且具有生产工艺简单、成本较低的优点,广泛应用于硬质合金、陶瓷、半导体等材料的磨削加工中。
近年来,随着制造业的发展,金刚石树脂砂轮的用量也逐渐增大。因此,对金刚石树脂砂轮的性能,尤其是耐用性提出了更高的要求。影响金刚石树脂砂轮耐用性的因素有很多,其中一个重要的因素就是树脂结合剂对金刚石磨料的把持能力。这是由于在磨削加工过程中,若树脂结合剂对磨料的把持力偏低,会导致磨料过早脱落、破碎,不能充分发挥其磨削作用。为了节约磨削加工的成本,提高金刚石树脂砂轮的使用寿命,有必要进行进一步的探索和研究。
发明内容
本发明目的就是为了弥补已有技术的缺陷,提供一种金刚石树脂砂轮及其制备方法。
本发明是通过以下技术方案实现的:
一种金刚石树脂砂轮的制备方法,包括以下步骤:
(1)将纳米金属氧化物加入聚酰胺酸溶液中分散均匀,然后加入金刚石磨料混合均匀,冷冻干燥后,进行热亚胺化,得到聚酰亚胺复合气凝胶包覆金刚石磨料;
(2)将所述聚酰亚胺复合气凝胶包覆金刚石磨料在硅烷偶联剂水解液中浸渍处理,干燥后得到硅烷改性聚酰亚胺复合气凝胶包覆金刚石磨料;
(3)将所述硅烷改性聚酰亚胺复合气凝胶包覆金刚石磨料与无机填料、热固性聚酰亚胺树脂混合均匀,得到混合料,将所述混合料加入模具中,热压成型,将得到的毛坯加热固化,得到金刚石树脂砂轮。
优选地,步骤(1)中,所述纳米金属氧化物、聚酰胺酸溶液、硅烷改性金刚石磨料的质量比为(0.5-1):(50-100):100。
优选地,步骤(1)中,聚酰胺酸溶液是由二酐单体和二胺单体在有机溶剂中经过溶液聚合反应得到,其固含量为3-5%;所述二酐单体为均苯四甲酸二酐、3,3',4,4'-联苯四甲酸二酐中的至少一种,所述二胺单体为4,4'-二氨基二苯醚,所述有机溶剂为N,N-二甲基甲酰胺、N,N-二甲基乙酰胺、N-甲基吡咯烷酮中的至少一种,所述二酐单体和二胺单体的摩尔比为1:(0.95-1.05)。
优选地,步骤(1)中,纳米金属氧化物为纳米氧化锌、纳米氧化铁、纳米氧化镁中的至少一种。
优选地,步骤(1)中,热亚胺化的过程为:先以2-5℃/min的升温速率升温至100-120℃,保温30-40min,再以2-5℃/min的升温速率升温至200-240℃,保温30-40min,再以以2-5℃/min的升温速率升温至300-320℃,保温60-120min。
优选地,步骤(2)中,聚酰亚胺复合气凝胶包覆金刚石磨料与硅烷偶联剂水解液的质量比为1:(10-50)。
优选地,步骤(2)中,所述硅烷偶联剂水解液是将硅烷偶联剂与无水乙醇、水按质量比为1:(7-9):(1-3)混合得到,所述硅烷偶联剂为硅烷偶联剂KH-550、硅烷偶联剂KH560、硅烷偶联剂KH570中的至少一种。
优选地,步骤(3)中,聚酰亚胺复合气凝胶包覆金刚石磨料与无机填料、热固性聚酰亚胺树脂的质量比为(20-30):(10-15):(55-70);步骤(3)中,无机填料为氧化锌、氧化铬、二硫化钼中的至少一种,优选由氧化锌、氧化铬、二硫化钼按质量比为(5-10):(5-10):(8-15)组成。
优选地,步骤(3)中,热压成型的温度为220-230℃,压力为5-10MPa,时间为30-60min;步骤(3)中,加热固化的温度为200-250℃,时间为10-15h。
一种金刚石树脂砂轮,由所述的制备方法制得。
本发明的优点是:
本发明通过将金刚石磨料与含纳米金属氧化物的聚酰胺酸溶液混合,先冷冻干燥,再经过热亚胺化从而在金刚石磨料表面形成并包覆含纳米金属氧化物骨架的聚酰亚胺气凝胶,该气凝胶与金刚石磨料表面结合牢固,而且具有稳定的多孔结构,采用硅烷对其改性使其与结合树脂的结合力提高,在将其与无机填料、热固性聚酰亚胺树脂混合并热压成型的过程中,结合树脂浸润进入气凝胶的多孔结构并与金刚石磨料表面发生接触,从而提高了金刚石磨料在树脂砂轮中的结合性能以及把持力,从而有效提高了金刚石磨料的利用率,延长了金刚石树脂砂轮的使用寿命,有利于节约磨削加工的成本。
具体实施方式
实施例1
一种金刚石树脂砂轮的制备方法,包括以下步骤:
(1)将纳米氧化锌加入聚酰胺酸溶液中分散均匀,然后加入RVD金刚石磨料混合均匀,冷冻干燥后,先以2℃/min的升温速率升温至100℃,保温30min,再以2℃/min的升温速率升温至200℃,保温30min,再以以2℃/min的升温速率升温至300℃,保温60min,得到聚酰亚胺复合气凝胶包覆金刚石磨料,纳米氧化锌、聚酰胺酸溶液、硅烷改性金刚石磨料的质量比为0.5:50:100,其中聚酰胺酸溶液的制备方法为将4,4'-二氨基二苯醚溶解在N-甲基吡咯烷酮中,然后加入均苯四甲酸二酐搅拌反应,得到固含量为3%的聚酰胺酸溶液,其中均苯四甲酸二酐和4,4'-二氨基二苯醚的摩尔比为1:1;
(2)将所述聚酰亚胺复合气凝胶包覆金刚石磨料在硅烷偶联剂水解液中浸渍处理,干燥后得到硅烷改性聚酰亚胺复合气凝胶包覆金刚石磨料,其中聚酰亚胺复合气凝胶包覆金刚石磨料与硅烷偶联剂水解液的质量比为1:10,硅烷偶联剂水解液是将硅烷偶联剂KH-550与无水乙醇、水按质量比为1:7:1混合得到;
(3)将所述硅烷改性聚酰亚胺复合气凝胶包覆金刚石磨料与无机填料、热固性聚酰亚胺树脂按质量比为20:10:70混合均匀,得到混合料,将所述混合料加入模具中,在温度为220℃、压力为5MPa的条件下热压成型60min,将得到的毛坯在200℃下加热固化15h,得到金刚石树脂砂轮,其中无机填料由氧化锌、氧化铬、二硫化钼按质量比为5:5:8组成。
实施例2
一种金刚石树脂砂轮的制备方法,包括以下步骤:
(1)将纳米氧化锌加入聚酰胺酸溶液中分散均匀,然后加入RVD金刚石磨料混合均匀,冷冻干燥后,先以5℃/min的升温速率升温至120℃,保温40min,再以5℃/min的升温速率升温至240℃,保温40min,再以以5℃/min的升温速率升温至320℃,保温120min,得到聚酰亚胺复合气凝胶包覆金刚石磨料,纳米氧化锌、聚酰胺酸溶液、硅烷改性金刚石磨料的质量比为1:100:100,其中聚酰胺酸溶液的制备方法为将4,4'-二氨基二苯醚溶解在N-甲基吡咯烷酮中,然后加入均苯四甲酸二酐搅拌反应,得到固含量为5%的聚酰胺酸溶液,其中均苯四甲酸二酐和4,4'-二氨基二苯醚的摩尔比为1:1;
(2)将所述聚酰亚胺复合气凝胶包覆金刚石磨料在硅烷偶联剂水解液中浸渍处理,干燥后得到硅烷改性聚酰亚胺复合气凝胶包覆金刚石磨料,其中聚酰亚胺复合气凝胶包覆金刚石磨料与硅烷偶联剂水解液的质量比为1:50,硅烷偶联剂水解液是将硅烷偶联剂KH-550与无水乙醇、水按质量比为1:9:3混合得到;
(3)将所述硅烷改性聚酰亚胺复合气凝胶包覆金刚石磨料与无机填料、热固性聚酰亚胺树脂按质量比为30:15:55混合均匀,得到混合料,将所述混合料加入模具中,在温度为230℃、压力为10MPa的条件下热压成型30min,将得到的毛坯在250℃下加热固化10h,得到金刚石树脂砂轮,其中无机填料由氧化锌、氧化铬、二硫化钼按质量比为10:10:15组成。
实施例3
一种金刚石树脂砂轮的制备方法,包括以下步骤:
(1)将纳米氧化锌加入聚酰胺酸溶液中分散均匀,然后加入RVD金刚石磨料混合均匀,冷冻干燥后,先以3℃/min的升温速率升温至115℃,保温35min,再以3℃/min的升温速率升温至220℃,保温35min,再以以3℃/min的升温速率升温至310℃,保温100min,得到聚酰亚胺复合气凝胶包覆金刚石磨料,纳米氧化锌、聚酰胺酸溶液、硅烷改性金刚石磨料的质量比为0.8:80:100,其中聚酰胺酸溶液的制备方法为将4,4'-二氨基二苯醚溶解在N-甲基吡咯烷酮中,然后加入均苯四甲酸二酐搅拌反应,得到固含量为4%的聚酰胺酸溶液,其中均苯四甲酸二酐和4,4'-二氨基二苯醚的摩尔比为1:1;
(2)将所述聚酰亚胺复合气凝胶包覆金刚石磨料在硅烷偶联剂水解液中浸渍处理,干燥后得到硅烷改性聚酰亚胺复合气凝胶包覆金刚石磨料,其中聚酰亚胺复合气凝胶包覆金刚石磨料与硅烷偶联剂水解液的质量比为1:30,硅烷偶联剂水解液是将硅烷偶联剂KH-550与无水乙醇、水按质量比为1:8:2混合得到;
(3)将所述硅烷改性聚酰亚胺复合气凝胶包覆金刚石磨料与无机填料、热固性聚酰亚胺树脂按质量比为25:12:60混合均匀,得到混合料,将所述混合料加入模具中,在温度为225℃、压力为8MPa的条件下热压成型40min,将得到的毛坯在230℃下加热固化12h,得到金刚石树脂砂轮,其中无机填料由氧化锌、氧化铬、二硫化钼按质量比为8:8:12组成。
对比例1
一种金刚石树脂砂轮的制备方法,包括以下步骤:
(1)将RVD金刚石磨料在硅烷偶联剂水解液中浸渍处理,干燥后得到硅烷改性金刚石磨料,其中金刚石磨料与硅烷偶联剂水解液的质量比为1:30,硅烷偶联剂水解液是将硅烷偶联剂KH-550与无水乙醇、水按质量比为1:8:2混合得到;
(3)将硅烷改性金刚石磨料与无机填料、热固性聚酰亚胺树脂按质量比为25:12:60混合均匀,得到混合料,将混合料加入模具中,在温度为225℃、压力为8MPa的条件下热压成型40min,将得到的毛坯在230℃下加热固化12h,得到金刚石树脂砂轮,其中无机填料由氧化锌、氧化铬、二硫化钼按质量比为8:8:12组成。
试验例
分别对实施例3和对比例1制得的砂轮进行磨削试验:
磨床:FGS818数控平面磨床;
工件:YG8硬质合金,硬度HRC78~82,尺寸104×104×30mm;
磨削液:水基磨削液。
具体实验过程为:将砂轮和YG8工件用丙酮清洗后干燥、称重,然后将砂轮安装在FGS818数控平面磨床上,采用表1中的参数条件对工件开展平面磨削试验。
表1磨削参数
试验完毕后,卸下砂轮和工件,用丙酮清洗后干燥,称重,计算磨削比。磨削比的计算公式为:磨削比=(磨削前工件重量-磨削后工件重量)/(磨削前砂轮重量-磨削后砂轮重量)。测试结果如表2所示。
表2磨削试验结果
实施例3 | 对比例1 | |
磨削比G(g/g) | 123.1 | 77.6 |
由此可见,本发明可以显著提高金刚石树脂砂轮的磨削比,说明本发明的砂轮制备方法可以改善金刚石磨料在树脂砂轮中的结合状态,增加对磨料的把持力,从而有效提高了金刚石磨料的利用率,延长了金刚石树脂砂轮的使用寿命。
Claims (10)
1.一种金刚石树脂砂轮的制备方法,其特征在于,包括以下步骤:
(1)将纳米金属氧化物加入聚酰胺酸溶液中分散均匀,然后加入金刚石磨料混合均匀,冷冻干燥后,进行热亚胺化,得到聚酰亚胺复合气凝胶包覆金刚石磨料;
(2)将所述聚酰亚胺复合气凝胶包覆金刚石磨料在硅烷偶联剂水解液中浸渍处理,干燥后得到硅烷改性聚酰亚胺复合气凝胶包覆金刚石磨料;
(3)将所述硅烷改性聚酰亚胺复合气凝胶包覆金刚石磨料与无机填料、热固性聚酰亚胺树脂混合均匀,得到混合料,将所述混合料加入模具中,热压成型,将得到的毛坯加热固化,得到金刚石树脂砂轮。
2.根据权利要求1所述的金刚石树脂砂轮的制备方法,其特征在于,步骤(1)中,所述纳米金属氧化物、聚酰胺酸溶液、硅烷改性金刚石磨料的质量比为(0.5-1):(50-100):100。
3.根据权利要求1所述的金刚石树脂砂轮的制备方法,其特征在于,步骤(1)中,聚酰胺酸溶液是由二酐单体和二胺单体在有机溶剂中经过溶液聚合反应得到,其固含量为3-5%;所述二酐单体为均苯四甲酸二酐、3,3',4,4'-联苯四甲酸二酐中的至少一种,所述二胺单体为4,4'-二氨基二苯醚,所述有机溶剂为N,N-二甲基甲酰胺、N,N-二甲基乙酰胺、N-甲基吡咯烷酮中的至少一种,所述二酐单体和二胺单体的摩尔比为1:(0.95-1.05)。
4.根据权利要求1所述的金刚石树脂砂轮的制备方法,其特征在于,步骤(1)中,纳米金属氧化物为纳米氧化锌、纳米氧化铁、纳米氧化镁中的至少一种。
5.根据权利要求1所述的金刚石树脂砂轮的制备方法,其特征在于,步骤(1)中,热亚胺化的过程为:先以2-5℃/min的升温速率升温至100-120℃,保温30-40min,再以2-5℃/min的升温速率升温至200-240℃,保温30-40min,再以以2-5℃/min的升温速率升温至300-320℃,保温60-120min。
6.根据权利要求1所述的金刚石树脂砂轮的制备方法,其特征在于,步骤(2)中,聚酰亚胺复合气凝胶包覆金刚石磨料与硅烷偶联剂水解液的质量比为1:(10-50)。
7.根据权利要求1所述的金刚石树脂砂轮的制备方法,其特征在于,步骤(2)中,所述硅烷偶联剂水解液是将硅烷偶联剂与无水乙醇、水按质量比为1:(7-9):(1-3)混合得到,所述硅烷偶联剂为硅烷偶联剂KH-550、硅烷偶联剂KH560、硅烷偶联剂KH570中的至少一种。
8.根据权利要求1所述的金刚石树脂砂轮的制备方法,其特征在于,步骤(3)中,聚酰亚胺复合气凝胶包覆金刚石磨料与无机填料、热固性聚酰亚胺树脂的质量比为(20-30):(10-15):(55-70);步骤(3)中,无机填料为氧化锌、氧化铬、二硫化钼中的至少一种,优选由氧化锌、氧化铬、二硫化钼按质量比为(5-10):(5-10):(8-15)组成。
9.根据权利要求1所述的金刚石树脂砂轮的制备方法,其特征在于,步骤(3)中,热压成型的温度为220-230℃,压力为5-10MPa,时间为30-60min;步骤(3)中,加热固化的温度为200-250℃,时间为10-15h。
10.一种金刚石树脂砂轮,其特征在于,由权利要求1-9任一项所述的制备方法制得。
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