CN113737162A - 一种Ni-P金刚石化学复合镀层的制备方法 - Google Patents
一种Ni-P金刚石化学复合镀层的制备方法 Download PDFInfo
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- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 claims description 20
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 20
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- WXHLLJAMBQLULT-UHFFFAOYSA-N 2-[[6-[4-(2-hydroxyethyl)piperazin-1-yl]-2-methylpyrimidin-4-yl]amino]-n-(2-methyl-6-sulfanylphenyl)-1,3-thiazole-5-carboxamide;hydrate Chemical compound O.C=1C(N2CCN(CCO)CC2)=NC(C)=NC=1NC(S1)=NC=C1C(=O)NC1=C(C)C=CC=C1S WXHLLJAMBQLULT-UHFFFAOYSA-N 0.000 claims description 3
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Abstract
本发明提供一种Ni‑P金刚石化学复合镀层的制备方法,涉及化学复合镀层技术领域,所述Ni‑P金刚石化学复合镀层的制备材料由硫酸镍、次亚磷酸钠、柠檬酸钠、络合剂和金刚石微粒构成。本发明,通过对镀件进行表面喷砂处理,提高镀件表面性能,使镀层能够更加牢固的镀覆在镀件表面,然后对镀件进行清洗处理,处理完成后,使用硫酸对镀件表面进行活性处理,然后对镀件进行预镀处理,使镀件表面形成预镀层,然后将镀件放入含有金刚石微粒的镀液内,使预镀层表面形成一层含有金刚石微粒的镀层,且金刚石微粒的直径大于外侧镀层的厚度,以便镀层在初始阶段就能够达到较好的耐磨效果,以便镀件能够具有较好的使用效果。
Description
技术领域
本发明涉及化学复合镀层技术领域,尤其涉及一种Ni-P金刚石化学复合镀层的制备方法。
背景技术
化学镀镍层有着优良的耐蚀性,但其耐磨性较差,但化学镀镍层可以通过依靠加入高硬度、高耐磨性的硬质粒子,使之与镍一起沉积所得到的复合镀层,从而提高了镀镍层的耐磨性,同时保持了镀镍层的耐蚀性,而Ni-P金刚石化学复合镀层就是通过向镀镍层加入金刚石微粒,使其形成高耐磨的化学复合镀层。
现有的Ni-P金刚石化学复合镀层在镀覆制备过程中,多大是直接将工件放入含有金刚石微粒的化学镀液内进行镀覆,这种方式在镀覆较厚的镀层时,金刚石容易被包覆在镍镀层内部,难以使镀层在初期达到较好的耐磨效果,需要使用一段时间才能具有较好的耐磨性,难以达到较好的使用效果。
发明内容
本发明的目的是为了解决现有技术中存在的缺点,而提出的一种Ni-P金刚石化学复合镀层的制备方法。
为了实现上述目的,本发明采用了如下技术方案:一种Ni-P金刚石化学复合镀层,所述Ni-P金刚石化学复合镀层的制备材料由硫酸镍、次亚磷酸钠、柠檬酸钠络合剂和金刚石微粒构成,且各材料的含量如下:硫酸镍25-40g/L,次亚磷酸钠15-18g/L,柠檬酸钠40-45g/L,络合剂0.8-1.5g/L,金刚石微粒4-10g/L。
为了利于镀层的进行,本发明的改进有,所述络合剂包括但不限于铬酸钾、乙酰丙酮、柠檬酸、酒石酸、草酸和磺基水杨酸。
为了制备金刚石微粒,本发明的改进有,所述金刚石微粒由采用爆轰合成,直径为12-18μm。
为了适用于不同的镀件,本发明的改进有,各材料的含量如下:硫酸镍30g/L,次亚磷酸钠15g/L,柠檬酸钠40g/L,络合剂1g/L,金刚石微粒5g/L。
为了适用于不同的镀件,本发明的改进有,各材料的含量如下:硫酸镍35g/L,次亚磷酸钠16g/L,柠檬酸钠42g/L,络合剂1.2g/L,金刚石微粒8g/L。
为了适用于不同的镀件,本发明的改进有,各材料的含量如下:硫酸镍40g/L,次亚磷酸钠18g/L,柠檬酸钠45g/L,络合剂1.4g/L,金刚石微粒10g/L。
一种Ni-P金刚石化学复合镀层的制备方法,包括以下步骤:
S1:对镀件进行喷砂处理,处理时间10-20分钟,去除镀件表面的杂质,使镀件表面粗化;
S2:将S1中处喷砂处理完的镀件放入浓度为10%的洗衣粉水溶液内进行超声波清洗,清洗时间为5-8分钟,然后将镀件取出使用自来水进行冲洗,冲洗完洗衣粉水溶液后,将镀件自然晾干备用;
S3:将S2中晾干的镀件放入浓度为5%的硫酸溶液中,浸泡4-6分钟,进行表面活性处理;
S4:然后制备初始化学镀液,使初始化学镀液的成分为硫酸镍25-40g/L,次亚磷酸钠15-18g/L,柠檬酸钠40-45g/L,络合剂0.8-1.5g/L,通过添加调节剂,将初始镀液的PH值调为4.4-4.8,然后取部分初始化学镀液,将S3中表面活性处理后的镀件放入初始化学镀液内进行预镀,镀覆温度为75-90℃,镀覆时间为2-2.5小时,镀层厚度为6-8μm;
S5:取S4中制备的初始化学镀液,往初始化学镀液内添加金刚石微粒,使金刚石微粒的含量为4-10g/L,形成金刚石镀液,通过添加调节剂,将金刚石镀液的PH值调节为4.4-4.8,然后将预镀后的镀件,放入金刚石镀液内进行镀覆,镀覆温度为75-90℃,镀覆时间为3-4小时,镀层厚度为10-12μm;
S6:将S5中镀覆完成的镀件取出,通过自来水进行冲洗,冲洗完成后,对镀件进行热处理,处理温度为170-190℃,处理时间为1.5-2.5小时,即可完成整个镀膜过程。
为了便于调节镀液的PH值,本发明的改进有,所述步骤S5中调节剂包括但不限于醋酸、醋酸钠和氢氧化钠。
为了防止金刚石微粒沉淀,本发明的改进有,所述步骤S5中,镀覆过程中需要每隔30分钟搅拌一次金刚石镀液。
与现有技术相比,本发明的优点和积极效果在于,
本发明中,通过对镀件进行表面喷砂处理,提高镀件表面性能,使镀层能够更加牢固的镀覆在镀件表面,然后对镀件进行清洗处理,处理完成后,使用硫酸对镀件表面进行活性处理,然后对镀件进行预镀处理,使镀件表面形成预镀层,然后将镀件放入含有金刚石微粒的镀液内,使预镀层表面形成一层含有金刚石微粒的镀层,且金刚石微粒的直径大于外侧镀层的厚度,以便镀层在初始阶段就能够达到较好的耐磨效果,以便镀件能够具有较好的使用效果。
附图说明
图1为本发明提出一种Ni-P金刚石化学复合镀层的制备方法的流程图。
具体实施方式
为了能够更清楚地理解本发明的上述目的、特征和优点,下面结合附图和实施例对本发明做进一步说明。需要说明的是,在不冲突的情况下,本申请的实施例及实施例中的特征可以相互组合。
在下面的描述中阐述了很多具体细节以便于充分理解本发明,但是,本发明还可以采用不同于在此描述的其他方式来实施,因此,本发明并不限于下面公开说明书的具体实施例的限制。
请参阅图1,本发明提供一种Ni-P金刚石化学复合镀层,Ni-P金刚石化学复合镀层的制备材料由硫酸镍、次亚磷酸钠、柠檬酸钠、络合剂和金刚石微粒构成,且各材料的含量如下:硫酸镍25-40g/L,次亚磷酸钠15-18g/L,柠檬酸钠40-45g/L,络合剂0.8-1.5g/L,金刚石微粒4-10g/L,化学镀(Electroless plating)也称无电解镀或者自催化镀(Auto-catalytic plating),是在无外加电流的情况下借助合适的还原剂,使镀液中金属离子还原成金属,并沉积到零件表面的一种镀覆方法,化学镀技术是在金属的催化作用下,通过可控制的氧化还原反应产生金属的沉积过程。与电镀相比,化学镀技术具有镀层均匀、针孔小、不需直流电源设备、能在非导体上沉积和具有某些特殊性能等特点。另外,由于化学镀技术废液排放少,对环境污染小以及成本较低,在许多领域已逐步取代电镀,成为一种环保型的表面处理工艺。目前,化学镀技术已在电子、阀门制造、机械、石油化工、汽车、航空航天等工业中得到广泛的应用。
具体的,络合剂包括但不限于铬酸钾、乙酰丙酮、柠檬酸、酒石酸、草酸和磺基水杨酸,络合剂能与金属离子形成络合离子的化合物,镀镍的溶液中除了主盐与还原剂以外,最重要的组成部分就是络合剂,在此也起了加速剂的作用,络合剂能够防止镀液析出沉淀,增加镀液稳定性并延长使用寿命,镀镍的络合剂能在镍吸附在镀件表面后,提高了它的活性,从而增加镀层反应速度。
具体的,金刚石微粒由采用爆轰合成,直径为12-18μm,金刚石微粒又称金刚石微粉,是指颗粒度细于36/54微米的金刚石颗粒,有单晶金刚石微粉和聚晶金刚石微粉。单晶金刚石微粉是由人造金刚石单晶磨粒,经过粉碎、整形处理,采用特殊的工艺方法生产。金刚石微粉硬度高、耐磨性好,可广泛用于切削、磨削、钻探等。是研磨抛光硬质合金、陶瓷、宝石、光学玻璃等高硬度材料的理想原料。金刚石微粉制品是利用金刚石微粉加工制成的工具和构件,金刚石微粉是人造金刚石单晶经过特殊工艺处理加工而形成的一种新型超硬超细磨料,是研磨抛光硬质合金、陶瓷、宝石、光学玻璃等高硬度材料的理想原料,金刚石制品是利用金刚石材料加工制成的工具和构件,应用十分广泛。金刚石微粉及制品广泛应用于汽车、机械、电子、航空、航天、光学仪器、玻璃、陶瓷、石油、地质等部门,随着技术和产品的不断发展,金刚石微粉及制品的利用领域还在不断拓宽。
实施例一
各材料的含量如下:硫酸镍30g/L,次亚磷酸钠15g/L,柠檬酸钠40g/L,络合剂1g/L,金刚石微粒5g/L。
Ni-P金刚石化学复合镀层的制备方法包括以下步骤:
S1:对镀件进行喷砂处理,处理时间12分钟,去除镀件表面的杂质,使镀件表面粗化;
S2:将S1中处喷砂处理完的镀件放入浓度为10%的洗衣粉水溶液内进行超声波清洗,清洗时间为5分钟,然后将镀件取出使用自来水进行冲洗,冲洗完洗衣粉水溶液后,将镀件自然晾干备用;
S3:将S2中晾干的镀件放入浓度为5%的硫酸溶液中,浸泡5分钟,进行表面活性处理;
S4:然后制备初始化学镀液,使初始化学镀液的成分为硫酸镍30g/L,次亚磷酸钠15g/L,柠檬酸钠40g/L,络合剂1g/L,通过添加调节剂,将初始镀液的PH值调为4.4-4.8,然后取部分初始化学镀液,将S3中表面活性处理后的镀件放入初始化学镀液内进行预镀,镀覆温度为80℃,镀覆时间为2小时,镀层厚度为6μm;
S5:取S4中制备的初始化学镀液,往初始化学镀液内添加金刚石微粒,使金刚石微粒的含量为5g/L,形成金刚石镀液,通过添加调节剂,将金刚石镀液的PH值调节为4.4-4.8,然后将预镀后的镀件,放入金刚石镀液内进行镀覆,镀覆温度为80℃,镀覆时间为3小时,镀层厚度为10μm;
S6:将S5中镀覆完成的镀件取出,通过自来水进行冲洗,冲洗完成后,对镀件进行热处理,处理温度为180℃,处理时间为2小时,即可完成整个镀膜过程。
具体的,步骤S5中调节剂包括但不限于醋酸、醋酸钠和氢氧化钠,能够对镀液的PH值进行调节,使镀覆反应能够更加快速的进行。
具体的,步骤S5中,镀覆过程中需要每隔30分钟搅拌一次金刚石镀液,防止金刚石微粒沉淀,使镀件能够得到更好的镀覆效果。
实施例二
各材料的含量如下:硫酸镍35g/L,次亚磷酸钠16g/L,柠檬酸钠42g/L,络合剂1.2g/L,金刚石微粒8g/L。
Ni-P金刚石化学复合镀层的制备方法包括以下步骤:
S1:对镀件进行喷砂处理,处理时间14分钟,去除镀件表面的杂质,使镀件表面粗化;
S2:将S1中处喷砂处理完的镀件放入浓度为10%的洗衣粉水溶液内进行超声波清洗,清洗时间为6分钟,然后将镀件取出使用自来水进行冲洗,冲洗完洗衣粉水溶液后,将镀件自然晾干备用;
S3:将S2中晾干的镀件放入浓度为5%的硫酸溶液中,浸泡5分钟,进行表面活性处理;
S4:然后制备初始化学镀液,使初始化学镀液的成分为硫酸镍35g/L,次亚磷酸钠16g/L,柠檬酸钠42g/L,络合剂1.2g/L,通过添加调节剂,将初始镀液的PH值调为4.4-4.8,然后取部分初始化学镀液,将S3中表面活性处理后的镀件放入初始化学镀液内进行预镀,镀覆温度为80℃,镀覆时间为2小时,镀层厚度为7μm;
S5:取S4中制备的初始化学镀液,往初始化学镀液内添加金刚石微粒,使金刚石微粒的含量为8g/L,形成金刚石镀液,通过添加调节剂,将金刚石镀液的PH值调节为4.4-4.8,然后将预镀后的镀件,放入金刚石镀液内进行镀覆,镀覆温度为80℃,镀覆时间为3小时,镀层厚度为11μm;
S6:将S5中镀覆完成的镀件取出,通过自来水进行冲洗,冲洗完成后,对镀件进行热处理,处理温度为180℃,处理时间为2小时,即可完成整个镀膜过程。
具体的,步骤S5中调节剂包括但不限于醋酸、醋酸钠和氢氧化钠,能够对镀液的PH值进行调节,使镀覆反应能够更加快速的进行。
具体的,步骤S5中,镀覆过程中需要每隔30分钟搅拌一次金刚石镀液,防止金刚石微粒沉淀,使镀件能够得到更好的镀覆效果。
实施例三
硫酸镍40g/L,次亚磷酸钠18g/L,柠檬酸钠45g/L,络合剂1.4g/L,金刚石微粒10g/L。
Ni-P金刚石化学复合镀层的制备方法包括以下步骤:
S1:对镀件进行喷砂处理,处理时间14分钟,去除镀件表面的杂质,使镀件表面粗化;
S2:将S1中处喷砂处理完的镀件放入浓度为10%的洗衣粉水溶液内进行超声波清洗,清洗时间为8分钟,然后将镀件取出使用自来水进行冲洗,冲洗完洗衣粉水溶液后,将镀件自然晾干备用;
S3:将S2中晾干的镀件放入浓度为5%的硫酸溶液中,浸泡6分钟,进行表面活性处理;
S4:然后制备初始化学镀液,使初始化学镀液的成分为硫酸镍40g/L,次亚磷酸钠18g/L,柠檬酸钠45g/L,络合剂1.4g/L,通过添加调节剂,将初始镀液的PH值调为4.4-4.8,然后取部分初始化学镀液,将S3中表面活性处理后的镀件放入初始化学镀液内进行预镀,镀覆温度为85℃,镀覆时间为2.5小时,镀层厚度为8μm;
S5:取S4中制备的初始化学镀液,往初始化学镀液内添加金刚石微粒,使金刚石微粒的含量为10g/L,形成金刚石镀液,通过添加调节剂,将金刚石镀液的PH值调节为4.4-4.8,然后将预镀后的镀件,放入金刚石镀液内进行镀覆,镀覆温度为85℃,镀覆时间为3.5小时,镀层厚度为12μm;
S6:将S5中镀覆完成的镀件取出,通过自来水进行冲洗,冲洗完成后,对镀件进行热处理,处理温度为190℃,处理时间为2.5小时,即可完成整个镀膜过程。
具体的,步骤S5中调节剂包括但不限于醋酸、醋酸钠和氢氧化钠,能够对镀液的PH值进行调节,使镀覆反应能够更加快速的进行。
具体的,步骤S5中,镀覆过程中需要每隔30分钟搅拌一次金刚石镀液,防止金刚石微粒沉淀,使镀件能够得到更好的镀覆效果。
本发明中,通过对镀件进行表面喷砂处理,提高镀件表面性能,使镀层能够更加牢固的镀覆在镀件表面,然后对镀件进行清洗处理,处理完成后,使用硫酸对镀件表面进行活性处理,然后对镀件进行预镀处理,使镀件表面形成预镀层,然后将镀件放入含有金刚石微粒的镀液内,使预镀层表面形成一层含有金刚石微粒的镀层,且金刚石微粒的直径大于外侧镀层的厚度,以便镀层在初始阶段就能够达到较好的耐磨效果,以便镀件能够具有较好的使用效果。
以上,仅是本发明的较佳实施例而已,并非是对本发明作其它形式的限制,任何熟悉本专业的技术人员可能利用上述揭示的技术内容加以变更或改型为等同变化的等效实施例应用于其它领域,但是凡是未脱离本发明技术方案内容,依据本发明的技术实质对以上实施例所作的任何简单修改、等同变化与改型,仍属于本发明技术方案的保护范围。
Claims (9)
1.一种Ni-P金刚石化学复合镀层,其特征在于:所述Ni-P金刚石化学复合镀层的制备材料由硫酸镍、次亚磷酸钠、柠檬酸钠、络合剂和金刚石微粒构成,且各材料的含量如下:硫酸镍25-40g/L,次亚磷酸钠15-18g/L,柠檬酸钠40-45g/L,络合剂0.8-1.5g/L,金刚石微粒4-10g/L。
2.根据权利要求1所述的一种Ni-P金刚石化学复合镀层,其特征在于:所述络合剂包括但不限于铬酸钾、乙酰丙酮、柠檬酸、酒石酸、草酸和磺基水杨酸。
3.根据权利要求1所述的一种Ni-P金刚石化学复合镀层,其特征在于:所述金刚石微粒由采用爆轰合成,直径为12-18μm。
4.根据权利要求1所述的一种Ni-P金刚石化学复合镀层,其特征在于:各材料的含量如下:硫酸镍30g/L,次亚磷酸钠15g/L,柠檬酸钠40g/L,络合剂1g/L,金刚石微粒5g/L。
5.根据权利要求1所述的一种Ni-P金刚石化学复合镀层,其特征在于:各材料的含量如下:硫酸镍35g/L,次亚磷酸钠16g/L,柠檬酸钠42g/L,络合剂1.2g/L,金刚石微粒8g/L。
6.根据权利要求1所述的一种Ni-P金刚石化学复合镀层,其特征在于:各材料的含量如下:硫酸镍40g/L,次亚磷酸钠18g/L,柠檬酸钠45g/L,络合剂1.4g/L,金刚石微粒10g/L。
7.根据权利要求1所述的一种Ni-P金刚石化学复合镀层的制备方法,其特征在于:包括以下步骤:
S1:对镀件进行喷砂处理,处理时间10-20分钟,去除镀件表面的杂质,使镀件表面粗化;
S2:将S1中处喷砂处理完的镀件放入浓度为10%的洗衣粉水溶液内进行超声波清洗,清洗时间为5-8分钟,然后将镀件取出使用自来水进行冲洗,冲洗完洗衣粉水溶液后,将镀件自然晾干备用;
S3:将S2中晾干的镀件放入浓度为5%的硫酸溶液中,浸泡4-6分钟,进行表面活性处理;
S4:然后制备初始化学镀液,使初始化学镀液的成分为硫酸镍25-40g/L,次亚磷酸钠15-18g/L,柠檬酸钠40-45g/L,络合剂0.8-1.5g/L,通过添加调节剂,将初始镀液的PH值调为4.4-4.8,然后取部分初始化学镀液,将S3中表面活性处理后的镀件放入初始化学镀液内进行预镀,镀覆温度为75-90℃,镀覆时间为2-2.5小时,镀层厚度为6-8μm;
S5:取S4中制备的初始化学镀液,往初始化学镀液内添加金刚石微粒,使金刚石微粒的含量为4-10g/L,形成金刚石镀液,通过添加调节剂,将金刚石镀液的PH值调节为4.4-4.8,然后将预镀后的镀件,放入金刚石镀液内进行镀覆,镀覆温度为75-90℃,镀覆时间为3-4小时,镀层厚度为10-12μm;
S6:将S5中镀覆完成的镀件取出,通过自来水进行冲洗,冲洗完成后,对镀件进行热处理,处理温度为170-190℃,处理时间为1.5-2.5小时,即可完成整个镀膜过程。
8.根据权利要求7所述的一种Ni-P金刚石化学复合镀层的制备方法,其特征在于:所述步骤S5中调节剂包括但不限于醋酸、醋酸钠和氢氧化钠。
9.根据权利要求7所述的一种Ni-P金刚石化学复合镀层的制备方法,其特征在于:所述步骤S5中,镀覆过程中需要每隔30分钟搅拌一次金刚石镀液。
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