CN113929312A - 一种无需贵金属活化在玻璃表面镀镍的方法 - Google Patents
一种无需贵金属活化在玻璃表面镀镍的方法 Download PDFInfo
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 101
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- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 24
- 239000007788 liquid Substances 0.000 claims description 18
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims description 16
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- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims description 12
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- 239000001632 sodium acetate Substances 0.000 claims description 12
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- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 claims description 8
- 229940038773 trisodium citrate Drugs 0.000 claims description 8
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- TXUICONDJPYNPY-UHFFFAOYSA-N (1,10,13-trimethyl-3-oxo-4,5,6,7,8,9,11,12,14,15,16,17-dodecahydrocyclopenta[a]phenanthren-17-yl) heptanoate Chemical compound C1CC2CC(=O)C=C(C)C2(C)C2C1C1CCC(OC(=O)CCCCCC)C1(C)CC2 TXUICONDJPYNPY-UHFFFAOYSA-N 0.000 description 3
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- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 description 1
- 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 description 1
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- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 description 1
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- 150000002940 palladium Chemical class 0.000 description 1
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 description 1
- 229910001379 sodium hypophosphite Inorganic materials 0.000 description 1
- GGCZERPQGJTIQP-UHFFFAOYSA-N sodium;9,10-dioxoanthracene-2-sulfonic acid Chemical compound [Na+].C1=CC=C2C(=O)C3=CC(S(=O)(=O)O)=CC=C3C(=O)C2=C1 GGCZERPQGJTIQP-UHFFFAOYSA-N 0.000 description 1
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- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
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Abstract
本发明公开了一种无需贵金属活化在玻璃表面镀镍的方法,属于化学镀镍技术领域。该方法包括:(1)粗化:将玻璃制品的待镀镍表面进行粗化;(2)活化:在粗化后的玻璃表面喷雾活化液,喷雾完成后采用150‑200℃热风将活化液吹干,再采用清水清洗玻璃表面;所述活化液含有NiSO4和NaH2PO2,所述NiSO4的浓度为130‑160g/L,所述NaH2PO2的浓度为200‑250g/L;(3)化学镀镍:在活化后的玻璃表面进行化学镀镍。该方法具有至少两个优点,一是无需使用含贵金属盐的活化液,能有效降低成本;二是各步骤均可采用喷雾的方式进行,便于局部施镀。
Description
技术领域
本发明属于化学镀镍技术领域,特别涉及一种无需贵金属活化在玻璃表面镀镍的方法。
背景技术
玻璃作为一种非晶态材料,具有高可见透光率、高电阻、制造成本低等优异性能,广泛应用于太阳能热水器的真空管制造、电真空器件、集成电路的封装基板、电光源等方面。玻璃作为基材时,可在其表面进行化学镀镍。但由于玻璃是非金属材料,在化学镀镍沉积过程中其表面不具有自催化活性,因此必须在化学施镀前对玻璃表面进行活化处理,目前大多数采用的是利用含有贵金属盐的活化液对玻璃表面进行活化,如钯盐、银盐等。但是现有工艺存在成本高、处理过程复杂,而且含有贵金属盐的活化液可能对环境具有较大污染。
发明内容
为了解决上述问题,本发明实施例提供了一种无需贵金属活化在玻璃表面镀镍的方法,该方法具有至少两个优点,一是无需使用含贵金属盐的活化液,能有效降低成本;二是各步骤均可采用喷雾的方式进行,便于局部施镀。所述技术方案如下:
本发明实施例提供了一种无需贵金属活化在玻璃表面镀镍的方法,该方法包括:
(1)粗化:将玻璃制品的待镀镍表面进行粗化。
(2)活化:在粗化后的玻璃表面喷雾活化液,喷雾完成后采用150-200℃热风将活化液吹干,再采用清水清洗玻璃表面以洗去活化液。其中,活化液含有NiSO4和NaH2PO2,NiSO4的浓度为130-160g/L, NaH2PO2的浓度为200-250g/L。其中,本实施例中的活化液的用量无严格要求,要求将待镀镍表面覆盖即可。在该步骤中,采用特定浓度的NiSO4和NaH2PO2在粗化后的玻璃表面生产少量的金属Ni单质,催化步骤(3)的进行。在该步骤中,需要在较高浓度与较高温度下(浸没法通常不能达到)进行。活化速度比较快。
(3)化学镀镍:在活化后的玻璃表面进行化学镀镍。
其中,步骤(1)包括:采用粗化液对玻璃表面进行粗化,粗化完成后,采用清水清洗玻璃表面以洗去粗化液。其中,粗化液含有氢氟酸和氟硅酸等,氢氟酸的浓度为3-10wt%,氟硅酸的浓度为3-10wt%。其中,粗化液也可以采用常规粗化液。本专利采用的粗化液对光纤表面具有良好的效果(常规的粗化液,不但粗化效果不好,还会使光纤的外径明显变小),且不会改变光纤的外径。
优选地,步骤(1)包括:在待镀镍的玻璃表面喷雾粗化液,喷雾完成后,室温静置0.5-2小时,再采用清水清洗玻璃表面以洗去粗化液。
在本发明的一种实施方式中,步骤(3)包括:将活化后的玻璃表面浸没在镀液中,于70-90℃下进行化学镀,施镀后采用清水清洗玻璃表面以洗去镀液。该过程与常规的化学镀的方式基本相同。如果要求镀镍表面更加平整,可采用本方法。
在本发明的另一种实施方式中,步骤(3)包括:在活化后的玻璃表面喷雾镀液,喷雾完成后采用40-60℃热风将镀液吹干,再采用清水清洗玻璃表面以洗去镀液。该方式适合各种玻璃表面的施镀,对玻璃表面进行局部施镀的效果好。如果要求局部镀镍,可采用本方法。
其中,镀液通常含有镍盐、还原剂和其他助剂等,镍盐通常为NiSO4,还原剂通常为NaH2PO2,助剂可以包括络合剂、缓冲剂等。具体地,镀液含有NiSO4、NaH2PO2、醋酸钠、乳酸和柠檬酸三钠等,NiSO4的浓度为20-25g/L,NaH2PO2的浓度为10-18g/L,醋酸钠的浓度为6-10g/L,乳酸的浓度为15-18g/L,柠檬酸三钠的浓度为2-8g/L。
优选地,镀液还含有硫脲(可作为稳定剂),硫脲的浓度为3-6PPM。
具体地,本发明提供的无需贵金属活化在玻璃表面镀镍的方法包括:
(1)粗化:在待镀镍的玻璃表面喷雾粗化液,喷雾完成后,室温静置0.5-2小时,再采用清水清洗玻璃表面。其中,粗化液含有氢氟酸和氟硅酸等,氢氟酸的浓度为3-10wt%,氟硅酸的浓度为3-10wt%。
(2)活化:在粗化后的玻璃表面喷雾活化液,喷雾完成后采用150-200℃热风将活化液吹干,再采用清水清洗玻璃表面。其中,活化液含有NiSO4和NaH2PO2,NiSO4的浓度为130-160g/L, NaH2PO2的浓度为200-250g/L。
(3)化学镀镍:将活化后的玻璃表面浸没在镀液中,于70-90℃下进行化学镀,施镀后采用清水清洗玻璃表面;或者在活化后的玻璃表面喷雾镀液,喷雾完成后采用40-60℃热风将镀液吹干,再采用清水清洗玻璃表面。其中,镀液含有NiSO4、NaH2PO2、醋酸钠、乳酸、柠檬酸三钠和硫脲等,NiSO4的浓度为20-25g/L,NaH2PO2的浓度为10-18g/L,醋酸钠的浓度为6-10g/L,乳酸的浓度为15-18g/L,柠檬酸三钠的浓度为2-8g/L,硫脲的浓度为3-6PPM。
其中,玻璃制品包括光纤、平面玻璃或凹凸面玻璃等,优选为光纤。
本发明实施例提供的技术方案具有如下有益效果:
(1)无需使用含贵金属盐的活化液,能有效降低成本。
(2)各步骤均可采用喷雾的方式进行,便于局部施镀。
(3)采用热风吹干的方式,可减低清洗时的用水量。
(4)镀镍效果与常规的化学镀镍的效果差不多。
(5)粗化时,对光纤表面的粗化效果好,且不会影响光纤的外径。
(6)采用喷雾烘干的方式,活化过程与化学镀镍的过程均非常快,提升生产效率。
(7)采用喷雾粗化、活化和镀镍,可降低粗化液、活化液和镀液的用量。
(8)传统的贵金属活化法通常使用钯活化体系,成本相当高,而且工艺过程复杂。通常用氯化亚锡敏化玻璃表面,然后再用钯离子活化,玻璃表面的亚锡将钯离子还原成金属。或者用氯化亚锡和氯化钯形成胶体钯体系,活化后再用酸解胶。或者用钯离子活化后玻璃表面后,再用还原剂压次磷酸钠或者水合肼将玻璃表面钯离子还原。传统的贵金属钯活化液都需要两步。而NiSO4和NaH2PO能形成亚稳态体系,能将活化剂和还原剂合并,一步就能活化。
附图说明
图1是实施例一的镀镍效果图;
图2是实施例二的镀镍效果图;
图3是实施例三的镀镍效果图;
图4是实施例四的镀镍效果图。
具体实施方式
为使本发明的目的、技术方案和优点更加清楚,下面将结合附图对本发明作进一步地详细描述。
实施例一
实施例一提供了一种在凹形玻璃面上镀镍的方法,包括以下步骤:
1、凹形玻璃面,喷5wt%的氢氟酸和5wt%的氟硅酸混合水溶液,室温静置1小时,清水洗去玻璃表面的粗化液,反复2次。
2、喷活化液,活化液NiSO4含量140g/L,NaH2PO2含量210g/L,喷完后,热风枪160℃吹干活化液。活化完成后,清水洗涤玻璃表面。
3、喷雾施镀,在玻璃面,喷镀液,60℃热风枪加热,施镀后,清水洗涤。凹形玻璃面施镀效果如图1所示,从图中可以看出,镀层均匀,表面光洁度好。镀层结合力的评价参照GB5270—85:热震实验,样品在200℃下烘烤10min,取出后立即投入室温冷水中,反复5次,用5倍放大镜观察表面无剥落、起泡。
实施例二
实施例二提供了一种在玻璃棒上镀镍的方法,包括以下步骤:
1、玻璃棒(凸型玻璃面),喷7wt%的氢氟酸和7wt%的氟硅酸混合水溶液,室温静置0.5小时,清水洗去玻璃表面的粗化液,反复3次。
2、喷活化液,活化液NiSO4含量150g/L,NaH2PO2含量230g/L,喷完后,热风枪180℃吹干活化液。活化完成后,清水洗涤玻璃表面。
3、浸没施镀,玻璃棒浸没于80℃镀液中,5分钟。玻璃棒(凸型玻璃面)施镀效果如图2所示,从图中可以看出,镀层均匀,表面光洁度好,局部施镀的效果好。镀层结合力的评价参照GB5270—85:热震实验,样品在200℃下烘烤10min,取出后立即投入室温冷水中,反复5次,用5倍放大镜观察表面无剥落、起泡。
实施例三
实施例三提供了一种在玻璃板上镀镍的方法,包括以下步骤:
1、玻璃板(平面玻璃),喷5wt%的氢氟酸和5wt%的氟硅酸混合水溶液,室温静置1小时,清水洗去玻璃表面的粗化液。
2、喷活化液,活化液NiSO4含量160g/L,NaH2PO2含量220g/L,喷完后,热风枪160℃吹干活化液。活化完成后,清水洗涤玻璃表面。
3、喷雾施镀,在玻璃面,喷镀液,50℃热风枪加热,施镀后,清水洗涤。平面玻璃面施镀效果如图3所示,从图中可以看出,镀层均匀,表面光洁度好,局部施镀的效果好。镀层结合力的评价参照GB5270—85:热震实验,样品在200℃下烘烤10min,取出后立即投入室温冷水中,反复5次,用5倍放大镜观察表面无剥落、起泡。
实施例四
实施例四提供了一种在光纤上镀镍的方法,包括以下步骤:
1、玻璃光纤(直径125um),喷8wt%的氢氟酸和8wt%的氟硅酸混合水溶液,室温静置1小时,清水洗去玻璃表面的粗化液。
2、喷活化液,活化液NiSO4含量150g/L,NaH2PO2含量220g/L,喷完后,热风枪160℃吹干活化液,清水洗涤玻璃表面。反复2次。
3、喷雾施镀,在光纤表面,喷镀液,55℃热风枪加热,施镀后,清水洗涤。50倍光学显微镜下,光纤施镀效果图4所示,从图中可以看出,镀层均匀,表面光洁度好。镀层结合力的评价参照GB5270—85:热震实验,样品在200℃下烘烤10min,取出后立即投入室温冷水中,反复5次,用5倍放大镜观察表面无剥落、起泡。
以上所述仅为本发明的较佳实施例,并不用以限制本发明,凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
Claims (9)
1.一种无需贵金属活化在玻璃表面镀镍的方法,其特征在于,所述方法包括:
(1)粗化:将玻璃制品的待镀镍表面进行粗化;
(2)活化:在粗化后的玻璃表面喷雾活化液,喷雾完成后采用150-200℃热风将活化液吹干,再采用清水清洗玻璃表面;所述活化液含有NiSO4和NaH2PO2,所述NiSO4的浓度为130-160g/L,所述NaH2PO2的浓度为200-250g/L;
(3)化学镀镍:在活化后的玻璃表面进行化学镀镍。
2.根据权利要求1所述的无需贵金属活化在玻璃表面镀镍的方法,其特征在于,步骤(1)包括:采用粗化液对玻璃表面进行粗化,粗化完成后,采用清水清洗玻璃表面;所述粗化液含有氢氟酸和氟硅酸,所述氢氟酸的浓度为3-10wt%,所述氟硅酸的浓度为3-10wt%。
3.根据权利要求2所述的无需贵金属活化在玻璃表面镀镍的方法,其特征在于,步骤(1)包括:在待镀镍的玻璃表面喷雾粗化液,喷雾完成后,室温静置0.5-2小时,再采用清水清洗玻璃表面。
4.根据权利要求1所述的无需贵金属活化在玻璃表面镀镍的方法,其特征在于,步骤(3)包括:将活化后的玻璃表面浸没在镀液中,于70-90℃下进行化学镀,施镀后采用清水清洗玻璃表面。
5.根据权利要求1所述的无需贵金属活化在玻璃表面镀镍的方法,其特征在于,步骤(3)包括:在活化后的玻璃表面喷雾镀液,喷雾完成后采用40-60℃热风将镀液吹干,再采用清水清洗玻璃表面。
6.根据权利要求4或5所述的无需贵金属活化在玻璃表面镀镍的方法,其特征在于,所述镀液含有NiSO4、NaH2PO2、醋酸钠、乳酸和柠檬酸三钠,所述NiSO4的浓度为20-25g/L,所述NaH2PO2的浓度为10-18g/L,所述醋酸钠的浓度为6-10g/L,所述乳酸的浓度为15-18g/L,所述柠檬酸三钠的浓度为2-8g/L。
7.根据权利要求6所述的无需贵金属活化在玻璃表面镀镍的方法,其特征在于,所述镀液还含有硫脲,所述硫脲的浓度为3-6PPM。
8.根据权利要求1所述的无需贵金属活化在玻璃表面镀镍的方法,其特征在于,所述方法包括:
(1)粗化:在待镀镍的玻璃表面喷雾粗化液,喷雾完成后,室温静置0.5-2小时,再采用清水清洗玻璃表面;所述粗化液含有氢氟酸和氟硅酸,所述氢氟酸的浓度为3-10wt%,所述氟硅酸的浓度为3-10wt%;
(2)活化:在粗化后的玻璃表面喷雾活化液,喷雾完成后采用150-200℃热风将活化液吹干,再采用清水清洗玻璃表面;所述活化液含有NiSO4和NaH2PO2,所述NiSO4的浓度为130-160g/L,所述NaH2PO2的浓度为200-250g/L;
(3)化学镀镍:将活化后的玻璃表面浸没在镀液中,于70-90℃下进行化学镀,施镀后采用清水清洗玻璃表面;或者在活化后的玻璃表面喷雾镀液,喷雾完成后采用40-60℃热风将镀液吹干,再采用清水清洗玻璃表面;所述镀液含有NiSO4、NaH2PO2、醋酸钠、乳酸、柠檬酸三钠和硫脲,所述NiSO4的浓度为20-25g/L,所述NaH2PO2的浓度为10-18g/L,所述醋酸钠的浓度为6-10g/L,所述乳酸的浓度为15-18g/L,所述柠檬酸三钠的浓度为2-8g/L,所述硫脲的浓度为3-6PPM。
9.根据权利要求1所述的无需贵金属活化在玻璃表面镀镍的方法,其特征在于,所述玻璃制品包括光纤、平面玻璃或凹凸面玻璃。
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