CN112144272A - 一种碳纤维化学镀镍表面改性的方法 - Google Patents
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- 229920000049 Carbon (fiber) Polymers 0.000 title claims abstract description 124
- 239000004917 carbon fiber Substances 0.000 title claims abstract description 124
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 122
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 74
- 238000007747 plating Methods 0.000 title claims abstract description 45
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- 239000000126 substance Substances 0.000 title claims abstract description 35
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- 235000019270 ammonium chloride Nutrition 0.000 claims abstract description 25
- 230000003213 activating effect Effects 0.000 claims abstract description 24
- 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 abstract description 18
- 239000011259 mixed solution Substances 0.000 claims abstract description 18
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 claims abstract description 18
- 229910001379 sodium hypophosphite Inorganic materials 0.000 claims abstract description 18
- 239000003292 glue Substances 0.000 claims abstract description 15
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 14
- 230000001235 sensitizing effect Effects 0.000 claims abstract description 11
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 27
- 239000008367 deionised water Substances 0.000 claims description 20
- 229910021641 deionized water Inorganic materials 0.000 claims description 20
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- 235000011150 stannous chloride Nutrition 0.000 claims description 7
- AXZWODMDQAVCJE-UHFFFAOYSA-L tin(II) chloride (anhydrous) Chemical compound [Cl-].[Cl-].[Sn+2] AXZWODMDQAVCJE-UHFFFAOYSA-L 0.000 claims description 7
- 238000007788 roughening Methods 0.000 claims description 4
- 238000003837 high-temperature calcination Methods 0.000 claims description 2
- 238000001354 calcination Methods 0.000 claims 2
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- 229910052751 metal Inorganic materials 0.000 abstract description 3
- 239000002184 metal Substances 0.000 abstract description 3
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- 230000007935 neutral effect Effects 0.000 description 18
- 238000003756 stirring Methods 0.000 description 12
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 7
- 239000001509 sodium citrate Substances 0.000 description 7
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 description 7
- NCPXQVVMIXIKTN-UHFFFAOYSA-N trisodium;phosphite Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])[O-] NCPXQVVMIXIKTN-UHFFFAOYSA-N 0.000 description 7
- 238000002156 mixing Methods 0.000 description 6
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 description 6
- 229940053662 nickel sulfate Drugs 0.000 description 6
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 description 6
- 230000000694 effects Effects 0.000 description 2
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
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- 230000003247 decreasing effect Effects 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
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- 238000010438 heat treatment Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- RRIWRJBSCGCBID-UHFFFAOYSA-L nickel sulfate hexahydrate Chemical compound O.O.O.O.O.O.[Ni+2].[O-]S([O-])(=O)=O RRIWRJBSCGCBID-UHFFFAOYSA-L 0.000 description 1
- 229940116202 nickel sulfate hexahydrate Drugs 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
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- 229920002239 polyacrylonitrile Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
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- 238000004544 sputter deposition Methods 0.000 description 1
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- 230000004580 weight loss Effects 0.000 description 1
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Abstract
本发明属于纤维材料表面改性技术领域，具体涉及一种碳纤维化学镀镍表面改性的方法，包括以下步骤：除胶，粗化，敏化，活化。首先通过高温灼烧除去碳纤维表面的胶，然后将处理好的碳纤维浸泡到氢氟酸和浓磷酸混合的溶液中，改变碳纤维表面微观结构，增大金属镀层之间的结合力，然后再将粗化后的碳纤维浸泡在SnCl2中，是碳纤维表面附着一层还原性好的物质，再将敏化后的碳纤维浸泡到由氯化钯，氯化铵，次磷酸钠组成的活化液中，使得在碳纤维形成一层贵金属单质，最后对活化好的碳纤维进行镀镍处理，改性后的碳纤维有好的润湿性，可以使镍镀层更加均匀致密，附着力强。
Description
技术领域
本发明属于纤维材料表面改性技术领域，具体涉及一种碳纤维化学镀镍表面改性的方法。
背景技术
碳纤维是通过高温热解聚丙烯腈基碳纤维、粘胶基碳纤维、沥青基碳纤维等有机纤维而制备出来的碳含量高于95％的纤维，它不仅具有碳材料的本征特性，还具有纤维的可加工性。碳纤维具有比模量高、比强度高、耐高温、耐辐射、密度低、导电、热膨胀系数小等一系列优良性能，在许多领域有广阔的应用前景。
然而，碳纤维的表面能低，具有活性的官能团含量较少，反应活性低，导致其与基体粘结性和浸润性较差，这极大地限制了碳纤维性能的发挥。碳纤维表面金属化是改变表面性质和结构，实现对碳纤维表面的控制，改善碳纤维的表面活性及与其它材料的相容性的有效方法，也是制备先进复合材料，获得各种新型功能材料的有效途径。碳纤维表面金属化的方法主要包括化学镀法、电镀法、气相沉积法、溅射法等。其中，化学镀所形成的镀层厚度均匀、光洁平整、致密无孔隙，工艺设备简单，易于控制，是非金属表面金属化的常用方法。碳纤维化学镀镍是最常用的方法之一，可以大大改善并提高碳纤维的性能。
发明内容
本发明的目的是提供一种碳纤维化学镀镍表面改性的方法，改性后的碳纤维有好的润湿性，可以使镍镀层更加均匀致密，附着力强。
一种碳纤维化学镀镍表面改性的方法，包括以下步骤：
(1)首先对碳纤维进行除胶处理，将碳纤维在300-500℃进行高温煅烧15-30min。
(2)将步骤(1)得到的碳纤维进行粗化处理，将碳纤维浸泡在氢氟酸和浓磷酸的混合溶液中，混合溶液的体积分数在10％-20％，浸泡时间为10-40min。取出后用去离子水清洗至中性，放置干燥。
(3)将步骤(2)得到的粗化后的碳纤维进行敏化处理，将碳纤维浸泡在SnCl2溶液中，质量浓度为5％-15％。浸泡时间为15-30min。
(4)将步骤(3)得到的敏化后的碳纤维进行活化处理，将碳纤维浸泡在氯化钯，氯化铵，次磷酸钠的混合溶液中，浸泡时间为10-30min。
(5)然后将活化好的碳纤维浸泡在准备好的化学镀液中，首先将六水硫酸镍溶于水，然后依次加入亚磷酸钠，柠檬酸钠，氯化铵和十二烷基硫酸钠，制得化学镀液。
本发明的有益效果是，以氢氟酸和浓磷酸为粗化液，可以更好的改变碳纤维表面的微观结构，增大金属镀层之间的结合力，以氯化钯，氯化铵，次磷酸钠的混合溶液为活化溶液，让碳纤维表面附着金属胶粒，可以使镍层更致密的附着在碳纤维表面。
具体实施方式
为了使本发明的目的、技术方案及优点更加清楚明白，以下结合实施例，对本发明进行进一步详细说明。应当理解，此处所描述的具体实施例仅仅用以解释本发明，并不用于限定本发明。
实施例一
碳纤维进行表面改性然后化学镀镍的方法，包括以下步骤：
(1)除胶，将碳纤维放在马弗炉中在300℃下进行高温灼烧30min。
(2)粗化，将步骤(1)除胶后的碳纤维浸泡在体积分数为10％的氢氟酸和浓磷酸的混合溶液中30min，然后取出后用去离子水洗至中性，干燥待用。
(3)敏化，将步骤(2)粗化后的碳纤维浸泡在质量浓度为5％的SnCl2溶液中15min，然后取出用去离子水洗至中性，干燥待用。
(4)活化，将氯化钯，氯化铵，次磷酸钠混合搅拌10min，制得活化液，氯化钯的浓度为0.5g/L，氯化铵的浓度为0.5g/L，次磷酸钠的浓度为1g/L，将步骤(3)敏化后的碳纤维浸泡活化液中10min，取出后用去离子水洗至中性，干燥待用。
(5)化学镀镍，将硫酸镍溶于水，然后分别加入加入亚磷酸钠，柠檬酸钠，氯化铵和十二烷基硫酸钠搅拌10min，制得化学镀液，将步骤(4)处理好的碳纤维浸泡在化学镀液中10min，得到表面镀镍碳纤维。
实施例二
碳纤维进行表面改性然后化学镀镍的方法，包括以下步骤：
(1)除胶，将碳纤维放在马弗炉中在400℃下进行高温灼烧20min。
(2)粗化，将步骤(1)除胶后的碳纤维浸泡在体积分数为15％的氢氟酸和浓磷酸的混合溶液中20min，然后取出后用去离子水洗至中性，干燥待用。
(3)敏化，将步骤(2)粗化后的碳纤维浸泡在质量浓度为10％的SnCl2溶液中20min，然后取出用去离子水洗至中性，干燥待用。
(4)活化，将氯化钯，氯化铵，次磷酸钠混合搅拌10min，制得活化液，氯化钯的浓度为1g/L，氯化铵的浓度为1g/L，次磷酸钠的浓度为2g/L，将步骤(3)敏化后的碳纤维浸泡活化液中20min，取出后用去离子水洗至中性，干燥待用。
(5)化学镀镍，将硫酸镍溶于水，然后分别加入加入亚磷酸钠，柠檬酸钠，氯化铵和十二烷基硫酸钠搅拌10min，制得化学镀液，将步骤(4)处理好的碳纤维浸泡在化学镀液中10min，得到表面镀镍碳纤维。
实施例三
碳纤维进行表面改性然后化学镀镍的方法，包括以下步骤：
(1)除胶，将碳纤维放在马弗炉中在500℃下进行高温灼烧10min。
(2)粗化，将步骤(1)除胶后的碳纤维浸泡在体积分数为20％的氢氟酸和浓磷酸的混合溶液中10min，然后取出后用去离子水洗至中性，干燥待用。
(3)敏化，将步骤(2)粗化后的碳纤维浸泡在质量浓度为15％的SnCl2溶液中30min，然后取出用去离子水洗至中性，干燥待用。
(4)活化，将氯化钯，氯化铵，次磷酸钠混合搅拌10min，制得活化液，氯化钯的浓度为1.5g/L，氯化铵的浓度为1.5g/L，次磷酸钠的浓度为3g/L，将步骤(3)敏化后的碳纤维浸泡活化液中30min，取出后用去离子水洗至中性，干燥待用。
(5)化学镀镍，将硫酸镍溶于水，然后分别加入加入亚磷酸钠，柠檬酸钠，氯化铵和十二烷基硫酸钠搅拌10min，制得化学镀液，将步骤(4)处理好的碳纤维浸泡在化学镀液中10min，得到表面镀镍碳纤维。
实施例四
碳纤维进行表面改性然后化学镀镍的方法，包括以下步骤：
(1)除胶，将碳纤维放在马弗炉中在300℃下进行高温灼烧20min。
(2)粗化，将步骤(1)除胶后的碳纤维浸泡在体积分数为20％的氢氟酸和浓磷酸的混合溶液中10min，然后取出后用去离子水洗至中性，干燥待用。
(3)敏化，将步骤(2)粗化后的碳纤维浸泡在质量浓度为15％的SnCl2溶液中30min，然后取出用去离子水洗至中性，干燥待用。
(4)活化，将氯化钯，氯化铵，次磷酸钠混合搅拌10min，制得活化液，氯化钯的浓度为2g/L，氯化铵的浓度为2g/L，次磷酸钠的浓度为4g/L，将步骤(3)敏化后的碳纤维浸泡活化液中20min，取出后用去离子水洗至中性，干燥待用。
(5)化学镀镍，将硫酸镍溶于水，然后分别加入加入亚磷酸钠，柠檬酸钠，氯化铵和十二烷基硫酸钠搅拌10min，制得化学镀液，将步骤(4)处理好的碳纤维浸泡在化学镀液中10min，得到表面镀镍碳纤维。
实施例五
碳纤维进行表面改性然后化学镀镍的方法，包括以下步骤：
(1)除胶，将碳纤维放在马弗炉中在400℃下进行高温灼烧20min。
(2)粗化，将步骤(1)除胶后的碳纤维浸泡在体积分数为10％的氢氟酸和浓磷酸的混合溶液中30min，然后取出后用去离子水洗至中性，干燥待用。
(3)敏化，将步骤(2)粗化后的碳纤维浸泡在质量浓度为5％的SnCl2溶液中15min，然后取出用去离子水洗至中性，干燥待用。
(4)活化，将氯化钯，氯化铵，次磷酸钠混合搅拌10min，制得活化液，氯化钯的浓度为1g/L，氯化铵的浓度为1g/L，次磷酸钠的浓度为2g/L，将步骤(3)敏化后的碳纤维浸泡活化液中10min，取出后用去离子水洗至中性，干燥待用。
(5)化学镀镍，将硫酸镍溶于水，然后分别加入加入亚磷酸钠，柠檬酸钠，氯化铵和十二烷基硫酸钠搅拌10min，制得化学镀液，将步骤(4)处理好的碳纤维浸泡在化学镀液中10min，得到表面镀镍碳纤维。
实施例六
碳纤维进行表面改性然后化学镀镍的方法，包括以下步骤：
(1)除胶，将碳纤维放在马弗炉中在500℃下进行高温灼烧10min。
(2)粗化，将步骤(1)除胶后的碳纤维浸泡在体积分数为15％的氢氟酸和浓磷酸的混合溶液中20min，然后取出后用去离子水洗至中性，干燥待用。
(3)敏化，将步骤(2)粗化后的碳纤维浸泡在质量浓度为10％的SnCl2溶液中20min，然后取出用去离子水洗至中性，干燥待用。
(4)活化，将氯化钯，氯化铵，次磷酸钠混合搅拌10min，制得活化液，氯化钯的浓度为1.5g/L，氯化铵的浓度为1.5g/L，次磷酸钠的浓度为3g/L，将步骤(3)敏化后的碳纤维浸泡活化液中15min，取出后用去离子水洗至中性，干燥待用。
(5)化学镀镍，将硫酸镍溶于水，然后分别加入加入亚磷酸钠，柠檬酸钠，氯化铵和十二烷基硫酸钠搅拌10min，制得化学镀液，将步骤(4)处理好的碳纤维浸泡在化学镀液中10min，得到表面镀镍碳纤维。
为了测试碳纤维与镍层的结合是否紧密，我们通过对镀镍的碳纤维进行热处理，观察碳纤维表面是否有镍层脱落或者起泡的情况，并且测量各个实例的失重率，下面对本发明进行性能测试。
表1不同实例拉伸强度，导电率与电磁屏蔽性能
我们可知，同样的没镀镍的碳纤维的电阻率为7.8Ω*m，所以我们可知碳纤维镀镍后电阻率明显下降。从上述表格来看，实例二效果最优，是由于在氢氟酸和浓磷酸混合液中粗化时间最合适，充分氧化侵蚀了碳纤维表面微观结构，而实验三中由于氢氟酸和浓磷酸混合溶液体积分数过高，而且浸泡时间过长，破坏了碳纤维的韧度，导致镍层不够致密，所以导电率下降。从上述数据可知，本发明采用的氢氟酸和浓磷酸的混合溶液作为粗化液效果显著提高。
以上所述仅为本发明的较佳实施例而已，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、等同替换和改进等，均应包含在本发明的保护范围之内。
Claims (5)
1.一种碳纤维化学镀镍表面改性的方法，其特征在于，包括以下步骤：除胶、粗化、敏化、活化；
(1)首先对碳纤维进行除胶处理，将碳纤维在300-500℃进行高温煅烧15-30min；
(2)将步骤(1)得到的碳纤维进行粗化处理，将碳纤维浸泡在氢氟酸和浓磷酸的混合溶液中，混合溶液的体积分数在10％-20％，浸泡时间为10-40min。取出后用去离子水清洗至中性，放置干燥；
(3)将步骤(2)得到的粗化后的碳纤维进行敏化处理，将碳纤维浸泡在SnCl2溶液中，质量浓度为5％-15％。浸泡时间为15-30min；
(4)将步骤(3)得到的敏化后的碳纤维进行活化处理，将碳纤维浸泡在氯化钯，氯化铵，次磷酸钠的混合溶液中，浸泡时间为10-30min。
2.根据权利1所述的一种碳纤维化学镀镍表面改性的方法，其特征在于，步骤(1)所述的高温煅烧温度为300-500℃，煅烧时间为15-30min。
3.根据权利1所述的一种碳纤维化学镀镍表面改性的方法，其特征在于，步骤(2)粗化液氢氟酸和浓磷酸的混合溶液的体积分数为10％-20％，浸泡时间为10-40min。
4.根据权利1所述的一种碳纤维化学镀镍表面改性的方法，其特征在于，步骤(3)敏化液质量浓度为5％-15％。浸泡时间为15-30min。
5.根据权利1所述的一种碳纤维化学镀镍表面改性的方法，其特征在于，步骤(4)活化液中氯化钯，氯化铵，次磷酸钠的浓度分别为：氯化钯0.5-2g/L，氯化铵0.5-2g/L，次磷酸钠1-4g/L。
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114622400A (zh) * | 2022-04-12 | 2022-06-14 | 武汉纺织大学 | 一种增强碳纤维抗氧化性能和电热性能的表面改性方法 |
| CN115700310A (zh) * | 2022-11-18 | 2023-02-07 | 惠州学院 | 一种镍金属烯修饰的复合碳纤维及其制备方法 |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106801335A (zh) * | 2016-12-12 | 2017-06-06 | 东莞市佳乾新材料科技有限公司 | 一种高性能表面镀镍碳纤维的制备方法 |
| CN106906646A (zh) * | 2017-03-02 | 2017-06-30 | 昆明理工大学 | 一种碳纤维表面金属化处理方法 |
| CN107815854A (zh) * | 2017-09-30 | 2018-03-20 | 中车青岛四方机车车辆股份有限公司 | 镀镍碳纤维膜、其制作方法、屏蔽结构与其制备方法 |
-
2020
- 2020-09-28 CN CN202011037027.XA patent/CN112144272A/zh active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106801335A (zh) * | 2016-12-12 | 2017-06-06 | 东莞市佳乾新材料科技有限公司 | 一种高性能表面镀镍碳纤维的制备方法 |
| CN106906646A (zh) * | 2017-03-02 | 2017-06-30 | 昆明理工大学 | 一种碳纤维表面金属化处理方法 |
| CN107815854A (zh) * | 2017-09-30 | 2018-03-20 | 中车青岛四方机车车辆股份有限公司 | 镀镍碳纤维膜、其制作方法、屏蔽结构与其制备方法 |
| US20200299894A1 (en) * | 2017-09-30 | 2020-09-24 | Crrc Qingdao Sifang Co., Ltd | Nickel-Plated Carbon Fiber Film, Manufacturing Method of Nickel-Plated Carbon Fiber Film, Shielding Structure and Preparation Method of Shielding Structure |
Non-Patent Citations (1)
| Title |
|---|
| 董艳晖等: "碳纤维表面化学镀镍工艺研究", 《电镀与涂饰》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114622400A (zh) * | 2022-04-12 | 2022-06-14 | 武汉纺织大学 | 一种增强碳纤维抗氧化性能和电热性能的表面改性方法 |
| CN115700310A (zh) * | 2022-11-18 | 2023-02-07 | 惠州学院 | 一种镍金属烯修饰的复合碳纤维及其制备方法 |
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