CN102002688A - No-palladium activate fluid formula and activation method of fabric chemical plating iron and nickel - Google Patents
No-palladium activate fluid formula and activation method of fabric chemical plating iron and nickel Download PDFInfo
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- CN102002688A CN102002688A CN 201010263096 CN201010263096A CN102002688A CN 102002688 A CN102002688 A CN 102002688A CN 201010263096 CN201010263096 CN 201010263096 CN 201010263096 A CN201010263096 A CN 201010263096A CN 102002688 A CN102002688 A CN 102002688A
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- fabric
- methyl alcohol
- potassium borohydride
- activation
- nickel
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Abstract
The invention discloses a no-palladium active fluid formula and an activation method of fabric chemical plating iron and nickel. The no-palladium active fluid formula comprises the following components in each liter of analytically pure methyl alcohol: 100-150g of nickelous acetate, 5-10mL of polyoxyethylene nonyl phenyl ether-10 surface active agent and 50-100g of potassium borohydride. The preparation method comprises the following steps of: preparing a methyl alcohol solution of potassium borohydride by using 50-100g of potassium borohydride in each liter of analytically pure methyl alcohol; and preparing mixed liquid by using following components by weight in each liter of analytically pure methyl alcohol: 100-150g of nickelous acetate and 5-10mL of polyoxyethylene nonyl phenyl ether-10 surface active agent. The activation method comprises the following steps of: when activating, firstly soaking a fabric for 3 minutes in the mixed liquid; then, taking out, immerging the fabric into the methyl alcohol solution of the potassium borohydride under a mixing condition to activate, wherein an activating process does not need mixing step, activating temperature condition is at room temperature and activation lasts for 25-35 minutes; after being activated, taking out and washing the fabric; and drying the fabric for 30 minutes in a thermostatic drying box of 60 DEG C. In the invention, catalytic active sites comprising nickel and nickel-boron alloy are formed on the surface of the fabric. The activation method is used for replacing an activation method of palladium activation and has the advantages of low temperature and economy.
Description
Technical field
The present invention relates to the chemical plating of non-metal material field, particularly a kind of no-palladium activating plating prescription and activation method of fabric chemical plating iron nickel.
Background technology
Metallized fabrics is a purposes flexible electromagnetic shielding material the most widely.Electroless plating is one of metallized effective way of non-metallic material, occupies critical role in the metallization of fabric field.The fabric fiber material surface does not have catalytic activity, forms one deck precious metal catalyst active centre (i.e. activation) on its surface, is the critical process that electroless plating prepares the flexible metal textiles.Traditional technology is to adopt PdCl
2-SnCl
2Activation---sensitizing.And this process treatment process complexity is used PdCl
2Cost an arm and a leg, and also have toxicity, make its application be subjected to certain restriction.Therefore, continually develop the novel activating process of low cost, environment-friendly type, saving precious metal, must have broad application prospects.
Report (the Lai Dongzhi that textile cloth no-palladium activating is arranged in the fabric, Chen Wenxing, Yao Yuefei, Liu Guanfeng. be applied to the new activation method [J] of fabric electroless plating. textile journal, 2006,27 (1): 34-37), but cotton fibre and chemical fiber textural difference are very big, and the too late chemical fiber of textile cloth industrial applicability, and make it not obtain more application.The present invention is solvent at normal temperatures with methyl alcohol, utilize the lyotropy of tensio-active agent OP-10, strengthen the absorption of polyester piece good to nickelous acetate, be adsorbed on nickelous acetate on the polyester piece good with stability than the direct reduction of the better strong reducing property POTASSIUM BOROHYDRIDE of sodium borohydride, thereby form nickeliferous and catalytic activity point ni-b alloy at fabric face, replacement palladium activatory chemical plating iron nickel no-palladium activating technology and prescription do not appear in the newspapers.
Summary of the invention
The no-palladium activating electroplate liquid formulation and the activation method that the purpose of this invention is to provide a kind of fabric chemical plating iron nickel.
Chemical plating iron nickel on the fabric, at first with fabric after scrubbing, oil removing, alligatoring, pre-activated are handled, carry out the chemical plating iron nickelalloy again.The present invention is exactly at activation stage, has proposed a kind of no-palladium activating liquid formula and activation method.
Chemical plating iron nickel no-palladium activating liquid formula is on the fabric: every liter of analytical pure methyl alcohol contains nickelous acetate 100-150g, polyoxyethylene nonylphenol ether-10 tensio-active agent 5-10mL and POTASSIUM BOROHYDRIDE 50-100g.
The activation method concrete steps are: contain the methanol solution that POTASSIUM BOROHYDRIDE 50-100g prepares POTASSIUM BOROHYDRIDE by every liter of analytical pure methyl alcohol, contain nickelous acetate 100-150g, polyoxyethylene nonylphenol ether-10 tensio-active agent 5-10mL by every liter of analytical pure methyl alcohol again and prepare mixed solution; During activation, earlier fabric is put into above-mentioned mixed solution and soak 30min, take out then, immerse in the methanol solution of above-mentioned POTASSIUM BOROHYDRIDE under agitation condition, activate, reactivation process does not need to stir.Temperature: room temperature, soak time: 25-35min takes out fabric washing, places 60 ℃ of dry 30min of thermostatic drying chamber to get final product after the activation.
The selection principle that activation solution is formed in the activating process is: at first nickel has very strong autocatalysis activity, utilizes reductive agent reduced nickel ion to produce active site.Hydroborate has reduction efficiency height, normal temperature as reductive agent obviously advantage such as can carry out.So select for use stability preferably POTASSIUM BOROHYDRIDE make reductive agent.The second, solvent must be fine to the solvability of nickel salt, and the wettability of polyester piece good in this solvent will get well, and can adsorb enough nickel, so just can be activated base cloth and good coating uniformly.So select for use methyl alcohol to make solvent, tensio-active agent polyoxyethylene nonylphenol ether-10 has the lyotropy choosing and does the additive use.The 3rd, solubleness in methyl alcohol such as single nickel salt, nickelous chloride is very little, and the oxidisability of nickelous nitrate is too strong, so the nickel salt in the activation solution is best with nickelous acetate.The 4th, POTASSIUM BOROHYDRIDE is slightly soluble in methyl alcohol, and it is saturated to keep activation solution, and activation efficiency is improved.Therefore, activation solution consists of: nickelous acetate, tensio-active agent polyoxyethylene nonylphenol ether-10, POTASSIUM BOROHYDRIDE, methyl alcohol (making solvent).
The present invention utilizes the potassium borohydride reduction nickelous acetate at normal temperatures, thereby forms nickeliferous and catalytic activity point ni-b alloy at fabric face, replaces the advantage that palladium activatory activation method has low temperature, economy with this.
Utilize scanning electron microscope that the iron-nickel alloy coating that obtains behind no-palladium activating is carried out pattern and characterize, can obviously find out coating in conjunction with densification, particles dispersed is more even.Utilize diffractometer that nickel coating is carried out Phase Structure Analysis, can find out obviously that being respectively 45 °, 52.5 ° at 2 θ angles diffraction peak (diffuse peaks) occurs, 2 θ angles are FeNi for 45 °
3Diffraction peak, 2 θ angles are non-crystalline state FeNi for 45 °
3, Ni
3The diffraction peak of P alloy illustrates that coating is duplex grain structure under plated state.Use energy spectrometer to measure polyester piece good plating iron nickel alloy coating composition and content, show that the content that contains Ni, Fe, P nickel in the coating is the highest.
Embodiment
Embodiment:
Formula for chemical plating nickel and technology:
(1) chemical scrubbing deoiling method: repeatedly the back is clean with distilled water flushing in common washing powder washing.
(2) coarsening solution prescription and processing condition
NaOH 200g/L
Time (t) 30min
65～70 ℃ of temperature (T)
(3) activation solution prescription and processing condition
Nickelous acetate 150g/ methyl alcohol (L);
Polyoxyethylene nonylphenol ether-10 5mL/ methyl alcohol (L)
Sodium borohydride 100g/ methyl alcohol (L);
Temperature (℃): room temperature
Time (min): 30
Activation method is: contain the methanol solution that POTASSIUM BOROHYDRIDE 50-100g prepares POTASSIUM BOROHYDRIDE by every liter of analytical pure methyl alcohol, contain nickelous acetate 100-150g, polyoxyethylene nonylphenol ether-10 tensio-active agent 5-10mL by every liter of analytical pure methyl alcohol again and prepare mixed solution; During activation, earlier fabric is put into above-mentioned mixed solution and soak 30min, take out then, immerse in the methanol solution of above-mentioned POTASSIUM BOROHYDRIDE under agitation condition, activate, reactivation process does not need to stir.Temperature: room temperature, soak time: 30min takes out fabric washing, places 60 ℃ of dry 30min of thermostatic drying chamber to get final product after the activation.
(4) chemical plating iron nickelalloy electroplate liquid formulation and processing condition
Prescription mainly is made up of following material: single nickel salt; Ferrous ammonium sulphate; Inferior sodium phosphate; Ammonium citrate; Seignette salt; Boric acid.
Single nickel salt 16g/L
Ferrous ammonium sulphate 16g/L
Inferior sodium phosphate 42g/L
Ammonium citrate 40g/L
Seignette salt 10g/L
Boric acid 30g/L
pH 9.0～10
80 ℃ of temperature
Dissolve earlier single nickel salt, ferrous ammonium sulphate, inferior sodium phosphate, ammonium citrate, Seignette salt and boric acid respectively.Under agitation condition, earlier ammonium citrate, Seignette salt are mixed and made into compound complex agent solution, under vigorous stirring, single nickel salt, l ferrous ammonium sulfate solution are slowly added in the compound complex agent solution successively then, under agitation respectively ortho phosphorous acid sodium solution, boric acid solution are slowly added in the above-mentioned solution then.Can also add stablizer thiocarbamide, accelerator Succinic Acid as one sees fit.Regulate the pH value with NaOH then, be diluted to volume required at last.
Claims (2)
1. the no-palladium activating liquid of a fabric chemical plating iron nickel, it is as follows to it is characterized in that filling a prescription: contain nickelous acetate 100-150g, polyoxyethylene nonylphenol ether-10 tensio-active agent 5-10mL and POTASSIUM BOROHYDRIDE 50-100g in every liter of analytical pure methyl alcohol.
2. the activation method of a fabric face chemical plating iron nickel no-palladium activating liquid as claimed in claim 1, it is characterized in that step is: contain the methanol solution that POTASSIUM BOROHYDRIDE 50-100g prepares POTASSIUM BOROHYDRIDE by every liter of analytical pure methyl alcohol, contain nickelous acetate 100-150g, polyoxyethylene nonylphenol ether-10 tensio-active agent 5-10mL by every liter of analytical pure methyl alcohol again and prepare mixed solution; During activation, earlier fabric is put into above-mentioned mixed solution and soak 30min, take out then, immerse in the methanol solution of above-mentioned POTASSIUM BOROHYDRIDE under agitation condition, activate, reactivation process does not need to stir; Temperature: room temperature, soak time: 25-35min takes out fabric washing, places 60 ℃ of dry 30min of thermostatic drying chamber to get final product after the activation.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010263096 CN102002688A (en) | 2010-08-24 | 2010-08-24 | No-palladium activate fluid formula and activation method of fabric chemical plating iron and nickel |
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|---|---|---|---|
| CN 201010263096 CN102002688A (en) | 2010-08-24 | 2010-08-24 | No-palladium activate fluid formula and activation method of fabric chemical plating iron and nickel |
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| CN102002688A true CN102002688A (en) | 2011-04-06 |
Family
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| CN 201010263096 Pending CN102002688A (en) | 2010-08-24 | 2010-08-24 | No-palladium activate fluid formula and activation method of fabric chemical plating iron and nickel |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102154818A (en) * | 2011-05-16 | 2011-08-17 | 东北林业大学 | Method for preparing nickel coating on surface of cotton fabric or linen fabric |
| CN103014680A (en) * | 2011-09-26 | 2013-04-03 | 中国科学院金属研究所 | Surface chemical nickel-plating no-palladium activation method of magnesium alloy micro-arc oxidation ceramic layer and application |
| CN103469562A (en) * | 2013-09-22 | 2013-12-25 | 武汉纺织大学 | Preparation method of fabric surface by employing atomizing chemical plating |
| CN103695905A (en) * | 2012-09-27 | 2014-04-02 | 中国科学院金属研究所 | Method for preparing composite nickel coating on surface of magnesium alloy micro-arc oxidation film |
| CN104213105A (en) * | 2014-10-11 | 2014-12-17 | 东北林业大学 | Method of nickel, ferrum and phosphorus ternary alloy chemical plating on wood surface |
| CN105200761A (en) * | 2015-10-13 | 2015-12-30 | 四川大学 | Palladium-free activation chemical nickel-plating method for electromagnetic shielding polyphenylene sulfide fiber |
| CN109735830A (en) * | 2019-02-19 | 2019-05-10 | 广东工业大学 | A kind of preparation method of activating solution and preparation method and carbon fibre composite |
| CN113151811A (en) * | 2021-04-13 | 2021-07-23 | 赤壁市聚茂新材料科技有限公司 | Non-palladium activated nickel plating solution and nickel plating method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1772950A (en) * | 2005-11-01 | 2006-05-17 | 桂林工学院 | No-palladium activating recipe for chemical nickel plating on plastic surface and its technological process |
| CN101096756A (en) * | 2006-06-30 | 2008-01-02 | 佛山市顺德区汉达精密电子科技有限公司 | Activation method for electroless plating nickel iron |
-
2010
- 2010-08-24 CN CN 201010263096 patent/CN102002688A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1772950A (en) * | 2005-11-01 | 2006-05-17 | 桂林工学院 | No-palladium activating recipe for chemical nickel plating on plastic surface and its technological process |
| CN101096756A (en) * | 2006-06-30 | 2008-01-02 | 佛山市顺德区汉达精密电子科技有限公司 | Activation method for electroless plating nickel iron |
Non-Patent Citations (1)
| Title |
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| 《纺织学报》 20060131 赖冬志等 应用于织物化学镀的新活化方法 第34-37页 1-2 第27卷, 第1期 2 * |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102154818A (en) * | 2011-05-16 | 2011-08-17 | 东北林业大学 | Method for preparing nickel coating on surface of cotton fabric or linen fabric |
| CN102154818B (en) * | 2011-05-16 | 2012-05-09 | 东北林业大学 | Method for preparing nickel coating on surface of cotton fabric or linen fabric |
| CN103014680A (en) * | 2011-09-26 | 2013-04-03 | 中国科学院金属研究所 | Surface chemical nickel-plating no-palladium activation method of magnesium alloy micro-arc oxidation ceramic layer and application |
| CN103695905A (en) * | 2012-09-27 | 2014-04-02 | 中国科学院金属研究所 | Method for preparing composite nickel coating on surface of magnesium alloy micro-arc oxidation film |
| CN103695905B (en) * | 2012-09-27 | 2016-03-16 | 中国科学院金属研究所 | A kind of method preparing composite nickel coating on magnesium alloy differential arc oxidation film surface |
| CN103469562A (en) * | 2013-09-22 | 2013-12-25 | 武汉纺织大学 | Preparation method of fabric surface by employing atomizing chemical plating |
| CN104213105A (en) * | 2014-10-11 | 2014-12-17 | 东北林业大学 | Method of nickel, ferrum and phosphorus ternary alloy chemical plating on wood surface |
| CN105200761A (en) * | 2015-10-13 | 2015-12-30 | 四川大学 | Palladium-free activation chemical nickel-plating method for electromagnetic shielding polyphenylene sulfide fiber |
| CN109735830A (en) * | 2019-02-19 | 2019-05-10 | 广东工业大学 | A kind of preparation method of activating solution and preparation method and carbon fibre composite |
| CN113151811A (en) * | 2021-04-13 | 2021-07-23 | 赤壁市聚茂新材料科技有限公司 | Non-palladium activated nickel plating solution and nickel plating method |
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Application publication date: 20110406 |