CN103233212A - Method for plating nickel-copper-phosphorus ternary alloy on wood surface - Google Patents
Method for plating nickel-copper-phosphorus ternary alloy on wood surface Download PDFInfo
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- CN103233212A CN103233212A CN2013101844417A CN201310184441A CN103233212A CN 103233212 A CN103233212 A CN 103233212A CN 2013101844417 A CN2013101844417 A CN 2013101844417A CN 201310184441 A CN201310184441 A CN 201310184441A CN 103233212 A CN103233212 A CN 103233212A
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- ternary alloy
- nickel
- wood
- phosphorus ternary
- chemical plating
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Abstract
The invention provides a method for plating a nickel-copper-phosphorus ternary alloy on a wood surface and relates to a method of chemical plating on the wood surface. The method provided by the invention aims to solve the problems of complex process of the existing chemical plating on the wood surface, low bonding strength between the coating and the wood layer and poor corrosion resistance. The method for plating the nickel-copper-phosphorus ternary alloy on the wood surface comprises the following steps of: 1, preparing a reducing agent from a NaBH4 solution and a NaOH solution; 2, preparing a chemical plating solution from nickel sulfate, copper sulfate, sodium hypophosphite, trisodium citrate, ammonium acetate and ammonia water; regulating the pH of the system to the range from 8 to 11 by using ammonia water, thus obtaining the chemical plating solution; and 3, immersing the wood in the reducing agent, then taking out and further immersing the wood in the chemical plating solution at a temperature ranging from 70 to 95 DEG C, thus obtaining the wood plated with the nickel-copper-phosphorus ternary alloy on the surface. The chemical plating process of the method provided by the invention is simple; the bonding strength between the coating and the wood layer can reach 4.387 MPa; and therefore, the corrosion performance of the wood is excellent.
Description
Technical field
The present invention relates to a kind of method of wood surface electroless plating.
Background technology
Electroless plating is a kind of process for treating surface, especially to matrix in irregular shape, can make the nonmetal substrate metallization, than being electroplate with better advantage, and the coating that obtains evenly, have mechanical property and decorate properties preferably, give material surface electroconductibility, capability of electromagnetic shielding and erosion resistance etc.
Traditional metal plating has the shortcoming that is difficult to overcome, and the electroconductibility of copper is very strong, but that metal level is easy in air is oxidized; Nickel plating is stable but erosion resistance is weaker.Because the Ni-Cu-P ternary alloy has better erosion resistance, thermostability, hardness, wear resistance and diamagnetism than Ni-P binary alloy, so get more and more people's extensive concerning.
For non-metallic material, its surface does not have catalyzer, so must activate before the plating, colloidal palladium (PdCl is generally adopted in traditional plating
2-SnCl
2) activation.Ma Meirong research plastic chemical plating Ni-Cu-P coating comprises following technical process: alkaline degreasing → high chromic acid content alligatoring → sodium sulfite solution reduction → HCl solution preimpregnation → colloidal palladium activation → NaOH solution dispergation → chemical plating Ni-Gu-P → drying → performance measurement.
But because PdCl
2The raw material costliness, and matrix easily adsorbs the inferior tin particle of one deck and influences the homogeneity of chemical plating, and the operation sequence complexity should not be controlled.In existing electroless plating ambrose alloy phosphorus technology, mainly exist metal and non-metallic layer bonding strength low, and formaldehyde, methyl alcohol and the hydrochloric acid etc. that use are poisonous, are not suitable for scale operation.
And at the patent No.: ZL200810064935.0, patent name: disclose a kind of method for preparing coating Ni-P in a kind of patent of method of wood surface chemical nickel plating, but the erosion resistance effect of coating is outstanding, causes application limited.
Summary of the invention
The present invention seeks in order to solve existing wood surface chemical plating technology complexity, coating and the lumber layer bonding strength is low and the problem of corrosion-resistant, and a kind of method of wood surface nickel-clad copper phosphorus ternary alloy is provided.
The method of wood surface nickel-clad copper phosphorus ternary alloy of the present invention follows these steps to realize:
One, reductive agent is by the NaBH of 2～7g/L
4The NaOH solution composition of solution and 1～6g/L;
Two, chemical plating solution is made up of the single nickel salt of 20～50g/L, the copper sulfate of 0.5～2.0g/L, the inferior sodium phosphate of 20～50g/L, the trisodium citrate of 30～60g/L, ammonium acetate and the ammoniacal liquor of 20～50g/L, by pH to 8～11 of ammoniacal liquor regulation system;
Three, with timber pickling to reductive agent 3～8min, take out timber horizontal positioned 0.6～1.2min at room temperature, impregnated in 15～30min in 70～95 ℃ the chemical plating solution then, obtain the timber of plating nickel on surface copper phosphorus ternary alloy.
The present invention is immersed NaBH with timber
4Solution, and then being loaded with NaBH
4The timber of solution is positioned in the chemical plating solution, NaBH
4With the Ni in the chemical plating solution
2+Reaction generates Ni
0As catalytic active center, Ni under 70～95 ℃ temperature
2+And Cu
2+With reductive agent H
2PO
2 -Reaction, codeposition generates the Ni-Cu-P ternary alloy.
The used activation solution proportioning of the method for wood surface nickel-clad copper phosphorus ternary alloy of the present invention is easy, and activation and electroless plating are finished in same solution, and technology is simple, and coating and lumber layer bonding strength reach more than the 4.3MPa, and erosion resistance is good.
Description of drawings
Fig. 1 is that the timber of the plating nickel on surface copper phosphorus ternary alloy that obtains of embodiment one amplifies 200 times SEM Electronic Speculum figure;
Fig. 2 is that the timber of the plating nickel on surface copper phosphorus ternary alloy that obtains of embodiment one amplifies 500 times SEM Electronic Speculum figure;
Fig. 3 is that the timber of the plating nickel on surface copper phosphorus ternary alloy that obtains of embodiment one amplifies 1000 times SEM Electronic Speculum figure;
Fig. 4 is that the timber of the plating nickel on surface copper phosphorus ternary alloy that obtains of embodiment one amplifies 3000 times SEM Electronic Speculum figure;
Fig. 5 is the electromagnet shield effect figure of the timber of the plating nickel on surface copper phosphorus ternary alloy that obtains of embodiment one, a represents not plate the timber electromagnet shield effect of nickel-clad copper phosphorus ternary alloy, and b represents the timber electromagnet shield effect of the plating nickel on surface copper phosphorus ternary alloy that embodiment one obtains;
Fig. 6 is the timber coating surface resistivity of the plating nickel on surface copper phosphorus ternary alloy that obtains of embodiment one to embodiment four and the graph of a relation of pH;
Fig. 7 is the timber Tafel graphic representation of the plating nickel on surface copper phosphorus ternary alloy that obtains of embodiment one, embodiment three and embodiment four;
Fig. 8 is the timber XRD figure of the plating nickel on surface copper phosphorus ternary alloy that obtains of embodiment one to embodiment four;
Fig. 9 is the timber XPS analysis constitutional diagram of the plating nickel on surface copper phosphorus ternary alloy that obtains of embodiment one, embodiment three and embodiment four,
Represent nickel,
Represent copper,
Represent phosphorus.
Embodiment
Embodiment one: the method for present embodiment wood surface nickel-clad copper phosphorus ternary alloy follows these steps to realize:
One, reductive agent is by the NaBH of 2～7g/L
4The NaOH solution composition of solution and 1～6g/L;
Two, chemical plating solution is made up of the single nickel salt of 20～50g/L, the copper sulfate of 0.5～2.0g/L, the inferior sodium phosphate of 20～50g/L, the trisodium citrate of 30～60g/L, ammonium acetate and the ammoniacal liquor of 20～50g/L, by pH to 8～11 of ammoniacal liquor regulation system;
Three, with timber pickling to reductive agent 3～8min, take out timber horizontal positioned 0.6～1.2min at room temperature, impregnated in 15～30min in 70～95 ℃ the chemical plating solution then, obtain the timber of plating nickel on surface copper phosphorus ternary alloy.
Present embodiment influences plating speed by the concentration of regulating NaOH solution in the reductive agent, so that coating is very fast, more uniform deposition, its activation stage reaction is as follows:
2Ni
2++BH
4 -+2H
2O→2Ni
0+2H
2↑+BO
2 -+4H
+
2Cu
2++BH
4 -+2H
2O→2Cu
0+2H
2↑+BO
2 -+4H
+
And at the activation stage of electroless plating, by CuSO in the control chemical plating solution
4Concentration so that coating is even because too much Cu deposition can suppress the catalysis of nickel nuclear, reduce speed of response, influence follow-up self-catalyzed reaction.Use ammoniacal liquor to regulate the pH of chemical plating solution, by its with plating bath in nickel and the cupric ion complexing concentration of controlling free ion, the electropotential that impels two metals is to negative mobile and be tending towards close, realization Ni-Cu codeposition.Its autocatalysis elementary reaction is as follows:
2H
2PO
2 -+4OH
-+Ni
2+→2HPO
3 2-+2H
2O+Ni↓+H
2↑
2H
2PO
2 -+4OH
-+Cu
2+→2HPO
3 2-+2H
2O+Cu↓+H
2↑
2H
2PO
2 -+6H
++4H
-→4H
2O+2P↓+3H
2↑
Embodiment two: what present embodiment and embodiment one were different is that the step 1 reductive agent is by the NaBH of 4～6g/L
4The NaOH solution composition of solution and 1～3g/L.Other step and parameter are identical with embodiment one.
Embodiment three: what present embodiment was different with embodiment one or two is that the step 2 chemical plating solution is made up of the single nickel salt of 23～35g/L, the copper sulfate of 0.5～1.5g/L, the inferior sodium phosphate of 30～45g/L, the trisodium citrate of 40～55g/L, ammonium acetate and the ammoniacal liquor of 25～40g/L.Other step and parameter are identical with embodiment one or two.
Embodiment four: present embodiment is different with one of embodiment one to three is pH to 8.5～10 by the ammoniacal liquor regulation system.Other step and parameter are identical with one of embodiment one to three.
Embodiment five: present embodiment is different with one of embodiment one to three is pH to 9.5 by the ammoniacal liquor regulation system.Other step and parameter are identical with one of embodiment one to three.
Embodiment six: present embodiment is different with one of embodiment one to five is that step 3 impregnated in 15～30min in 83～93 ℃ the chemical plating solution.Other step and parameter are identical with one of embodiment one to five.
Embodiment seven: what present embodiment was different with one of embodiment one to six is that the used timber of step 3 is birch veneer.Other step and parameter are identical with one of embodiment one to six.
Embodiment one: the method for present embodiment wood surface nickel-clad copper phosphorus ternary alloy follows these steps to realize:
One, reductive agent is by the NaBH of 5g/L
4The NaOH solution composition of solution and 2g/L;
Two, chemical plating solution is made up of the single nickel salt of 30g/L, the copper sulfate of 1g/L, the inferior sodium phosphate of 40g/L, the trisodium citrate of 50g/L, ammonium acetate and the ammoniacal liquor of 35g/L, by the pH to 9.5 of ammoniacal liquor regulation system;
Three, with timber pickling to reductive agent 5min, take out timber horizontal positioned 1min at room temperature, impregnated in 20min in 90 ℃ the chemical plating solution then, obtain the timber of plating nickel on surface copper phosphorus ternary alloy.
The SEM Electronic Speculum figure that the timber amplification of the plating nickel on surface copper phosphorus ternary alloy that present embodiment obtains is 200 times as shown in Figure 1; Amplify 500 times SEM Electronic Speculum figure as shown in Figure 2; Amplify 1000 times SEM Electronic Speculum figure as shown in Figure 3; Amplify 3000 times SEM Electronic Speculum figure as shown in Figure 4.
The wood utilization vertical pulling method of the plating nickel on surface copper phosphorus ternary alloy that present embodiment is obtained is measured the bonding strength between coating and the birch veneer, and the bonding strength that records between coating and the timber can reach 4.387MPa.
The electromagnet shield effect figure of the timber of the plating nickel on surface copper phosphorus ternary alloy that present embodiment obtains as shown in Figure 5, as can be seen from Figure 5 when electromagnetic frequency when 9KHz changes to 1.5GHz, electromagnet shield effect on average is higher than 60dB.
Embodiment two: present embodiment and embodiment one are different is pH to 8.5 by the ammoniacal liquor regulation system, obtains chemical plating solution.Other step and parameter are identical with embodiment one.
Embodiment three: present embodiment and embodiment one are different is pH to 9.0 by the ammoniacal liquor regulation system, obtains chemical plating solution.Other step and parameter are identical with embodiment one.
Embodiment four: present embodiment and embodiment one are different is pH to 10 by the ammoniacal liquor regulation system, obtains chemical plating solution.Other step and parameter are identical with embodiment one.
The timber coating surface resistivity of the plating nickel on surface copper phosphorus ternary alloy that embodiment one to embodiment four obtains and the graph of a relation of pH as shown in Figure 6, as shown in Figure 6 when the pH=8.5 of ammoniacal liquor regulation system, surface resistivity R=981.6m Ω/cm
2; During pH=9.0, surface resistivity R=639.8m Ω/cm
2; During pH=9.5, surface resistivity R=408.1m Ω/cm
2; During pH=10.0, surface resistivity R=377.4m Ω/cm
2
The timber Tafel curve of the plating nickel on surface copper phosphorus ternary alloy that embodiment one, embodiment three and embodiment four obtain as shown in Figure 7, test result sees Table 1;
Table 1
The XRD figure of the timber of the plating nickel on surface copper phosphorus ternary alloy that embodiment one to embodiment four obtains as shown in Figure 8; ° be typical wood-cellulose peak in 2 θ=22.18,2 θ=44.52 ° are the peaks of Ni (111), as can be seen from Figure 8 along with pH raises, cellulosic peak more and more a little less than, the peak of Ni (111) is more and more sharp-pointed, shown that coating is worth increase to become thicker with pH, crystal formation gradually becomes the crystallite attitude from non-crystalline state.
The timber XPS analysis constitutional diagram of the plating nickel on surface copper phosphorus ternary alloy that embodiment one, embodiment three and embodiment four obtain as shown in Figure 9, from then on figure increases along with pH as can be known, nickel content raises gradually, copper and phosphorus content reduce.
Claims (7)
1. the method for a wood surface nickel-clad copper phosphorus ternary alloy is characterized in that the method for wood surface nickel-clad copper phosphorus ternary alloy follows these steps to realize:
One, reductive agent is by the NaBH of 2～7g/L
4The NaOH solution composition of solution and 1～6g/L;
Two, chemical plating solution is made up of the single nickel salt of 20～50g/L, the copper sulfate of 0.5～2.0g/L, the inferior sodium phosphate of 20～50g/L, the trisodium citrate of 30～60g/L, ammonium acetate and the ammoniacal liquor of 20～50g/L, by pH to 8～11 of ammoniacal liquor regulation system;
Three, with timber pickling to reductive agent 3～8min, take out timber horizontal positioned 0.6～1.2min at room temperature, impregnated in 15～30min in 70～95 ℃ the chemical plating solution then, obtain the timber of plating nickel on surface copper phosphorus ternary alloy.
2. the method for a kind of wood surface nickel-clad copper phosphorus ternary alloy according to claim 1 is characterized in that the step 1 reductive agent is by the NaBH of 4～6g/L
4The NaOH solution composition of solution and 1～3g/L.
3. the method for a kind of wood surface nickel-clad copper phosphorus ternary alloy according to claim 1 is characterized in that the step 2 chemical plating solution is made up of the single nickel salt of 23～35g/L, the copper sulfate of 0.5～1.5g/L, the inferior sodium phosphate of 30～45g/L, the trisodium citrate of 40～55g/L, ammonium acetate and the ammoniacal liquor of 25～40g/L.
4. the method for a kind of wood surface nickel-clad copper phosphorus ternary alloy according to claim 1 is characterized in that pH to 8.5～10 by the ammoniacal liquor regulation system.
5. the method for a kind of wood surface nickel-clad copper phosphorus ternary alloy according to claim 4 is characterized in that the pH to 9.5 by the ammoniacal liquor regulation system.
6. the method for a kind of wood surface nickel-clad copper phosphorus ternary alloy according to claim 1 is characterized in that step 3 impregnated in 15～30min in 83～93 ℃ the chemical plating solution.
7. according to the method for each described a kind of wood surface nickel-clad copper phosphorus ternary alloy of claim 1 to 6, it is characterized in that the used timber of step 3 is birch veneer.
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|---|---|---|---|
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104947092A (en) * | 2015-07-22 | 2015-09-30 | 东北林业大学 | Preparation method of corrosion-resisting high-conductivity wood electromagnetic shielding material |
| CN109986665A (en) * | 2019-04-04 | 2019-07-09 | 南京林业大学 | A kind of high conductivity high-flexibility nickel plating wood chip and preparation method thereof |
| CN110484899A (en) * | 2019-09-19 | 2019-11-22 | 东莞市通科电子有限公司 | A kind of chemical nickel-plating liquid and its nickel plating technology for electronic component pin nickel plating |
| CN115003848A (en) * | 2020-01-24 | 2022-09-02 | 蒂森克虏伯钢铁欧洲股份公司 | Steel component with a manganese-containing corrosion protection coating |
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| CN102363879A (en) * | 2011-11-15 | 2012-02-29 | 东北林业大学 | Surface chemical copper plating method for wood |
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2013
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104947092A (en) * | 2015-07-22 | 2015-09-30 | 东北林业大学 | Preparation method of corrosion-resisting high-conductivity wood electromagnetic shielding material |
| CN104947092B (en) * | 2015-07-22 | 2017-12-19 | 东北林业大学 | A kind of preparation method of corrosion resistant highly conductive wooden electromagnetic screen material |
| CN109986665A (en) * | 2019-04-04 | 2019-07-09 | 南京林业大学 | A kind of high conductivity high-flexibility nickel plating wood chip and preparation method thereof |
| CN110484899A (en) * | 2019-09-19 | 2019-11-22 | 东莞市通科电子有限公司 | A kind of chemical nickel-plating liquid and its nickel plating technology for electronic component pin nickel plating |
| CN115003848A (en) * | 2020-01-24 | 2022-09-02 | 蒂森克虏伯钢铁欧洲股份公司 | Steel component with a manganese-containing corrosion protection coating |
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Application publication date: 20130807 |