CN115852679A - Method for realizing copper-nickel double-layer chemical plating by silk fabric iron activation method - Google Patents
Method for realizing copper-nickel double-layer chemical plating by silk fabric iron activation method Download PDFInfo
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 93
- 239000004744 fabric Substances 0.000 title claims abstract description 79
- 238000000034 method Methods 0.000 title claims abstract description 55
- 238000007747 plating Methods 0.000 title claims abstract description 54
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 52
- 229910000570 Cupronickel Inorganic materials 0.000 title claims abstract description 31
- YOCUPQPZWBBYIX-UHFFFAOYSA-N copper nickel Chemical compound [Ni].[Cu] YOCUPQPZWBBYIX-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 230000004913 activation Effects 0.000 title claims description 83
- 239000000126 substance Substances 0.000 title claims description 30
- 239000000243 solution Substances 0.000 claims abstract description 29
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 28
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229910052700 potassium Inorganic materials 0.000 claims abstract description 22
- 239000011591 potassium Substances 0.000 claims abstract description 22
- 230000008569 process Effects 0.000 claims abstract description 18
- 229960002089 ferrous chloride Drugs 0.000 claims abstract description 17
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 claims abstract description 17
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 14
- 229920001690 polydopamine Polymers 0.000 claims abstract description 14
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910052802 copper Inorganic materials 0.000 claims abstract description 12
- 239000010949 copper Substances 0.000 claims abstract description 12
- -1 iron ions Chemical class 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 6
- 230000010355 oscillation Effects 0.000 claims abstract description 6
- 238000002791 soaking Methods 0.000 claims abstract description 6
- 230000003197 catalytic effect Effects 0.000 claims abstract description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 21
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 16
- 238000005406 washing Methods 0.000 claims description 15
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 239000000843 powder Substances 0.000 claims description 10
- LENZDBCJOHFCAS-UHFFFAOYSA-N tris Chemical compound OCC(N)(CO)CO LENZDBCJOHFCAS-UHFFFAOYSA-N 0.000 claims description 9
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 claims description 8
- 239000003381 stabilizer Substances 0.000 claims description 8
- 239000007983 Tris buffer Substances 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- ZGTMUACCHSMWAC-UHFFFAOYSA-L EDTA disodium salt (anhydrous) Chemical compound [Na+].[Na+].OC(=O)CN(CC([O-])=O)CCN(CC(O)=O)CC([O-])=O ZGTMUACCHSMWAC-UHFFFAOYSA-L 0.000 claims description 4
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 4
- 239000004471 Glycine Substances 0.000 claims description 4
- 241000080590 Niso Species 0.000 claims description 4
- 125000000896 monocarboxylic acid group Chemical group 0.000 claims description 4
- BHZOKUMUHVTPBX-UHFFFAOYSA-M sodium acetic acid acetate Chemical compound [Na+].CC(O)=O.CC([O-])=O BHZOKUMUHVTPBX-UHFFFAOYSA-M 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 4
- 230000009920 chelation Effects 0.000 claims 1
- 238000002360 preparation method Methods 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 3
- 238000004140 cleaning Methods 0.000 abstract description 2
- 238000007772 electroless plating Methods 0.000 abstract description 2
- 239000012670 alkaline solution Substances 0.000 abstract 1
- 238000001994 activation Methods 0.000 description 76
- 238000000151 deposition Methods 0.000 description 12
- 230000008021 deposition Effects 0.000 description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 238000001465 metallisation Methods 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 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 2
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 239000013522 chelant Substances 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 229910017052 cobalt Inorganic materials 0.000 description 2
- 239000010941 cobalt Substances 0.000 description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 2
- 239000008139 complexing agent Substances 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 229910001379 sodium hypophosphite Inorganic materials 0.000 description 2
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 229910001429 cobalt ion Inorganic materials 0.000 description 1
- XLJKHNWPARRRJB-UHFFFAOYSA-N cobalt(2+) Chemical compound [Co+2] XLJKHNWPARRRJB-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229940078494 nickel acetate Drugs 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000012279 sodium borohydride Substances 0.000 description 1
- 229910000033 sodium borohydride Inorganic materials 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
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Abstract
The method comprises the steps of taking a silk fabric as a base material, firstly placing the fabric into a prepared polydopamine solution for standing for 24 hours, then cleaning and drying the fabric, then placing the fabric into a ferrous chloride solution with the concentration of 35-45 g/L for soaking for 5 minutes, chelating and adsorbing iron ions, applying ultrasonic wave for assisting oscillation for 2 minutes in the process, then placing the fabric into an alkaline solution of potassium borohydride with the concentration of 4-5 g/L for reducing the iron ions on the fabric for 5-15 minutes to obtain elemental iron with catalytic activity, carrying out electroless copper plating on the elemental iron, carrying out electroless nickel plating on the copper-plated fabric by adopting the method, and finally successfully realizing copper-nickel double-layer electroless plating on the silk fabric.
Description
Technical Field
The invention relates to a pretreatment activation process for electroless copper plating and nickel plating on silk fabric, belonging to the field of chemical plating.
Background
The surface of the metallized fabric can have electromagnetic shielding performance so as to resist the harm of electromagnetic waves to human bodies, for example, people working in special environments and pregnant women need to wear the fabric with the electromagnetic shielding performance, and silk is used as a high-performance textile material and has the characteristics of skin friendliness, softness and the like. The nickel has magnetism absorption, electromagnetic waves generate magnetic loss through the nickel layer, the metal copper has good conductivity, the surface of the fabric after the copper-nickel double-layer chemical plating can be provided with a metal layer with a gradient structure to achieve good electromagnetic shielding performance, and at present, the research on double-layer metallization on the surface of the silk fabric is less.
Chemical plating is used as an excellent surface metallization treatment technology, most activation methods adopted by chemical copper plating and nickel plating adopt precious metals, such as palladium activation or silver activation, the activation method is high in cost and harmful to the environment, an activation method for promoting nickel acetate and sodium hypophosphite to react at high temperature to generate a nickel elementary substance to form an autocatalytic activation center for chemical nickel plating is researched, but the activation method is not suitable for high-temperature-resistant materials such as fabric, an activation method for reducing cobalt ions by sodium borohydride to obtain elementary substance cobalt is researched, however, cobalt is still a heavy metal which can generate adverse effects on the environment, chinese patent No. 101096756A discloses an iron activation method for chemical nickel plating, trivalent iron is reduced by sodium hypophosphite, but experiments find that the activation effect is not ideal when the method is applied to fabric, the fabric surface cannot be plated completely, and the plating binding force is poor.
Disclosure of Invention
The invention provides a novel pretreatment activation process for chemically plating copper and nickel on silk fabric, which saves cost, has no harm to the environment, does not need high temperature condition and has good bonding force.
In order to solve the problems, the activating solution adopted by the invention comprises the following components: ferrous chloride solution with the concentration of 35-45 g/L, potassium borohydride solution with the concentration of 4-5 g/L and potassium hydroxide with the concentration of 0.8-1.5 g/L. Firstly, silk fabric modified by polydopamine is put into ferrous chloride solution to chelate iron ions so as to adsorb more iron ions, the iron ions are infiltrated into the pores of the fabric under the action of ultrasonic oscillation and are uniformly adsorbed, the ultrasonic oscillation time is 2min and the power is 80w, then alkaline potassium borohydride solution is used for reducing the iron ions on the surface of the fabric to obtain an iron simple substance with the activation capacity, the activation time is 5-15 min, the activation temperature is 30-40 ℃, then chemical copper-nickel plating is carried out, double-layer metallization on the silk fabric is realized, and a plating layer on the surface of the silk fabric modified by polydopamine does not fall off or peel after being repeatedly bent, so that good binding force is shown.
The silk fabric iron activation method for realizing copper-nickel double-layer chemical plating comprises the following steps: deoiling → washing → degumming → washing → coarsening → washing → polydopamine modification → washing → iron activation → washing → electroless copper plating → washing → iron activation → washing → electroless nickel plating → washing → drying.
The silk fabric iron activation method realizes copper-nickel double-layer chemical plating, absolute ethyl alcohol is adopted in the oil removing step, naOH 4g/L is adopted for glue removal, the time is 15min at the temperature of 50 ℃, and sodium carbonate 20g/L can be adopted for glue removal at the temperature of 65 ℃ for 30 min.
The silk fabric iron activation method realizes copper-nickel double-layer chemical plating, and the coarsening process comprises the steps of dissolving 30g/L hydrochloric acid and 50g/L acetic acid in a mixed solution of distilled water and ethanol with the volume ratio of 1.
The silk fabric iron activation method realizes copper-nickel double-layer chemical plating, and the modification process of polydopamine comprises the following steps: firstly weighing Tris (Tris-hydroxymethyl-aminomethane) powder, adding the Tris powder into deionized water to prepare a solution of 2.8g/L, adding polydopamine hydrochloride powder at the concentration of 4g/L, then adjusting the pH value to 8.5 with hydrochloric acid, soaking the coarsened fabric into the solution, standing at room temperature for 24 hours, then washing with deionized water, and then drying in an oven at 45 ℃.
The silk fabric iron activation method realizes copper-nickel double-layer chemical plating, and the copper plating formula and the process conditions adopted by the activation method are CuSO 4 ∙5H 2 O 16 g/L，NaKC 4 H 4 O 6 14g/L of EDTA-2Na 20g/L, 15g/L of NaOH, 12ml/L of HCHO, trace amount of stabilizer, temperature of 30-40 ℃ and time of 45min.
The silk fabric iron activation method realizes copper-nickel double-layer chemical plating, and the activation method adopts a nickel plating formula and process conditions as follows: niSO 4 ∙6H 2 O 28g/L，H 2 NCH 2 8g/L COOH (glycine), 15g/L HAC-NaAC (acetic acid-sodium acetate), naH 2 PO 2 ∙H 2 O30 g/L, stabilizer trace, temperature 80 ℃ and time 45min.
The washing step is to wash off organic solvent and residual impurities on the surface of the fabric, but the activated fabric should be properly washed with water to avoid the detachment of a large amount of elementary iron on the surface of the fabric due to excessive washing, and the coarsening is to generate pits on the surface of the fabric to provide a growth carrier for the attachment of subsequent activated particles and the deposition of a coating.
The invention has the following beneficial effects: the invention adopts polydopamine to modify the surface of the fabric, not only makes the surface of the matrix rougher, but also can chelate and adsorb iron ions, improves the uniformity and the bonding force of the silk fabric coating, has good reduction effect of potassium borohydride on the iron ions, improves the stability of potassium borohydride solution due to the addition of potassium hydroxide, is not easy to lose efficacy, and obviously excels in economy compared with other activation modes by taking iron as the activation method, and is environment-friendly and pollution-free.
Drawings
Fig. 1 is an original SEM image of silk fabric.
Fig. 2 is SEM image of silk fabric after activation.
FIG. 3 is SEM image of silk fabric after electroless copper plating.
FIG. 4 is SEM image of silk fabric after electroless copper-nickel plating.
Figure 5 is EDS image after silk fabric activation.
FIG. 6 is EDS picture after copper-nickel electroless plating of silk fabric.
Fig. 7 is a graph of electromagnetic shielding performance of silk fabric before and after chemical plating.
Detailed Description
The following description of specific operations and implementations of the invention is provided.
Example 1: the process flow of the silk fabric copper-nickel double-layer metal chemically plated by the iron activation method comprises the following steps: degreasing (absolute ethyl alcohol) → water washing → degumming (sodium hydroxide 4g/L,50 ℃,15 min) → water washing → coarsening (30 g/L hydrochloric acid, 50g/L acetic acid, dissolved in a mixed solution of distilled water and ethyl alcohol in a volume ratio of 1: weighing Tris (Tris (hydroxymethyl aminomethane) powder, adding the Tris powder into deionized water to prepare a solution of 2.8g/L, weighing 4g of polydopamine hydrochloride powder, adding the polydopamine hydrochloride powder into the solution, adjusting the pH value to 8.5 by using hydrochloric acid, soaking the coarsened fabric into the solution, standing at room temperature for 24 hours, washing by using deionized water, and drying in an oven at 45 ℃.
The specific operation mode of the silk fabric iron activation is as follows: firstly, clamping a silk fabric modified by polydopamine by using tweezers, putting the silk fabric into a beaker filled with 35-45 g/L ferrous chloride solution for soaking for 5min, applying ultrasonic wave for assisting oscillation for 2min in the process, fully penetrating iron ions into pores of the silk fabric, wherein the ultrasonic power is 80w, then taking out the fabric from the solution, putting the fabric into the beaker filled with alkaline potassium borohydride solution for reduction, and obtaining an iron simple substance with catalytic activity, wherein the activation time of the process is 5-15 min, and the activation temperature is 30-40 ℃, and the alkaline potassium borohydride is prepared in the following way: adding 0.8 to 1.5g of potassium hydroxide into a beaker, then adding deionized water until the solution is nearly 1L, stirring uniformly, finally adding 4 to 5g of potassium borohydride, and stirring uniformly again.
The copper plating formula and the process condition are CuSO 4 ∙5H 2 O 16g/L，NaKC 4 H 4 O 6 14g/L，EDTA-2Na 20g/L，NaOH 15g/L，12ml/L of HCHO, trace stabilizer, temperature of 30-40 ℃ and time of 45min, and the specific operation is as follows: firstly, naKC is added 4 H 4 O 6 14g/L EDTA-2Na 20g/L solution are mixed to form a compound complexing agent, and then CuSO is added in sequence 4 ∙5H 2 O16 g/L and NaOH 15g/L solution, adding reducing agent HCHO 12ml/L and stirring evenly, finally adding stabilizing agent, and placing the activated silk fabric in the solution for chemical copper plating.
The nickel plating formula and the process condition are NiSO 4 ∙6H 2 O 28g/L，H 2 NCH 2 8g/L of COOH (glycine), 15g/L of HAC-NaAC (acetic acid-sodium acetate), naH 2 PO 2 ∙H 2 O30 g/L, stabilizer trace, temperature of 80 ℃, time of 45min, and specific operations are as follows: firstly, H is 2 NCH 2 8g/L COOH (glycine) and 15g/L HAC-NaAC (acetic acid-sodium acetate) complexing agent, and then sequentially adding NiSO 4 ∙6H 2 O 28g/L，NaH 2 PO 2 ∙H 2 Adding 30g/L of O and a stabilizer, uniformly stirring every reagent in the process, cleaning and drying the copper-plated silk fabric, performing iron activation process treatment, and then putting the silk fabric into the nickel plating solution for chemical plating.
The surface appearance of the silk fabric in the main process stage of chemical plating is observed by utilizing a scanning electron microscope, as shown in figures 1, 2, 3 and 4, after the fabric is plated with copper-nickel chemically, the surface plating layer is uniform and compact, surface element components before and after the chemical plating of the silk fabric are analyzed by an energy spectrometer, as shown in figures 5 and 6, and in figure 5, the activated fabric surface contains more iron elements, and the iron active particles are attached to the fabric surface by combining figure 2, and figures 4 and 6 further prove that the activation method successfully realizes the copper-nickel double-layer chemical plating on the silk fabric, and from figure 7, the original silk fabric does not have electromagnetic shielding performance, after the copper-nickel is plated chemically, the electromagnetic shielding performance can reach 90 decibels in a broadband interval of 0.5-18 GHZ, and the technical requirements of military industry are met.
Taking the deposition rate of the copper plating layer as an evaluation index, and carrying out orthogonal tests on four factors, namely the ferrous chloride concentration (35-45 g/L), the potassium borohydride concentration (4-5 g/L), the activation time (5-15min) and the activation temperature (30-40 ℃), under the conditions of soaking time of 5min, ultrasonic-assisted oscillation time of 2min, power of 80w and potassium hydroxide concentration of 1 g/L.
Example 2: the surface of the silk fabric is plated with copper-nickel by an iron activation method, and the activation factors are as follows: 35g/L of ferrous chloride, 4g/L of potassium borohydride, 5min of activation time and 25/DEG C of activation temperature, and the rest conditions are the same as those in the example 1, and the obtained deposition rate is 6.31 mu m/h.
Example 3: the surface of the silk fabric is plated with copper-nickel by an iron activation method, and the activation factors are as follows: 35g/L of ferrous chloride, 4.5g/L of potassium borohydride, 10min of activation time, 30/DEG C of activation temperature, and the rest conditions are the same as those in example 1, and the obtained deposition rate is 6.65 mu m/h.
Example 4: the surface iron activation method for silk fabric is used for chemically plating copper-nickel, and the activation factors are as follows: 35g/L of ferrous chloride, 5g/L of potassium borohydride, 15min of activation time and 35/DEG C of activation temperature, and the rest conditions are the same as those in example 1, and the deposition rate is 6.63 mu m/h.
Example 5: the surface iron activation method for silk fabric is used for chemically plating copper-nickel, and the activation factors are as follows: 40g/L of ferrous chloride, 4g/L of potassium borohydride, 15min of activation time and 30/DEG C of activation temperature, and the rest conditions are the same as those in the example 1, and the obtained deposition rate is 7.23 mu m/h.
Example 6: the surface iron activation method for silk fabric is used for chemically plating copper-nickel, and the activation factors are as follows: 40g/L of ferrous chloride, 4.5g/L of potassium borohydride, 5min of activation time, 35/DEG C of activation temperature, and the rest conditions are the same as those of the example 1, and the deposition rate is 6.96 mu m/h.
Example 7: the surface iron activation method for silk fabric is used for chemically plating copper-nickel, and the activation factors are as follows: 40g/L of ferrous chloride, 5g/L of potassium borohydride, 10min of activation time, 25/DEG C of activation temperature and the same conditions as in example 1 are adopted, and the deposition rate is 7.21 mu m/h.
Example 8: the surface iron activation method for silk fabric is used for chemically plating copper-nickel, and the activation factors are as follows: 45g/L of ferrous chloride, 4g/L of potassium borohydride, 10min of activation time and 35/DEG C of activation temperature, and the rest conditions are the same as those in the example 1, and the deposition rate is 7.56 mu m/h.
Example 9: the surface iron activation method for silk fabric is used for chemically plating copper-nickel, and the activation factors are as follows: 45g/L of ferrous chloride, 4.5g/L of potassium borohydride, 15min of activation time, 25/DEG C of activation temperature and the same conditions as in example 1 are adopted, and the deposition rate is 7.13 mu m/h.
Example 10: the surface iron activation method for the silk fabric is used for chemically plating copper-nickel, and the activation factors are as follows: 45g/L of ferrous chloride, 5g/L of potassium borohydride, 5min of activation time and 30/DEG C of activation temperature, and the rest conditions are the same as those in example 1, and the deposition rate is 7.39 mu m/h.
From the above examples it can be seen that: the deposition rate of example 8 was 7.56 μm/h, which is a preferred example, i.e., the formulation and process conditions of the activation solution were: 45g/L ferrous chloride, 4g/L potassium borohydride, 1g/L potassium hydroxide, 10min activation time, 35 ℃ activation temperature, and the best mode of the invention is not limited thereto, and it is obvious to those skilled in the art that modifications and substitutions made in the claims are within the scope of the invention.
Claims (4)
1. The silk fabric iron activation method realizes copper-nickel double-layer chemical plating, and is characterized in that the process firstly modifies polydopamine to realize chelation of iron ions, and the preparation process of polydopamine solution comprises the following steps: weighing Tris (Tris-hydroxymethyl aminomethane) powder, adding the Tris powder into deionized water to prepare a solution of 2.8g/L, adding polydopamine hydrochloride powder at a concentration of 4g/L, adjusting the pH value of the solution to 8.5 with hydrochloric acid, soaking the coarsened fabric into the solution, standing at room temperature for 24 hours, washing with deionized water, drying in an oven at 45 ℃, and then performing iron activation and electroless copper-nickel plating.
2. The silk fabric iron activation method for realizing copper-nickel double-layer chemical plating according to claim 1, wherein the iron activation formula comprises the following components: 35-45 g/L of ferrous chloride, 4-5 g/L of potassium borohydride and 0.8-1.5 g/L of potassium hydroxide, and the process comprises the following steps: placing the silk fabric modified by polydopamine in a ferrous chloride solution for 5min, applying ultrasonic wave for assisting oscillation for 2min in the process, wherein the ultrasonic power is 80w, taking out the fabric from the solution, transferring the fabric to an alkaline potassium borohydride solution prepared from 4-5 g/L potassium borohydride and 0.8-1.5 g/L potassium hydroxide, and reducing iron ions for 5-15 min at the temperature of 30-40 ℃ to obtain the iron simple substance with catalytic activity.
3. The silk fabric iron activation method for realizing copper-nickel double-layer chemical plating according to claim 1, wherein the copper plating formula and process conditions adopted by iron activation are as follows: cuSO 4 ∙5H 2 O 16g/L，NaKC 4 H 4 O 6 14g/L of EDTA-2Na 20g/L, 15g/L of NaOH, 12ml/L of HCHO, trace amount of stabilizer, temperature of 30-40 ℃ and time of 45min.
4. The silk fabric iron activation method for realizing copper-nickel double-layer chemical plating according to claim 1, wherein the nickel plating formula and the process conditions adopted by iron activation are as follows: niSO 4 ∙6H 2 O 28g/L，H 2 NCH 2 8g/L of COOH (glycine), 15g/L of HAC-NaAC (acetic acid-sodium acetate), naH 2 PO 2 ∙H 2 30g/L of O, a trace amount of stabilizer, a temperature of 80 ℃ and a time of 45min.
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