CN102041492A - Method for carrying out surface modification on plating layer of chemical-plating nickel-cobalt-ferrum alloy fabric by utilizing rare-earth metal salt - Google Patents
Method for carrying out surface modification on plating layer of chemical-plating nickel-cobalt-ferrum alloy fabric by utilizing rare-earth metal salt Download PDFInfo
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Abstract
The invention relates to a method for carrying out surface modification on a plating layer of a chemical-plating nickel-cobalt-ferrum alloy fabric by utilizing a rare-earth metal salt, comprising a plating solution preparation method and a chemical-plating treatment method for the surface of the fabric. The main salts for chemical plating is Ni (nickel)-Co (cobalt)-Fe (ferrum)-P (phosphorus), rare-earth metal salt is cerous nitrate, cerous sulfate, lanthanum chloride, lanthanum nitrate or yttrium nitrate, and serves as an additive, and the added amount is 0.2g/L-0.6g/L. A reducing agent is sodium hypophosphite, borane or formaldehyde; a complexing agent is sodium potassium tartrate, sodium citrate or hydroxyl carboxylate; a stabilizing agent is maleic acid or thiocarbamide and derivatives thereof; and a buffering agent is ammonium sulfate or ammonium chloride. The chemical-plating treatment method for the surface of the fabric comprises the steps: oil removing, roughening, sensitizing, activating, decolliding, reducing, chemically plating and drying. Compared with the prior art, the method has the advantages that the operation is simple, the cost is low, the obtained material is light in weight, the corrosion is resistant, and the electromagnetic shielding performance is good.
Description
Technical field
The invention belongs to electroless plating and fabric surface treatments technical field, relate to the method that a kind of coating that utilizes rare earth metal salt pair chemical nickel plating ferro-cobalt polyester piece good carries out surface modification.
Background technology
Purpose at fabric face metal refining coating is for anti-electromagnetic-radiation and protection against corrosion.At present, electroless plating method is in one of main method of polyester piece good surface deposition metal, utilizes this method can be at polyester piece good surface deposition one deck, multiple layer metal or alloy layer.Adopt polyster fibre cloth as the matrix of implementing chemical plating metal, the electromagnetic shielding weaving face fabric of preparing can keep the original softness of fabric, frivolous, gas-pervious characteristic, has also that plated film is thin, a metal strong adhesion, characteristics that capability of electromagnetic shielding is good.In the prior art before the present invention, the multilayer deposition preparation can be referring to " sufacing " 2008 the 37th volumes the 2nd phase 21-22 page or leaf; The alloy deposition preparation method can be referring to " functional materials " 2009 the 10th volumes the 40th phase 1626-1628 page or leaf.But, the electromagnetic shielding polyester piece good of method for preparing, metal plating is skewness on fiber, and the coating degree that becomes more meticulous is not high, causes capability of electromagnetic shielding and corrosion resistance nature to be affected.(referring to Fig. 1).
Summary of the invention
At above-mentioned prior art situation, the objective of the invention is to, a kind of surface modification effect that utilizes rare earth metal salt is provided, improve become more meticulous degree and improve the method for electromagnet shield effect of chemical nickel plating ferro-cobalt fabric coating surface, can not only make the coating surface metal deposition fine and close more, even, and the magnetic property of raising coating, strengthen the anti-electromagnetic-radiation ability.
Now design of the present invention and technical solution are described below:
The effect of rare earth mainly shows refinement crystalline structure structure, and harmful element content in purification and the reduction metallic substance improves high temperature corrosion agent resistance of oxidation and reaches aspects such as metallic surface modifications.In addition, rare earth also has good magnetic, can produce bigger influence to electromagnetic radiation, so both required corrosion-resistantly at some, requires the field of electromagnetic protection again, and rare earth has wide application space.
The present invention utilizes rare earth metal salt pair fabric coating to carry out surface modifying method, implements electroless plating at fabric face, it is characterized in that: comprise the surface chemical plating treatment process of plating bath compound method and fabric, concrete steps are described as follows respectively:
1, plating bath compound method:
Step 1: accurately take by weighing electroless plating master's salt, reductive agent, complexing agent, stablizer, the additive of calculated amount, use a small amount of distilled water or deionized water dissolving respectively;
Step 2:, under constantly stirring, pour in the solution of complexing agent with consoluet electroless plating master's salts solution;
Step 3: in the solution of above-mentioned complexing agent, inject the additive rare earth metal salt solutions, more consoluet reductant solution is injected this solution after the stirring;
Step 4: respectively buffer reagent, stabiliser solution are poured under fully stirring set by step in 3 solution that prepare;
Step 5: be diluted to volume calculated with distilled water or deionized water;
Step 6: the dilute solution with acid or alkali is regulated the pH value;
Step 7: careful filtering solution;
Step 8: sample examination, carry out plating after qualified.
The present invention further provides a kind of rare earth metal salt pair fabric coating and carry out plating bath compound method in the surface modifying method, it is characterized in that: described electroless plating master's salt is Ni nickel-Co cobalt-Fe iron-P phosphorus, it is the electroless plating basic components, rare earth metal salt cerous nitrate, cerous sulfate, Lanthanum trichloride, lanthanum nitrate or Yttrium trinitrate are additives, and addition is 0.2g/L～0.6g/L.
The present invention further provides a kind of rare earth metal salt pair fabric coating and carry out plating bath compound method in the surface modifying method, it is characterized in that: described reductive agent is inferior sodium phosphate, borine or formaldehyde; Described complexing agent is Seignette salt, Trisodium Citrate or hydroxycarboxylate; Described stablizer is toxilic acid or thiocarbamide and derivative thereof; Described buffer reagent is ammonium sulfate or ammonium chloride.
The present invention further provides a kind of rare earth metal salt pair fabric coating and carry out plating bath compound method in the surface modifying method, it is characterized in that: the pH value of plating bath is 8.5～9.5, regulates with ammoniacal liquor.
2, fabric face electroless plating treatment process:
Step 1: oil removing; → step 2: alligatoring; → step 3: sensitization, activation; → step 4: dispergation; → step 5: reduction; → step 6: electroless plating; → step 7: oven dry.
The present invention further provides a kind of rare earth metal salt pair fabric coating and carry out fabric face electroless plating treatment process in the surface modifying method, it is characterized in that: described deoiling step 1 is meant removes fabric residual oil stain and spot in manufacturing processed; Described degreaser is sodium hydroxide 10～30g/L, tensio-active agent 3～8ml/L; The oil removing process condition is: under 30～70 ℃ of conditions, and oil removing ultrasonic oscillation 20～40 minutes;
The present invention further provides a kind of rare earth metal salt pair fabric coating and carry out fabric face electroless plating treatment process in the surface modifying method, it is characterized in that: described alligatoring step 2 is to instigate fabric to be formed with to be beneficial to the sunk surface that metal plating adheres to, and the alligatoring agent is the sodium hydroxide of 150～200g/L; The processing condition of alligatoring are: under 60～100 ℃ of conditions, and ultrasonic oscillation 10～30 minutes;
The present invention further provides a kind of rare earth metal salt pair fabric coating and carry out fabric face electroless plating treatment process in the surface modifying method, it is characterized in that: described sensitization, activation step 3 are meant the chemical reducing agent that has reductive action with the fiber surface absorption after alligatoring of sensitizing agent tin chloride and activator Palladous chloride, make it to be formed with to be beneficial to the metal core that metal adheres to; , sensitization, activator be made up of the tin chloride of 15～20g/L, the Palladous chloride of 0.15～0.2g/L, the concentrated hydrochloric acid of 8～10mL/L, the sodium-chlor of 140～180g/L; Sensitization, activatory processing condition are for to soak 1～3 hour in 50～70 ℃ of sensitizations, activator;
The present invention further provides a kind of rare earth metal salt pair fabric coating and carry out fabric face electroless plating treatment process in the surface modifying method, it is characterized in that: described dispergation step 4 is meant divalence or the tetravalent tin ion with the dissolve with hydrochloric acid solution partial hydrolysis; Described dispergator is concentrated hydrochloric acid 80～120mL/L; Dispergation processing condition: under 30～50 ℃ of conditions, in dispergator, soaked 40～60 seconds;
The present invention further provides a kind of rare earth metal salt pair fabric coating and carry out fabric face electroless plating treatment process in the surface modifying method, it is characterized in that: described reduction step 5 is meant that Palladous chloride is reduced into gold belongs to Palladium attached to fabric face; Described reductive agent is the inferior sodium phosphate of 20～30g/L; Reducing process condition: at ambient temperature fabric was soaked in reductive agent 3～7 minutes.
The present invention further provides fabric face electroless plating treatment process, it is characterized in that: described electroless plating step 6 is meant that pretreated fabric substrate is put into the chemical plating fluid for preparing in advance according to plating bath compound method of the present invention carries out chemical plating metal; The temperature of chemistry plating metal is at 70～90 ℃, and regulating plating bath pH is 8.5～9.0, promptly obtains the Fabric composites of coated with uniform alloyed metal layer.
The inventive method is compared with prior art, simple to operate, doing body material with fabric carries out carrying out chemical plating metal on its surface after a series of pre-treatment in early stage, utilize the surface modification effect of rare earth nitrate, the refinement matrix metal, make metal level combine with fabric firmly, improve electromagnet shield effect.
Description of drawings
Fig. 1: (A) do not add the fabric face sem photograph of Rare-Earth Ce
Fig. 2: (B) the fabric face sem photograph of interpolation rare earth cerium Ce 0.2g/L
Fig. 3: (C) the fabric face sem photograph of interpolation rare earth cerium Ce 0.4g/L
Fig. 4: (D) the fabric face sem photograph of interpolation rare earth cerium Ce 0.6g/L
Fig. 5: rate of body weight gain is all the electromagnet shield effect correlation curve figure that added and do not add Rare-Earth Ce coating at 95% o'clock
Wherein: (A) do not add the electromagnet shield effect curve of rare earth cerium Ce;
(B) the electromagnet shield effect curve of interpolation rare earth cerium Ce 0.2g/L;
(C) the electromagnet shield effect curve of interpolation rare earth cerium Ce 0.4g/L;
(D) the electromagnet shield effect curve of interpolation rare earth cerium Ce 0.6g/L
Embodiment
Embodiment below in conjunction with concrete experiment is further described (referring to Fig. 2,3,4,5) to the inventive method.
Below be the embodiment of the invention is added different content in Electroless Plating Ni-Co-Fe-P basic components Ce (NO
3)
3Carry out the plating experiment, basic components sees Table 1.The rare earth addition is respectively 0.2g/L, 0.4g/L, 0.6g/L.
The prescription and the technology of table 1 Electroless Plating Ni-Co-Fe-P alloy electroplating bath
By the coating morphology after the field emission scanning electron microscope test as shown in Figure 1.As seen along with the interpolation of rare earth, the coating surface knob reduces, and it is fine and close, even, smooth more that coating becomes.
Under relatively more equal weightening finish, add rare earth and do not add rare earth coated electromagnet shield effect (SE:Shielding Effectiveness), test is an example with 4 kinds of composition samples that weightening finish is all about 95%, the test frequency range is 20MHz～1500MHz, the result as shown in Figure 2, the electromagnet shield effect of 4 kinds of heterogeneity coating is all along with the increase of frequency descends to some extent, the adding of Rare-Earth Ce can not change this general trend, but can improve the electromagnet shield effect of coating, and along with the increase of rare earth adding quantity, electromagnet shield effect also increases
Table 2 be rate of body weight gain about 110% but the different sample of Coating composition, under 35 ℃, be immersed in the surface ratio resistance result that some hrs records after waiting in the 5%NaCl solution.Prolongation along with soak time, not adding the coating surface of Rare-Earth Ce increases apparent in view than resistance value, the specimen surface that adds Rare-Earth Ce than resistance value increasing degree less than the sample that does not add Rare-Earth Ce, but along with the increase coating corrosion resistance nature of Rare-Earth Ce addition descends on the contrary to some extent, the surface ratio resistance value raises.
Table 2 rate of body weight gain is the specimen surface Corrosion results (Ω) about 110% all
Surface chemical plating process method step according to plating bath preparation of the present invention and fabric is handled specific as follows:
1, plating bath compound method:
Step 1: accurately take by weighing calculated amount electroless plating master salt single nickel salt 25g/L, ferrous sulfate 8g/L, cobalt chloride 10g/L, rare-earth salts 0.2g/L, reductive agent 35g/L, complexing agent 30g/L, buffer reagent 14g/L, dissolve with appropriate amount of deionized water respectively;
Step 2:, under constantly stirring, pour in the solution of complexing agent with consoluet 3 kinds of electroless plating master salts solutions;
Step 3: inject cerous nitrate solution, after the stirring consoluet reductant solution is injected 2 solution that prepare set by step;
Step 4: respectively buffer agent solution is poured under fully stirring set by step in 3 solution that prepare;
Step 5: use the deionized water diluting soln;
Step 6: regulate pH value to 9.0 with ammoniacal liquor, simultaneously solution is formulated as 1L;
Step 7: careful filtering solution;
Step 8: sample examination, carry out plating after qualified.
2, the fabric face electroless plating is handled:
Step 1: oil removing: degreaser sodium hydroxide 25g/L, tensio-active agent 5ml/L, under 30～70 ℃ of conditions, oil removing ultrasonic oscillation 30 minutes;
Step 2: alligatoring: alligatoring agent sodium hydroxide 200g/L, 80 ℃ of alligatoring ultrasonic oscillations 20 minutes;
Step 3: sensitization, activation: with sensitization, the activator of Palladous chloride 0.15g/L, concentrated hydrochloric acid 10mL/L, tin protochloride 15g/L, sodium-chlor 140g/L preparation, sensitization under 60 ℃ of conditions, activation 2 hours;
Step 4: dispergation: use concentrated hydrochloric acid 100mL/L, under 50 ℃ of conditions, soaked 1 minute;
Step 5: reduction: use inferior sodium phosphate 20g/L, soaking at room temperature 5 minutes.
Step 6: electroless plating: pretreated terylene base material is put into the chemical plating fluid for preparing in advance, and at 90 ℃, pH is that pH carried out chemical plating metal at 9.0 o'clock, promptly obtains the polyester piece good matrix material of coated with uniform alloyed metal layer.
Step 7: the polyester piece good matrix material that obtains coated with uniform layer of metal alloy after the oven dry.
Claims (10)
1. utilize rare earth metal salt pair fabric coating to carry out surface modifying method, implement electroless plating, comprise the surface chemical plating treatment process of plating bath compound method and fabric, it is characterized in that at fabric face:
Described plating bath compound method concrete steps are as follows:
Step 1: accurately take by weighing electroless plating master's salt, reductive agent, complexing agent, stablizer, the additive of calculated amount, use a small amount of distilled water or deionized water dissolving respectively;
Step 2:, under constantly stirring, pour in the solution of complexing agent with consoluet electroless plating master's salts solution;
Step 3: in the solution of above-mentioned complexing agent, inject the additive rare earth metal salt solutions, more consoluet reductant solution is injected this solution after the stirring;
Step 4: respectively buffer reagent, stabiliser solution are poured under fully stirring set by step in 3 solution that prepare;
Step 5: be diluted to volume calculated with distilled water or deionized water;
Step 6: the dilute solution with acid or alkali is regulated the pH value;
Step 7: careful filtering solution;
Step 8: sample examination, carry out plating after qualified.
Described fabric face electroless plating treatment process concrete steps are as follows:
Step 1: oil removing; → step 2: alligatoring; → step 3: sensitization, activation; → step 4: dispergation; → step 5: reduction; → step 6: electroless plating; → step 7: oven dry.
2. the rare earth metal salt pair fabric coating that utilizes according to claim 1 carries out surface modifying method, it is characterized in that: the electroless plating master's salt in the described plating bath compound method is Ni nickel-Co cobalt-Fe iron-P phosphorus, it is the electroless plating basic components, rare earth metal salt cerous nitrate, cerous sulfate, Lanthanum trichloride, lanthanum nitrate or Yttrium trinitrate are additives, and addition is 0.2g/L～0.6g/L.
3. carry out surface modifying method according to claim 1 or 2 arbitrary described rare earth metal salt pair fabric coating that utilize, it is characterized in that: the reductive agent in the described plating bath compound method is inferior sodium phosphate, borine or formaldehyde; Complexing agent in the described plating bath compound method is Seignette salt, Trisodium Citrate or hydroxycarboxylate; Stablizer in the described plating bath compound method is toxilic acid or thiocarbamide and derivative thereof; Buffer reagent in the described plating bath compound method is ammonium sulfate or ammonium chloride.
4. carry out surface modifying method according to the arbitrary described rare earth metal salt pair fabric coating that utilizes of claim 1～3, it is characterized in that: the pH value of plating bath is 8.5～9.5, regulates with ammoniacal liquor.
5. the rare earth metal salt pair fabric coating that utilizes according to claim 1 carries out surface modifying method, it is characterized in that: the deoiling step 1 in the described fabric face electroless plating treatment process is meant removes fabric residual oil stain and spot in manufacturing processed; Described degreaser is sodium hydroxide 10～30g/L, tensio-active agent 3～8ml/L; The oil removing process condition is: under 30～70 ℃ of conditions, and oil removing ultrasonic oscillation 20～40 minutes;
6. carry out surface modifying method according to claim 1,5 arbitrary described rare earth metal salt pair fabric coating that utilize, it is characterized in that: the alligatoring step 2 in the described fabric face electroless plating treatment process is to instigate fabric to be formed with to be beneficial to the sunk surface that metal plating adheres to, and the alligatoring agent is the sodium hydroxide of 150～200g/L; The processing condition of alligatoring are: under 60～100 ℃ of conditions, and ultrasonic oscillation 10～30 minutes;
7. carry out surface modifying method according to claim 1,6 arbitrary described rare earth metal salt pair fabric coating that utilize, it is characterized in that:: sensitization, the activation step 3 in the described fabric face electroless plating treatment process is meant the chemical reducing agent that has reductive action with the fiber surface absorption after alligatoring of sensitizing agent tin chloride and activator Palladous chloride, makes it to be formed with to be beneficial to the metal core that metal adheres to; , sensitization, activator be made up of the tin chloride of 15～20g/L, the Palladous chloride of 0.15～0.2g/L, the concentrated hydrochloric acid of 8～10mL/L, the sodium-chlor of 140～180g/L; Sensitization, activatory processing condition are for to soak 1～3 hour in 50～70 ℃ of sensitizations, activator;
8. carry out surface modifying method according to claim 1,7 arbitrary described rare earth metal salt pair fabric coating that utilize, it is characterized in that: the dispergation step 4 in the described fabric face electroless plating treatment process is meant divalence or the tetravalent tin ion with the dissolve with hydrochloric acid solution partial hydrolysis; Described dispergator is concentrated hydrochloric acid 80～120mL/L; Dispergation processing condition: under 30～50 ℃ of conditions, in dispergator, soaked 40～60 seconds;
9. carry out surface modifying method according to claim 1,8 arbitrary described rare earth metal salt pair fabric coating that utilize, it is characterized in that: the reduction step 5 in the described fabric face electroless plating treatment process is meant that Palladous chloride is reduced into gold belongs to Palladium attached to fabric face; Described reductive agent is the inferior sodium phosphate of 20～30g/L; Reducing process condition: at ambient temperature fabric was soaked in reductive agent 3～7 minutes.
10. carry out surface modifying method according to claim 1,9 arbitrary described rare earth metal salt pair fabric coating that utilize, it is characterized in that: the electroless plating step 6 in the described fabric face electroless plating treatment process is meant that pretreated fabric substrate is put into the chemical plating fluid for preparing in advance according to plating bath compound method of the present invention carries out chemical plating metal; The temperature of chemistry plating metal is at 70～90 ℃, and regulating plating bath pH is 8.5～9.0, promptly obtains the Fabric composites of coated with uniform alloyed metal layer.
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Application publication date: 20110504 |