CN101215693A - Method for preparing high-performance conductive fiber - Google Patents
Method for preparing high-performance conductive fiber Download PDFInfo
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- CN101215693A CN101215693A CNA2008100190509A CN200810019050A CN101215693A CN 101215693 A CN101215693 A CN 101215693A CN A2008100190509 A CNA2008100190509 A CN A2008100190509A CN 200810019050 A CN200810019050 A CN 200810019050A CN 101215693 A CN101215693 A CN 101215693A
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Abstract
The invention relates to a method for preparing a high performance conductive fiber, which comprises the following steps: V1ing, pretreatment and washing. V2ing, fiber is socked by coarsening agent to improve the surface structure of the fiber. V3ing, the fiber is socked by stannous chloride or cadmium chloride solution, and a layer of tin ions or cadmium ions are adsorbed on the surface of the fiber. V4ing, the fiber is socked by palladium chloride solution, and the tin ions or cadmium ions which are replaced by palladium colloid are adsorbed on the surface of the fiber. V5ing, electroless copper plating. V6ing, after being socked by oxalic acid solution, the fiber is dried. V7ing, the fiber which is plated with copper is socked and treated by tin dichloride solution. V8ing, the copper-plating fiber is socked by palladium chloride solution, and the tin ions or cadmium ions which are replaced by palladium colloid are adsorbed on the surface of the fiber. V9ing, chemical nickel plating. V10ing, after being socked by deionized water, the fiber is dried, and a product is obtained. The invention has small pollution to environment and less energy dissipation, and is easy to industrially produce. The conductive fiber which is prepared using the invention has excellent conductivity, the resistance of the specific surface area is 1-10 ohm, the original characteristics of the fiber is preserved, and the high performance conductive fiber is capable of being used for various non-woven fabrics.
Description
Technical field
The invention provides a kind of preparation method of high-performance conductive fiber, thereby this method is by making fiber have antistatic and radiation proof function at general fibre coating surface metallic conduction thin layer.
Background technology
The develop rapidly with scientific and technological level of improving constantly along with social productive forces, the modernization in city and industrialized process are also more and more faster, the problem of environmental pollution that brings thus is also outstanding day by day, the arrival in electrification epoch, making electromagnetic radiation pollution become water gradually pollutes, another source of pollution after the atmospheric pollution, sound pollution.Crisis and opportunity are also deposited, after the popularizing of electronic product, and the also corresponding birth of the product of various anti-electromagnetic shieldings.And as with people's daily life the closest wear clothing, become the primary object of research naturally, so various electro-conductive fiber with anti-capability of electromagnetic shielding constantly occurs.The present best metallic conduction fiber of conductivity, its preparation method mainly contains following several.1) traditional electro-plating method: this method need expend very big electric power resource, and contains cyanogen and electroplate very serious to the pollution of environment; 2, cyanideless electro-plating method: this method covering power and covering power all have much room for improvement; 3) vacuum sputtering coating method: this method needs relatively more accurate laboratory apparatus, and it is universal to be unfavorable for that large industrialized is produced, and also needs after the vacuum plating through plating step.The applicant thinks that above-mentioned three kinds of methods all are not optimal fiber method for plating metal.
Summary of the invention
What the present invention will solve is exactly the existing above-mentioned defective of existing metallic conduction fiber preparation method, provides a kind of new metal to cover the preparation method of electro-conductive fiber.
The present invention is by matrix fiber (referring to polyster fibre and nylon fiber) being washed impurity such as removing the dust greasy dirt; alligatoring makes surface modification and increases surface adhesion force; the thin metal layer that the sensitization activation makes the fiber top layer produce katalysis is beneficial to subsequent reactions; utilize chemical plating method at fiber surface metal lining copper nickel then; last armor coated and obtain the electro-conductive fiber of high conductivity, concrete technical scheme is as follows:
The first step: pre-treatment and washing, remove fiber surface impurity with washings;
Second step: alligatoring, adopt the alligatoring agent to soak fiber, the fiber surface structure is carried out modification, make its surface irregularity and be beneficial to adsorbing metal ions;
The 3rd step: sensitization, at first soaked fiber 1 0～20 minutes with tin protochloride or cadmium chloride solution, make fiber surface absorption one deck tin ion or cadmium ion;
The 4th step: activation: soak fiber with palladium chloride solution and made palladium colloid replacement tin ion or cadmium be adsorbed on fiber surface in 10～20 minutes, thereby form the layer of metal Catalytic Layer;
The 5th step: electroless copper:
1) with following material and water preparation copper facing reaction solution, the content of each material is in every liter of reaction solution:
Copper sulfate: 5～20g/L
EDTA disodium: 20～40g/L
Seignette salt: 20～40g/L
Sodium hydroxide: 5～15g/L
Formaldehyde: 30～60mL/L
2) pH value to 10～11.5 of conditioned reaction liquid are immersed fiber in the reaction solution, and 80 ℃ were reacted 90～100 minutes down, obtain the electro-conductive fiber that coating surface has copper;
The 6th step: solidify: with promptly getting work in-process after the oxalic acid solution immersion back oven dry;
The 7th step: sensitization, there is the fiber of copper to carry out immersion treatment 5～15 minutes with tindichloride solution to plating, make the surface form very thin metal catalytic layer;
The 8th step: activation, soak the copper facing fiber with palladium chloride solution and made palladium colloid replacement tin ion or cadmium be adsorbed on fiber surface in 3～10 minutes, thereby form the layer of metal Catalytic Layer;
The 9th step: chemical nickel plating
Method one:
1) with following material and deionized water preparation reaction solution, the content of each material is in every liter of reaction solution:
Single nickel salt: 20～50g/L
Trisodium Citrate: 10～30g/L
Ammonium chloride: 20～40g/L
Sodium hydroxide: 5～15g/L
Inferior sodium phosphate: 20～60g/L
2) pH value to 9～9.5 of conditioned reaction liquid are immersed fiber in the reaction solution, and 50 ℃ were reacted 120～180 minutes down, obtain the electro-conductive fiber that the copper coating surface has nickel;
Method two:
1) with following material and deionized water preparation reaction solution, the content of each material is in every liter of reaction solution:
Nickelous chloride: 25～50g/L
Seignette salt: 10～30g/L
Trisodium Citrate: 10～30g/L
Sodium hydroxide: 5～15g/L
Hydrazine hydrate: 80～200mL/L
2) pH value to 10～10.5 of conditioned reaction liquid are immersed fiber in the reaction solution, and 95 ℃ were reacted 60～120 minutes down, obtain the electro-conductive fiber that the copper coating surface has nickel;
Method three:
1) with following material and deionized water preparation reaction solution, the content of each material is in every liter of reaction solution:
Single nickel salt: 20～50g/L
Trisodium Citrate: 8～20g/L
Sodium-acetate: 10～25g/L
Inferior sodium phosphate: 20～50g/L
2) pH value to 4～5 of conditioned reaction liquid are immersed fiber in the reaction solution, and 85 ℃ were reacted 60～120 minutes down, obtain the electro-conductive fiber that the copper coating surface has nickel;
The tenth step: solidify, get product after the oven dry after soaking with deionized water.
Mixing, washing liquid or 1～5g/L sodium hydroxide solution that step 1 adopts commercially available common washing composition to form with the ratio of 1: 2～1: 10 grams per milliliter of dehydrated alcohol carry out pre-treatment to fiber.
The described alligatoring agent of step 2 is analytically pure 1, the 2-ethylene dichloride, and dimethylbenzene, soak time is 10～20 minutes.
Step 3 adopts is that volumetric concentration is that tin protochloride or the volumetric concentration of 2～5g/L is the cadmium chloride solution of 2～5g/L, and the time of sensitization is 10～20 minutes.
0.01～0.05g/L that the palladium chloride solution volumetric concentration that step 4 adopts is, soak time be 10～20 minutes with.
Step 5 adopts deionized water to prepare reaction solution, the pH value that adopts analytical pure ammoniacal liquor to come conditioned reaction liquid.
The concentration of the described oxalic acid solution of step 6 is 2～5g/L, and oven dry is 150 ℃ of heating seasoninies after 2～10 minutes down.
The volumetric concentration of the used tindichloride solution of step 7 is 1～4g/L, and the time of sensitization is 5～15 minutes.
The volumetric concentration of the palladium chloride solution that step 8 adopts is 0.01～0.03g/L, and the activatory time is 3～10 minutes.
Step 9 adopts deionized water to prepare reaction solution, the pH value that adopts analytical pure ammoniacal liquor conditioned reaction liquid to the pH value of alkalescence or analytical pure sulfuric acid conditioned reaction liquid to acidity.
It is 5～25 minutes that step 10 is solidified the time of soaking with deionized water, and oven dry is to heat 5～15 minutes down at 150 ℃.
The present invention is simple to operation, and it is very little to the pollution of environment to compare the tradition plating, and power consumption is few, and than the easier suitability for industrialized production of vacuum sputtering.It is good to adopt the present invention to make the electro-conductive fiber conductivity, and specific surface area resistance reaches 1～10 ohm, and has kept the characteristic of original fiber, can be applied in multiple yarn fabric.
Embodiment
With specific examples the present invention is further elaborated below, only is used for explanation, do not limit scope of invention.
Embodiment 1:
Present embodiment adopts nylon to make matrix fiber
The first step, pre-treatment is carried out immersion treatment by 1: 5 (mass/volume) blended solution to fiber with commercially available White cat detergent and dehydrated alcohol, and soak time was generally 10 to 20 minutes, decided to remove surface blot and other impurity on the fiber clean level.
In second step, alligatoring uses 1, and the 2-ethylene dichloride soaked fiber 20 minutes, and it is carried out surface treatment, makes the coarse of its surface-area increase and structure change.
In the 3rd step, sensitization is soaked fiber with the tindichloride solution of 2.5g/L, and soak time is 15 minutes, makes the very thin metal catalytic layer of surface formation.
In the 4th step, activation was carried out immersion treatment 20 minutes with the palladium chloride solution of 0.02g/L to fiber.
The 5th step, electroless copper
Copper sulfate, disodium ethylene diamine tetraacetate, Seignette salt, sodium hydroxide and deionized water are mixed with the aqueous solution, add formaldehyde before the reaction again, be mixed with the copper facing reaction solution, the content of above-mentioned each material is in every liter of reaction solution:
Copper sulfate 10g/L
Disodium ethylene diamine tetraacetate 20g/L
Seignette salt 19g/L
Sodium hydroxide 8g/L
Formaldehyde 45mL/L
About the pH value to 12 with ammoniacal liquor conditioned reaction liquid, fiber is immersed in the reaction solution, 80 ℃ were reacted 90～100 minutes down, and reaction solution pH drops to about 9 reactions and stops, and obtains the electro-conductive fiber that coating surface has copper.(wherein disodium ethylene diamine tetraacetate can replace with ethylenediamine tetraacetic acid (EDTA).)
The 6th step, solidify, soaked fiber 10 minutes with volumetric concentration for the 2g/L oxalic acid solution, 150 ℃ of oven dry seasoninies after 2～5 minutes down, promptly make work in-process.
In the 7th step, in the 7th step, sensitization was carried out immersion treatment 10 minutes with the tindichloride solution of 2g/L to fiber, made the very thin metal catalytic layer of surface formation.
In the 8th step, activation was carried out immersion treatment 5 minutes with the palladium chloride solution of 0.01g/L to fiber, made the palladium colloid be adsorbed on the copper coating surface
The 9th step, chemical nickel plating
Single nickel salt, Trisodium Citrate, ammonium chloride, sodium hydroxide and deionized water are mixed with solution, add the ortho phosphorous acid sodium solution before the reaction again, be mixed with the nickel plating reaction solution, the content of above-mentioned each material is in every liter of reaction solution:
Single nickel salt 25g/L
Citric acid is received 15g/L
Ammonium chloride 25g/L
Sodium hydroxide 10g/L
Inferior sodium phosphate 25g/L
With pH value to 9.5～10 of ammoniacal liquor conditioned reaction liquid, fiber is immersed in the reaction solution, reaction stopped when 50 ℃ 120 minutes pH values to reaction solution of reaction dropped to 7 left and right sides down, obtained the electro-conductive fiber that the copper coating surface has nickel.
The tenth step, solidify, dried in 5～10 minutes in 150 ℃ of heating after 20 minutes with the deionized water immersion.
Test shows, this copper nickel bonded electro-conductive fiber has kept the high conductivity of copper and the erosion resistance of nickel, and specific surface area resistance reaches 1～10 ohm, and color is the dark white of nickel, and the coating phosphorus content is low, is fit to the high-count fabric requirement.
Embodiment 2:
Present embodiment adopts nylon to make matrix fiber
The first step, pre-treatment is carried out immersion treatment with the sodium hydroxide solution of 2g/L to fiber, and soak time was generally 15 minutes, to remove surface blot and other impurity.
In second step, alligatoring uses dimethylbenzene to soak fiber 15 minutes, and it is carried out surface treatment, makes the coarse of its surface-area increase and structure change.
In the 3rd step, sensitization is soaked fiber with the tindichloride solution of 2g/L, and soak time is 20 minutes, makes the very thin metal catalytic layer of surface formation.
In the 4th step, activation was carried out immersion treatment 20 minutes with the palladium chloride solution of 0.02g/L to fiber, made the palladium colloid replace tin ion formation metal catalytic layer.
The 5th step, electroless copper
Copper sulfate, disodium ethylene diamine tetraacetate, Seignette salt, sodium hydroxide and deionized water are mixed with the aqueous solution, add formaldehyde before the reaction again, be mixed with the copper facing reaction solution, the content of above-mentioned each material is in every liter of reaction solution:
Copper sulfate 12g/L
Disodium ethylene diamine tetraacetate 25g/L
Seignette salt 20g/L
Sodium hydroxide 10g/L
Formaldehyde 50mL/L
About the pH value to 12 with ammoniacal liquor conditioned reaction liquid, fiber is immersed in the reaction solution, 80 ℃ were reacted 90～100 minutes down, and reaction solution pH drops to about 9 reactions and stops, and obtains the electro-conductive fiber that coating surface has copper.
The 6th step, solidify, soaked fiber 10 minutes with volumetric concentration for the 2g/L oxalic acid solution, 150 ℃ of oven dry seasoninies after 2～5 minutes down, promptly make work in-process.
In the 7th step, in the 7th step, sensitization was carried out immersion treatment 10 minutes with the tindichloride solution of 2g/L to fiber, made the very thin metal catalytic layer of surface formation.
In the 8th step, activation was carried out immersion treatment 5 minutes with the palladium chloride solution of 0.01g/L to fiber, made the palladium colloid be adsorbed on the copper coating surface
The 9th step, chemical nickel plating
Nickelous chloride, Seignette salt, Trisodium Citrate, sodium hydroxide and deionized water are mixed with solution, add hydrazine hydrate before the reaction again, be mixed with the nickel plating reaction solution, the content of above-mentioned each material is in every liter of reaction solution:
Nickelous chloride 30g/L
Seignette salt 15g/L
Trisodium Citrate 15g/L
Sodium hydroxide 6.5g/L
Hydrazine hydrate 100mL/L
PH value to 10 with ammoniacal liquor conditioned reaction liquid immerses fiber in the reaction solution, and 95 ℃ were reacted 70 minutes down, obtain the electro-conductive fiber that the copper coating surface has nickel.
The tenth step, solidify, dried in 5～10 minutes in 150 ℃ of heating after 20 minutes with the deionized water immersion.
Test shows, the copper nickel electro-conductive fiber of this method preparation has kept the high conductivity of copper and the non-corrosibility of nickel equally, and specific surface area resistance reaches 1～10 ohm equally, and coating is not phosphorous, and color is darker partially than embodiment 1, and feel is compared softness.
Embodiment 3:
Present embodiment adopts terylene to make matrix fiber
The first step, pre-treatment is carried out immersion treatment by 1: 4 (mass/volume) blended solution to fiber with commercially available White cat detergent and dehydrated alcohol, and soak time was generally 10 to 20 minutes, decided to remove surface blot and other impurity on the fiber clean level.
In second step, alligatoring uses 1, and the 2-ethylene dichloride soaked fiber 20 minutes, and it is carried out surface treatment, makes the coarse of its surface-area increase and structure change.
In the 3rd step, sensitization is soaked fiber with the tindichloride solution of 2g/L, and soak time is 20 minutes, makes the very thin metal catalytic layer of surface formation.
In the 4th step, activation is carried out immersion treatment 20 minutes to obtain the metal catalytic layer of palladium coating with the palladium chloride solution of 0.02g/L to fiber.
The 5th step, electroless copper
Copper sulfate, disodium ethylene diamine tetraacetate, Seignette salt, sodium hydroxide and deionized water are mixed with the aqueous solution, add formaldehyde before the reaction again, be mixed with the copper facing reaction solution, the content of above-mentioned each material is in every liter of reaction solution:
Copper sulfate 8g/L
Disodium ethylene diamine tetraacetate 20g/L
Seignette salt 15g/L
Sodium hydroxide 10g/L
Formaldehyde 45mL/L
About the pH value to 12 with ammoniacal liquor conditioned reaction liquid, fiber is immersed in the reaction solution, 80 ℃ were reacted 90～100 minutes down, and reaction solution pH drops to about 9 reactions and stops, and obtains the electro-conductive fiber that coating surface has copper.
The 6th step, solidify, soaked fiber 10 minutes with volumetric concentration for the 2g/L oxalic acid solution, 150 ℃ of oven dry seasoninies after 2～5 minutes down, promptly make work in-process.
In the 7th step, in the 7th step, sensitization was carried out immersion treatment 10 minutes with the tindichloride solution of 2g/L to fiber, made the very thin metal catalytic layer of surface formation.
In the 8th step, activation was carried out immersion treatment 5 minutes with the palladium chloride solution of 0.01g/L to fiber, made the palladium colloid be adsorbed on the copper coating surface
The 9th step, chemical nickel plating
Single nickel salt, Trisodium Citrate, sodium-acetate and deionized water are mixed with solution, add the ortho phosphorous acid sodium solution before the reaction again, be mixed with the nickel plating reaction solution, the content of above-mentioned each material is in every liter of reaction solution:
Single nickel salt 25g/L
Citric acid is received 10g/L
Sodium-acetate 15g/L
Inferior sodium phosphate 25g/L
PH value to 4.8 with sulfuric acid conditioned reaction liquid immerses fiber in the reaction solution, and 85 ℃ were reacted 90 minutes down, obtain the electro-conductive fiber that the copper coating surface has nickel.
The tenth step, solidify, dried in 5～10 minutes in 150 ℃ of heating after 20 minutes with the deionized water immersion.
Test shows, the long-pending resistance of the metallic conduction specific fiber surface of this method preparation is 0.8～12 ohm, and color is whiter, and phosphorus content is more higher than embodiment 1, and feel is harder, is fit to the manufacturing of rough fibre product.
Embodiment 4:
Present embodiment adopts terylene to make matrix fiber
The first step, pre-treatment is carried out immersion treatment by 1: 4 (mass/volume) blended solution to fiber with commercially available White cat detergent and dehydrated alcohol, and soak time was generally 10 to 20 minutes, decided to remove surface blot and other impurity on the fiber clean level.
In second step, alligatoring uses 1, and the 2-ethylene dichloride soaked fiber 20 minutes, and it is carried out surface treatment, makes the coarse of its surface-area increase and structure change.
In the 3rd step, sensitization is soaked fiber with the tindichloride solution of 2.5g/L, and soak time is 20 minutes, makes the very thin metal catalytic layer of surface formation.
In the 4th step, activation was carried out immersion treatment 20 minutes with the palladium chloride solution of 0.02g/L to fiber.
The 5th step, electroless copper
Copper sulfate, disodium ethylene diamine tetraacetate, Seignette salt, sodium hydroxide and deionized water are mixed with the aqueous solution, add formaldehyde before the reaction again, be mixed with the copper facing reaction solution, the content of above-mentioned each material is in every liter of reaction solution:
Copper sulfate 8g/L
Disodium ethylene diamine tetraacetate 20g/L
Seignette salt 15g/L
Sodium hydroxide 10g/L
Formaldehyde 40mL/L
About the pH value to 12 with ammoniacal liquor conditioned reaction liquid, fiber is immersed in the reaction solution, 80 ℃ were reacted 90～100 minutes down, and reaction solution pH drops to about 9 reactions and stops, and obtains the electro-conductive fiber that coating surface has copper.(wherein disodium ethylene diamine tetraacetate can replace with ethylenediamine tetraacetic acid (EDTA).)
The 6th step, solidify, soaked fiber 20 minutes with volumetric concentration for the 2g/L oxalic acid solution, 150 ℃ of oven dry seasoninies after 2～5 minutes down, promptly make work in-process.
In the 7th step, in the 7th step, sensitization was carried out immersion treatment 10 minutes with the tindichloride solution of 2g/L to fiber, made the very thin metal catalytic layer of surface formation.
In the 8th step, activation was carried out immersion treatment 5 minutes with the palladium chloride solution of 0.01g/L to fiber, made the palladium colloid be adsorbed on the copper coating surface
The 9th step, chemical nickel plating
Single nickel salt, Trisodium Citrate, ammonium chloride, sodium hydroxide and deionized water are mixed with solution, add the ortho phosphorous acid sodium solution before the reaction again, be mixed with the nickel plating reaction solution, the content of above-mentioned each material is in every liter of reaction solution:
Single nickel salt 40g/L
Citric acid is received 30g/L
Ammonium chloride 30g/L
Sodium hydroxide 25g/L
Inferior sodium phosphate 35g/L
With pH value to 9.5～10 of ammoniacal liquor conditioned reaction liquid, fiber is immersed in the reaction solution, reaction stopped when 50 ℃ 180 minutes pH values to reaction solution of reaction dropped to 7 left and right sides down, obtained the electro-conductive fiber that the copper coating surface has nickel.
The tenth step, solidify, dried in 5～10 minutes in 150 ℃ of heating after 20 minutes with the deionized water immersion.
Test shows, this copper nickel bonded electro-conductive fiber has kept the high conductivity of copper and the erosion resistance of nickel, and specific surface area resistance reaches 1～10 ohm, and color is the dark white of nickel, and the coating phosphorus content is low, is fit to the high-count fabric requirement.
Embodiment 5:
Present embodiment adopts terylene to make matrix fiber
The first step, pre-treatment is carried out immersion treatment with the sodium hydroxide solution of 2g/L to fiber, and soak time was generally 15 minutes, to remove surface blot and other impurity.
In second step, alligatoring uses dimethylbenzene to soak fiber 15 minutes, and it is carried out surface treatment, makes the coarse of its surface-area increase and structure change.
In the 3rd step, sensitization is soaked fiber with the tindichloride solution of 2.5g/L, and soak time is 20 minutes, makes the very thin metal catalytic layer of surface formation.
In the 4th step, activation was carried out immersion treatment 20 minutes with the palladium chloride solution of 0.03g/L to fiber, made the palladium colloid replace tin ion formation metal catalytic layer.
The 5th step, electroless copper
Copper sulfate, disodium ethylene diamine tetraacetate, Seignette salt, sodium hydroxide and deionized water are mixed with the aqueous solution, add formaldehyde before the reaction again, be mixed with the copper facing reaction solution, the content of above-mentioned each material is in every liter of reaction solution:
Copper sulfate 12g/L
Disodium ethylene diamine tetraacetate 25g/L
Seignette salt 20g/L
Sodium hydroxide 10g/L
Formaldehyde 50mL/L
About the pH value to 12 with ammoniacal liquor conditioned reaction liquid, fiber is immersed in the reaction solution, 80 ℃ were reacted 90～100 minutes down, and reaction solution pH drops to about 9 reactions and stops, and obtains the electro-conductive fiber that coating surface has copper.
The 6th step, solidify, soaked fiber 10 minutes with volumetric concentration for the 2g/L oxalic acid solution, 150 ℃ of oven dry seasoninies after 2～5 minutes down, promptly make work in-process.
In the 7th step, in the 7th step, sensitization was carried out immersion treatment 10 minutes with the tindichloride solution of 2g/L to fiber, made the very thin metal catalytic layer of surface formation.
In the 8th step, activation was carried out immersion treatment 5 minutes with the palladium chloride solution of 0.01g/L to fiber, made the palladium colloid be adsorbed on the copper coating surface
The 9th step, chemical nickel plating
Nickelous chloride, Seignette salt, Trisodium Citrate, sodium hydroxide and deionized water are mixed with solution, add hydrazine hydrate before the reaction again, be mixed with the nickel plating reaction solution, the content of above-mentioned each material is in every liter of reaction solution:
Nickelous chloride 45g/L
Seignette salt 25g/L
Trisodium Citrate 18g/L
Sodium hydroxide 10g/L
Hydrazine hydrate 120mL/L
PH value to 10 with ammoniacal liquor conditioned reaction liquid immerses fiber in the reaction solution, and 95 ℃ were reacted 120 minutes down, obtain the electro-conductive fiber that the copper coating surface has nickel.
The tenth step, solidify, dried in 5～10 minutes in 150 ℃ of heating after 20 minutes with the deionized water immersion.
Test shows, the copper nickel electro-conductive fiber of this method preparation has kept the high conductivity of copper and the non-corrosibility of nickel equally, and specific surface area resistance reaches 1～10 ohm equally, and coating is not phosphorous, and color is darker partially than embodiment 1.To compare copper higher for the content of nickel in the coating, and fiber stiffness can increase to some extent.
Embodiment 6:
Present embodiment adopts nylon to make matrix fiber
The first step, pre-treatment is carried out immersion treatment by 1: 2 (mass/volume) blended solution to fiber with commercially available White cat detergent and dehydrated alcohol, and soak time is 20 minutes.In second step, alligatoring uses 1, and the 2-ethylene dichloride soaked fiber 20 minutes, and it is carried out surface treatment, makes the coarse of its surface-area increase and structure change.
In the 3rd step, sensitization is soaked fiber with the tindichloride solution of 2g/L, and soak time is 20 minutes, makes the very thin metal catalytic layer of surface formation.
In the 4th step, activation is carried out immersion treatment 20 minutes to obtain the metal catalytic layer of palladium coating with the palladium chloride solution of 0.02g/L to fiber.
The 5th step, electroless copper
Copper sulfate, disodium ethylene diamine tetraacetate, Seignette salt, sodium hydroxide and deionized water are mixed with the aqueous solution, add formaldehyde before the reaction again, be mixed with the copper facing reaction solution, the content of above-mentioned each material is in every liter of reaction solution:
Copper sulfate 12g/L
Disodium ethylene diamine tetraacetate 20g/L
Seignette salt 16g/L
Sodium hydroxide 14g/L
Formaldehyde 45mL/L
About the pH value to 12 with ammoniacal liquor conditioned reaction liquid, fiber is immersed in the reaction solution, 80 ℃ were reacted 90～100 minutes down, and reaction solution pH drops to about 9 reactions and stops, and obtains the electro-conductive fiber that coating surface has copper.
The 6th step, solidify, soaked fiber 10 minutes with volumetric concentration for the 2g/L oxalic acid solution, 150 ℃ of oven dry seasoninies after 2～5 minutes down, promptly make work in-process.
In the 7th step, in the 7th step, sensitization was carried out immersion treatment 15 minutes with the tindichloride solution of 2g/L to fiber, made the very thin metal catalytic layer of surface formation.
In the 8th step, activation was carried out immersion treatment 5 minutes with the palladium chloride solution of 0.02g/L to fiber, made the palladium colloid be adsorbed on the copper coating surface
The 9th step, chemical nickel plating
Single nickel salt, Trisodium Citrate, sodium-acetate and deionized water are mixed with solution, add the ortho phosphorous acid sodium solution before the reaction again, be mixed with the nickel plating reaction solution, the content of above-mentioned each material is in every liter of reaction solution:
Single nickel salt 40g/L
Citric acid is received 15g/L
Sodium-acetate 18g/L
Inferior sodium phosphate 33g/L
PH value to 5.0 with sulfuric acid conditioned reaction liquid immerses fiber in the reaction solution, and 85 ℃ were reacted 120 minutes down, obtain the electro-conductive fiber that the copper coating surface has nickel.
The tenth step, solidify, dried in 5～10 minutes in 150 ℃ of heating after 20 minutes with the deionized water immersion.
Test shows, the long-pending resistance of the metallic conduction specific fiber surface of this method preparation is 0.8～12 ohm, and color is whiter, and phosphorus content is more higher than embodiment 1, and feel is harder, is fit to the manufacturing of rough fibre product.Control reaction pH regulates between 4～5.5, fine-tuning coating phosphorus content, and this on the whole method coating phosphorus content is higher.
Claims (11)
1. the preparation method of a high-performance conductive fiber is characterized in that comprising the steps:
The first step: pre-treatment and washing, remove fiber surface impurity with washings;
Second step: alligatoring, adopt the alligatoring agent to soak fiber, the fiber surface structure is carried out modification, make its surface irregularity and be beneficial to adsorbing metal ions;
The 3rd step: sensitization, soak fiber with tin protochloride or cadmium chloride solution, make fiber surface absorption one deck tin ion or cadmium ion;
The 4th step: activation: soak fiber with palladium chloride solution and make palladium colloid replacement tin ion or cadmium be adsorbed on fiber surface, thereby form the layer of metal Catalytic Layer;
The 5th step: electroless copper:
1) with following material and water preparation copper facing reaction solution, the content of each material is in every liter of reaction solution:
Copper sulfate: 5～20g/L
EDTA disodium: 20～40g/L
Seignette salt: 20～40g/L
Sodium hydroxide: 5～15g/L
Formaldehyde: 30～60mL/L
2) pH value to 10～11.5 of conditioned reaction liquid are immersed fiber in the reaction solution, and 80 ℃ were reacted 90～100 minutes down, obtain the electro-conductive fiber that coating surface has copper;
The 6th step: solidify: with promptly getting work in-process after the oxalic acid solution immersion back oven dry;
The 7th step: sensitization, there is the fiber of copper to carry out immersion treatment with tindichloride solution to plating, make the surface form metal catalytic layer;
The 8th step: activation, soak the copper facing fiber with palladium chloride solution and make palladium colloid replacement tin ion be adsorbed on fiber surface, thereby form the layer of metal Catalytic Layer;
The 9th step: chemical nickel plating, adopt one of following three kinds of methods
Method one:
1) following material and deionized water preparation reaction solution, the content of each material is in every liter of reaction solution:
Single nickel salt: 20～50g/L
Trisodium Citrate: 10～30g/L
Ammonium chloride: 20～40g/L
Sodium hydroxide: 5～15g/L
Inferior sodium phosphate: 20～60g/L
2) pH value to 9～9.5 of conditioned reaction liquid are immersed fiber in the reaction solution, and 50 ℃ were reacted 120～180 minutes down, obtain the electro-conductive fiber that the copper coating surface has nickel;
Method two:
1) with following material and deionized water preparation reaction solution, the content of each material is in every liter of reaction solution:
Nickelous chloride: 25～50g/L
Seignette salt: 10～30g/L
Trisodium Citrate: 10～30g/L
Sodium hydroxide: 5～15g/L
Hydrazine hydrate: 80～200mL/L
2) pH value to 10～10.5 of joint reaction solution are immersed fiber in the reaction solution, and 95 ℃ were reacted 60～120 minutes down, obtain the electro-conductive fiber that the copper coating surface has nickel;
Method three:
1) with following material and deionized water preparation reaction solution, the content of each material is in every liter of reaction solution:
Single nickel salt: 20～50g/L
Trisodium Citrate: 8～20g/L
Sodium-acetate: 10～25g/L
Inferior sodium phosphate: 20～50g/L
2) pH value to 4～5 of conditioned reaction liquid are immersed fiber in the reaction solution, and 85 ℃ were reacted 60～120 minutes down, obtain the electro-conductive fiber that the copper coating surface has nickel;
The tenth step: solidify, soak the back oven dry with deionized water and get product.
2. the preparation method of high-performance conductive fiber according to claim 1 is characterized in that step 1 adopts commercially available common washing composition and dehydrated alcohol according to mixing, washing liquid or the 1～5g/L sodium hydroxide solution that the ratio of 1: 2～1: 10 grams per milliliter forms fiber to be carried out pre-treatment.
3. the preparation method of high-performance conductive fiber according to claim 1 is characterized in that the described alligatoring agent of step 2 is 1,2-ethylene dichloride or dimethylbenzene, and soak time is 10～20 minutes.
4. the preparation method of high-performance conductive fiber according to claim 1, what it is characterized in that step 3 adopts is that volumetric concentration is that tin protochloride or the volumetric concentration of 2～5g/L is the cadmium chloride solution of 2～5g/L, the time of sensitization is 10～20 minutes.
5. the preparation method of high-performance conductive fiber according to claim 1 is characterized in that the palladium chloride solution volumetric concentration that step 4 adopts is 0.01～0.05g/L, and soak time is 10～20 minutes.
6. the preparation method of high-performance conductive fiber according to claim 1 is characterized in that step 5 and step 9 adopt pH value that ammoniacal liquor comes conditioned reaction liquid to alkalescence, and the pH value that adopts sulfuric acid conditioned reaction liquid is to acidity.
7. the preparation method of high-performance conductive fiber according to claim 1, the volumetric concentration that it is characterized in that the described oxalic acid solution of step 6 is 2～5g/L, and soak time is 10～20 minutes, and oven dry is 150 ℃ of heating seasoninies after 2～10 minutes down.
8. the preparation method of high-performance conductive fiber according to claim 1, the volumetric concentration that it is characterized in that the used tindichloride solution of step 7 sensitization is 1～4g/L, the time of sensitization is 5～15 minutes.
9. the preparation method of high-performance conductive fiber according to claim 1 is characterized in that the volumetric concentration of the palladium chloride solution that step 8 activation is adopted is 0.01～0.03g/L, and the activatory time is 3～10 minutes.
10. the preparation method of high-performance conductive fiber according to claim 1 is characterized in that it is 5～25 minutes that step 10 is solidified the time of soaking with deionized water, and oven dry is 150 ℃ of heating 5～15 minutes down.
11. the preparation method of high-performance conductive fiber is characterized in that described fiber is terylene or nylon according to claim 1.
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