CN104975277A - Preparation method of copper/nickel iron phosphorus alloy plating double-plating-layer fabric - Google Patents

Abstract

The invention relates to a preparation method of copper/nickel iron phosphorus alloy plating double-plating-layer fabric. The preparation method specifically comprises the following steps that (a), washing and oil removal are conducted; (b), a mixed water solution of strong reducing agents and surface active agents is used for dipping the fabric; (c), chemical copper plating is conducted; (d), washing is conducted; (e), the copper-plated fabric is dipped with a water solution of strong reducing agents; and (f), chemical nickel iron phosphorus alloy plating is conducted. The prepared copper/nickel iron phosphorus alloy plating double-plating-layer fabric not only has the superior electromagnetic shielding performance of an inner layer of copper, but also has the good abrasive resistance and corrosion resistance of an outer layer of nickel iron phosphorus alloy, and can be used in the electromagnetic shielding field. Therefore, the copper/nickel iron phosphorus alloy plating double-plating-layer fabric can be widely applied to special departments like aviation, spaceflight, war industry and communication and can also meet the individual protection requirements of staff occupied in radar, medical treatment, television relay and the like. Meanwhile, the palladium-free activation method has the advantages of being economical, easy and convenient to operate and the like compared with a palladium activation method.

Description

The preparation method of the two coating fabric of a kind of copper facing/ferronickel phosphorus alloy

Technical field

The invention provides the preparation method of the two coating fabric of nickel-clad iron phosphorus alloy again after a kind of copper facing.This technique is passed through at fabric face metal lining copper and mickel ferrophosphor(us) electrically conductive layer, thus make its antistatic, conducting function not only with copper but also there is the functions such as ferronickel phosphorus alloy wear resistance, solidity to corrosion, remain the lightweight of fabric, the natural characteristics such as soft simultaneously.Therefore the specials such as Aeronautics and Astronautics, navigation, military project, medical treatment can be widely used in, as anti-electrostatic and the Electromagnetically shielding fabrics of individual protection.Meanwhile, the invention provides the palladium-free activation process of a kind of electroless copper and chemical nickel plating ferrophosphor(us).

Background technology

Along with the develop rapidly of scientific and technological level, increasing electric/electronic device has spread to the every field of human lives, the electromagnetic interference simultaneously caused by hertzian wave and electromagnetic compatibility problem also day by day serious.The hertzian wave meeting severe jamming TV that electronic machine produces, the normal work of telecommunication equipment.Nineteen eighty-three, US Federal Communication Committee passes a resolution, and all electronic machines all require to carry out shielding to the hertzian wave of 10 MHz ~ 1000 MHz, and current countries in the world are also being handled like this.US Federal Communication Committee thinks that electronics enclosure useful chemical coating is to meet shielding requirements, and the shell estimating at 500,000,000 square metres of instruments needs shielding, and wherein 100,000,000 square metres can adopt the method for chemical nickel plating and electroless copper combined plating to solve.The effectiveness of electroless copper is 1000 times ~ 100,000 times of chemical Ni-plating layer, but its wear resistance and solidity to corrosion poor, so add one deck chemical Ni-plating layer on the surface just can obtain satisfied effect.After this copper facing, nickel-clad iron phosphorus alloy fabric had both maintained lightweight, the snappiness of common fabric because of it again, there is again certain conductivity, excellent capability of electromagnetic shielding, wear resistance and solidity to corrosion, therefore must gather around have broad application prospects in national defence, economic dispatch field.

Patent CN 103061114A teaches a kind of preparation method of Electromagnetically shielding fabrics, and this method plasma technique carries out chemical silvering, and cost is higher, and is unsuitable for scale operation.Patent CN 101532248B teaches a kind of preparation method of copper-clad electromagnetic wave shielding fabric, and first the method makes fabric face hydroxylation, and then makes fabric face sulfhydrylation, finally carries out electroless copper.But the wear resistance of layers of copper and solidity to corrosion poor, being long placed in air can blackening, thus capability of electromagnetic shielding is declined.Patent CN 100338301C refer to a kind of preparation method of conductive dacron fabric for electromagnetic wave shielding, and the method adopts sensitization-activation method to carry out pre-treatment to polyester piece good, and this process treatment process is complicated, uses Palladous chloride expensive.

This patent adopts palladium-free activation process to prepare two coating fabrics of copper facing/ferronickel phosphorus alloy, relative to traditional technology, not only technological operation is simple, economical, and the capability of electromagnetic shielding that prepared matrix material has copper concurrently has again wear resistance and the solidity to corrosion of ferronickel phosphorus alloy, has broad application prospects in electromagnetic shielding field.

Summary of the invention

The object of the invention is to provide the preparation method of the two coating fabric of a kind of copper facing/ferronickel phosphorus alloy.

The present invention by first carrying out cleaning oil removal treatment to fabric, removes the finish of fiber in the course of processing and surface smut; After oil removing, by textile impregnation in the mixing solutions of strong reductant and tensio-active agent, increase the wettability of fabric, fabric face is made to adsorb one deck strong reducible agent, for the metal ion in initial reduction plating solution, and using the metal simple-substance be reduced at first as catalyzer, carry out self-catalyzed reaction, then carry out electroless copper; By the fabric washed with de-ionized water after copper facing, continue copper facing textile impregnation in strong reductant solution, make copper facing fabric face adsorb one deck strong reducible agent, in this, as the target spot of autocatalysis; Finally, chemical nickel plating ferrophosphor(us) is carried out.

The preparation method of the two coating fabric of the present invention's a kind of copper facing/ferronickel phosphorus alloy, is characterized in that having following process and step:

A. the washing of organic polymer synthetic fabrics and oil removing: fabric is put into acetone, takes out after ultrasonic cleaning 30 ~ 90 min, use deionized water rinsed clean;

B. fabric face activation: the mixed aqueous solution fabric after oil removing being put into reductive agent and tensio-active agent, wherein reductive agent is sodium borohydride or POTASSIUM BOROHYDRIDE, concentration is 2 ~ 20 g/L, tensio-active agent is sodium lauryl sulphate or Sodium dodecylbenzene sulfonate, concentration is 1 ~ 10 mg/L, at 20 ~ 40 DEG C, take out after dipping 10 ~ 60 min;

C. electroless copper:

Copper plating bath with following material and water formulated, in reaction solution, the content of each material is:

Cupric sulfate pentahydrate 10 ~ 15g/L

Seignette salt (complexing agent) 10 ~ 20 g/L

Na ₂eDTA(disodium ethylene diamine tetraacetate, complexing agent) 15 ~ 20 g/L

NaOH(PH conditioning agent) 10 ~ 15 g/L

HCHO 12～17 g/L

Duplex pyridine (stablizer) 0.015 ~ 0.020 g/L

Yellow prussiate of potash (stablizer) 0.007 ~ 0.010 g/L

Fabric is immersed in plating solution, at 40 ~ 50 DEG C, take out after reaction 0.5 ~ 1 h, use deionized water rinsed clean, be placed in dry 30 min of loft drier, obtain the conductive fabric that surface uniform plating has copper;

D. clean: by the fabric washed with de-ionized water after copper facing;

E. copper facing fabric face activation: copper facing fabric is put into the strong reductant aqueous solution, and the composition of reductive agent is sodium borohydride or POTASSIUM BOROHYDRIDE, and concentration is 2 ~ 20 g/L, at 20 ~ 40 DEG C, takes out after dipping 10 ~ 60 min;

F. chemical nickel plating ferrophosphor(us):

Nickel-clad iron phosphorus alloy liquid with following material and water formulated, in reaction solution, the content of each material is:

Six water nickelous chloride 90 ~ 130 g/L

Ferric ammonium sulfate 5 ~ 8 g/L

Seignette salt (complexing agent) 40 ~ 60 g/L

Sodium hypophosphite (reductive agent) 7 ~ 15 g/L

Ammoniacal liquor (PH conditioning agent) 80 ~ 130 g/L

Copper facing fabric is immersed in plating solution, at 70 ~ 80 DEG C, takes out after reaction 0.5 ~ 1 h, use deionized water rinsed clean, be placed in dry 30 min of loft drier, obtain surface uniform, serving is ferronickel phosphorus alloy, two coating fabrics that interior coating is copper.

Accompanying drawing explanation

Fig. 1 is scanning electronic microscope (SEM) figure of fabric after the copper facing of the embodiment of the present invention 1 gained.

Fig. 2 is scanning electronic microscope (SEM) figure of fabric after the embodiment of the present invention 1 gained nickel-clad iron phosphor alloy coating.

Embodiment

after now specific embodiments of the invention being described in.

embodiment 1

preparation process in the present embodiment and step as described below:

(1) oil removing: fabric is put into acetone soln, takes out after ultrasonic cleaning 30 min, uses deionized water rinsed clean.

(2) activate: by the textile impregnation after washing in the sodium borohydride of 5 g/L and the mixing solutions of 3mg/L sodium lauryl sulphate, take out after soaking 10 min at 20 DEG C.

(3) electroless copper: the fabric after activation is put into copper plating bath, chemical bronze plating liquid consists of: cupric sulfate pentahydrate 10 g/L, Seignette salt 15 g/L, disodium ethylene diamine tetraacetate 15 g/L, NaOH 15 g/L, HCHO 12 g/L, duplex pyridine 0.020 g/L, yellow prussiate of potash 0.007 g/L.Bath temperature is 40 DEG C, plating time 30 min.

(4) clean: by the fabric washed with de-ionized water after copper facing.

(5) activate: by the textile impregnation after washing in the sodium borohydride solution of 2 g/L, take out after soaking 20 min at 30 DEG C.

(6) chemical nickel plating ferrophosphor(us): plating solution consists of: six water nickelous chloride 90 g/L, ferric ammonium sulfate 8 g/L, Seignette salt 40 g/L, sodium hypophosphite 15 g/L, ammoniacal liquor 80 g/L.Bath temperature is 60 DEG C, plating time 60 min.

embodiment 2

preparation process in the present embodiment and step as described below:

(1) oil removing: fabric is put into acetone soln, takes out after ultrasonic cleaning 90 min, uses deionized water rinsed clean.

(2) activate: by the textile impregnation after washing in the POTASSIUM BOROHYDRIDE of 2 g/L and the mixing solutions of 10mg/L Sodium dodecylbenzene sulfonate, take out after soaking 60 min at 40 DEG C.

(3) electroless copper: the fabric after activation is put into copper plating bath, chemical bronze plating liquid consists of: cupric sulfate pentahydrate 15 g/L, Seignette salt 10 g/L, disodium ethylene diamine tetraacetate 20 g/L, NaOH 10 g/L, HCHO 15 g/L, duplex pyridine 0.015 g/L, yellow prussiate of potash 0.010 g/L.Bath temperature is 50 DEG C, plating time 60 min.

(4) clean: by the fabric washed with de-ionized water after copper facing.

(5) activate: by the textile impregnation after washing in the solution of potassium borohydride of 6 g/L, take out after soaking 10 min at 40 DEG C.

(6) chemical nickel plating ferrophosphor(us): plating solution consists of: six water nickelous chloride 130 g/L, ferric ammonium sulfate 5 g/L, Seignette salt 60 g/L, sodium hypophosphite 10 g/L, ammoniacal liquor 80 g/L.Bath temperature is 80 DEG C, plating time 30 min.

embodiment 3

preparation process in the present embodiment and step as described below:

(1) oil removing: fabric is put into acetone soln, takes out after ultrasonic cleaning 60 min, uses deionized water rinsed clean.

(2) activate: by the textile impregnation after washing in the POTASSIUM BOROHYDRIDE of 20 g/L and the mixing solutions of 1mg/L sodium lauryl sulphate, take out after soaking 40 min at 30 DEG C.

(3) electroless copper: the fabric after activation is put into copper plating bath, chemical bronze plating liquid consists of: cupric sulfate pentahydrate 12 g/L, Seignette salt 20 g/L, disodium ethylene diamine tetraacetate 17 g/L, NaOH 12 g/L, HCHO 17 g/L, duplex pyridine 0.017 g/L, yellow prussiate of potash 0.009 g/L.Bath temperature is 45 DEG C, plating time 40 min.

(4) clean: by the fabric washed with de-ionized water after copper facing.

(5) activate: by the textile impregnation after washing in the solution of potassium borohydride of 10 g/L, take out after soaking 30 min at 25 DEG C.

(6) chemical nickel plating ferrophosphor(us): plating solution consists of: six water nickelous chloride 110 g/L, ferric ammonium sulfate 7 g/L, Seignette salt 50 g/L, sodium hypophosphite 7 g/L, ammoniacal liquor 100 g/L.Bath temperature is 70 DEG C, plating time 40 min.

Claims (1)

1. a preparation method for the two coating fabric of copper facing/ferronickel phosphorus alloy, is characterized in that having following process and step:

A. the washing of organic polymer synthetic fabrics and oil removing: fabric is put into acetone, takes out after ultrasonic cleaning 30 ~ 90 min, use deionized water rinsed clean;

B. fabric face activation: the mixed aqueous solution fabric after oil removing being put into reductive agent and tensio-active agent, wherein reductive agent is sodium borohydride or POTASSIUM BOROHYDRIDE, and concentration is 2 ~ 20 g/L; Tensio-active agent is sodium lauryl sulphate or Sodium dodecylbenzene sulfonate, and concentration is 1 ~ 10 mg/L, at 20 ~ 40 DEG C, takes out after dipping 10 ~ 60 min;

C. electroless copper:

Copper plating bath with following material and water formulated, in reaction solution, the content of each material is:

Cupric sulfate pentahydrate 10 ~ 15g/L

Seignette salt (complexing agent) 10 ~ 20 g/L

Na ₂eDTA(disodium ethylene diamine tetraacetate, complexing agent) 15 ~ 20 g/L

NaOH(PH conditioning agent) 10 ~ 15 g/L

HCHO 12～17 g/L

Duplex pyridine (stablizer) 0.015 ~ 0.020 g/L

Yellow prussiate of potash (stablizer) 0.007 ~ 0.010 g/L

Fabric is immersed in plating solution, at 40 ~ 50 DEG C, take out after reaction 0.5 ~ 1 h, use deionized water rinsed clean, be placed in dry 30 min of loft drier, obtain the conductive fabric that surface uniform plating has copper;

D. clean: by the fabric washed with de-ionized water after copper facing;

E. copper facing fabric face activation: copper facing fabric is put into the strong reductant aqueous solution, and the composition of reductive agent is sodium borohydride or POTASSIUM BOROHYDRIDE, and concentration is 2 ~ 20 g/L, at 20 ~ 40 DEG C, takes out after dipping 10 ~ 60 min;

F. chemical nickel plating ferrophosphor(us):

Nickel-clad iron phosphorus alloy liquid with following material and water formulated, in reaction solution, the content of each material is:

Six water nickelous chloride 90 ~ 130 g/L

Ferric ammonium sulfate 5 ~ 8 g/L

Seignette salt (complexing agent) 40 ~ 60 g/L

Sodium hypophosphite (reductive agent) 7 ~ 15 g/L

Ammoniacal liquor (PH conditioning agent) 80 ~ 130 g/L

Copper facing fabric is immersed in plating solution, at 70 ~ 80 DEG C, takes out after reaction 0.5 ~ 1 h, use deionized water rinsed clean, be placed in dry 30 min of loft drier, obtain surface uniform, serving is ferronickel phosphorus alloy, two coating fabrics that interior coating is copper.