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CN101760734A - Tin-nickel chemical plating prescription and process on surface of glass fiber - Google Patents

Tin-nickel chemical plating prescription and process on surface of glass fiber Download PDF

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Publication number
CN101760734A
CN101760734A CN201010103214A CN201010103214A CN101760734A CN 101760734 A CN101760734 A CN 101760734A CN 201010103214 A CN201010103214 A CN 201010103214A CN 201010103214 A CN201010103214 A CN 201010103214A CN 101760734 A CN101760734 A CN 101760734A
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China
Prior art keywords
tin
plating
nickel
glass fibre
solution
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Pending
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CN201010103214A
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Chinese (zh)
Inventor
管登高
孙传敏
钟素华
林金辉
王自友
卢长寿
孙遥
徐冠立
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Chengdu Univeristy of Technology
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Chengdu Univeristy of Technology
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Priority to CN201010103214A priority Critical patent/CN101760734A/en
Publication of CN101760734A publication Critical patent/CN101760734A/en
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Abstract

The invention relates to tin-nickel chemical plating prescription and process on the surface of glass fiber, which can be used for preparing electroconductive glass fiber materials in special fields of electromagnetic wave shielding, wave absorption, stealth and anti-static, and the like. A pretreatment process before the surface of the glass fiber is plated with tin and nickel mainly comprises the following steps of: deoiling, coarsening, sensibilizing, activating, and the like. The tin-nickel plating process and prescription mainly comprise stannic chloride, nickel chloride, sodium hypophosphite and sodium citrate, wherein the pH value is 3 to 6, the plating temperature is 80 to 100 DEG C, the plating time is 0.5 to 5 hours, and the drying temperature is 60 to 100 DEG C. The invention is simple, convenient and easy to operate and control; and the prepared tin-nickel chemical plating glass fiber has satisfied technical parameters and can be widely applied to tin-nickel chemical plating on the surface of nonmetal powders.

Description

Fiberglass surfacing tin-nickel plating prescription and technology
One, technical field
The invention belongs to the electroless plating technology field, the electroconductive glass fibre material of special dimensions such as being specifically related to a kind ofly to can be used for electromagnetic wave shielding, inhaling ripple, be stealthy and antistatic preparation---fiberglass surfacing tin-nickel plating is filled a prescription and technology.
Two, background technology
Along with developing rapidly of electric power and electronic information technology, electromagnetic radiation pollution has become big public hazards of current society, the electromagnetic interference that electromagnetic radiation causes, electromagnetic information are divulged a secret and electromagnetic environment to pollute the influence that economic construction, national defense safety and social life are brought more and more serious.Be the control electromagnetic radiation pollution, the stray electrical magnetic wave that disturbs the electronic and electrical equipment works better is inhaled ripple to the employing electro-conductive material and shielding processing is especially necessary.Though and the electroconductibility of metals such as traditional gold and silver, copper, nickel is good,, has greatly limited its marketing and used because its cost is too high.
Glass fibre is to be raw material with glass sphere or discarded glass, and the diameter that forms through prepared such as high temperature melting, wire drawings is a kind of filamentary material of several microns to tens microns.Glass fibre is a kind of ceramic of excellent performance, and its insulativity, thermotolerance and erosion resistance are good, the physical strength height.Along with developing rapidly of market economy; glass fibre is mainly as electrically insulating material; strongthener; industrial filter material; anticorrosion, moistureproof, heat insulation, sound insulation, cushioning material have become the requisite starting material of industry such as building, traffic, electronics, electric, chemical industry, metallurgy, environment protection, national defence.However, because glass fibre is crisp, wear resistance and electroconductibility are relatively poor, have influenced the cost performance of glass fibre to a certain extent, limit its range of application.And can give characteristics such as some special mechanics of glass fibre, electricity and magnetics by the physical and chemical modified technology.
Electroless plating is a kind of environmental protection and surface metalation method of modifying cheaply since the coating of electroless plating technology preparation evenly, firmly and composition be easy to control, electroless plating has become one of common method of preparation electro-conductive material.The preparation principle of fiberglass surfacing tin-nickel plating is: be matrix with the glass fibre, utilize reductive agent that metal ion chemical reductions such as tin nickel in the solution are being the fiberglass surfacing of catalytic activity, under the situation that does not have extrinsic current to pass through, make it to form electroconductive coating, thereby obtain zinc-plated nickel glass fibre.Zinc-plated nickel glass fibre can be used as the functional stuffing of electrically conducting coating, is used for electromagnetic wave shielding, inhales ripple, stealthy, antistatic and heating field.The zinc-plated nickel technology of fiberglass surfacing electroless plating is expected to for improving the added value of glass fibre, for the comprehensive exploitation that improves non-metallic material with utilize level that a kind of new technological method is provided.
At present, have about the disclosed patent of fiberglass surfacing electroless plating technology: the pre-treating process of the chemical plating conductive magneto-conductive glass fibre (patent No.: 200710017812.7), Ni-Fe-La-P four-component alloy plating solution for chemical plating on surface of fiberglass and preparation method thereof (patent No.: 200710017925.7), five-component alloy plating solution for chemical plating on surface of fiberglass and preparation method thereof (patent No.: 200710017926.1), Ni-Fe-La-P four-component alloy plating solution for chemical plating on fiberglass and preparation method thereof (patent No.: 200710017929.5).
China's patent applied for 200710017812.7 relates to a kind of pre-treating process of chemical plating conductive magneto-conductive glass fibre, by adopting homemade activation solution to make sensitization, one step of activation finish and optimize pre-treating technology, use composite coupling agent to strengthen Pa in glass fibre and the activation solution 2+Chemical adsorption capacity.
China's patent applied for 200710017925.7 relates to a kind of Ni-Fe-La-P four-component alloy plating solution for chemical plating on surface of fiberglass and preparation method thereof, its plating bath is made up of nickelous chloride, ferrous sulfate, lanthanum trioxide, Trisodium Citrate, oxysuccinic acid, Succinic Acid, inferior sodium phosphate, ammonium sulfate, distilled water, thiocarbamide, urea and concentrated hydrochloric acid, owing to add an amount of La in chemical plating fluid 2O 3, phosphorus content is 1.8%~17% in the obtained alloy layer.
China's patent applied for 200710017926.1 relates to a kind of glass fibre Electroless Plating Ni-Co-Fe-La-P quinary alloy plating bath and preparation method thereof, its plating bath is made up of nickelous chloride, rose vitriol, inferior sodium phosphate, ferrous sulfate, lanthanum trioxide, Trisodium Citrate, oxysuccinic acid, Succinic Acid, ammonium sulfate, distilled water, thiocarbamide, urea and concentrated hydrochloric acid, owing to add an amount of La in chemical plating fluid 2O 3, phosphorus content is 3%~17% in the obtained alloy layer.
China's patent applied for 200710017929.5 relates to a kind of Ni-Fe-La-P four-component alloy plating solution for chemical plating on fiberglass and preparation method thereof, its plating bath is made up of nickelous chloride, rose vitriol, lanthanum trioxide, Trisodium Citrate, oxysuccinic acid, Succinic Acid, inferior sodium phosphate, ammonium sulfate, distilled water, thiocarbamide, urea and concentrated hydrochloric acid, owing to add an amount of La in chemical plating fluid 2O 3, phosphorus content is 6%~23% in the obtained alloy layer.
By retrieval, do not find to adopt chemical plating method to prepare the patent application or the bibliographical information of tin-nickel plating glass fibre.
Three, summary of the invention
The purpose of this invention is to provide a kind of prescription and technology for preparing zinc-plated nickel electroconductive glass fibre----fiberglass surfacing tin-nickel plating in the fiberglass surfacing tin-nickel plating.Mainly be that glass fibre is after pre-treatment such as oil removing, alligatoring, sensitization, activation, utilize reductive agent that tin nickel metal ion chemical reduction in the solution is being the fiberglass surfacing of catalytic activity, under the situation that does not have extrinsic current to pass through, make it to form metal plating, thereby make the electroconductive glass fibre of surperficial stanniferous nickel, improve the chemical ingredients of glass fibre on the one hand, improve the conductivity of glass fibre on the other hand.
For solving the problems of the technologies described above, the present invention adopts following technical proposals:
1, the electroplate liquid formulation of fiberglass surfacing tin-nickel plating is as follows:
Tin chloride 30~60g/L
Nickelous chloride 10~30g/L
Inferior sodium phosphate 40~80g/L
Trisodium Citrate 70~100g/L
2, the pretreatment technology step of glass fibre is as follows:
(1) uses the acetone oil removing, and wash with distilled water;
(2) it is in 0.5~5% the silane coupler solution, flood 2-20 minute that the glass fibre step (1) handled immerses concentration, filters, and dries;
(3) the glass fibre immersion concentration of step (2) being handled is that the salpeter solution of 40-65% carries out roughening treatment processing 10~60 minutes, and the temperature maintenance of salpeter solution is at 40~80 ℃;
(4) it is 5~20g/L SnCl that the glass fibre of step (3) being handled immerses concentration 22H 2Carrying out sensitization in O and the 10~30g/L HCl mixing solutions handles;
(5) glass fibre that step (4) was handled is at 0.1~2g/L PdCl 2With carry out activation treatment in 1~20mL/L HCl mixing solutions.
3, fiberglass surfacing tin-nickel plating process step is as follows:
(1) by the described tin-nickel plating prescription of claim 1, uses the dissolved in distilled water tin chloride respectively, nickelous chloride, inferior sodium phosphate and Trisodium Citrate;
(2) consoluet tin chloride and nickel chloride solution are mixed after, join in the sodium citrate solution, stir;
(3) the ortho phosphorous acid sodium solution is slowly added the solution that step (2) is prepared, and dilution cause volume required, with salt acid for adjusting pH value to 3~6;
(4) glass fibre after will handling by the described pretreatment technology of claim 2 is put into the plating bath that step (3) prepared and is carried out tin-nickel plating, 80~100 ℃ of plating temperatures, plating time 0.5~5 hour;
(5) with above-mentioned prepared zinc-plated nickel glass fibre oven dry, 60~100 ℃ of bake out temperatures.
The zinc-plated nickel glass fibre of method for preparing with X-ray energy spectrometer test surfaces chemical ingredients, contains Sn 10~40wt%, Ni 2~20wt% through the densification of microscopic examination coating.Special dimensions such as this electroconductive glass fibre can be used for electromagnetic wave shielding, inhales ripple, stealthy and antistatic.
The present invention has following characteristics:
1, the tin-nickel plating glass fibre that is provided has the favorable conductive characteristic, and the surface contains Sn 10~40wt%, Ni 2~20wt%.
2, compare with function solenoid fillers such as the sphere of using always, sheets, the tin-nickel plating glass fibre is a kind of micron order filamentary material, and improvement is coated with the layer function skeleton good action.
3, the preparation of tin-nickel plating glass fibre is all carried out at low temperatures, and save energy is easy to use.
4, the preparation method of tin-nickel plating glass fibre simple, convenient, be easy to operate and control, use conventional equipment fully, can be widely used on the non-metallic powder in the tin-nickel plating process, investment is little, risk is less, is convenient to promote.
Four, embodiment
Below by embodiment the present invention is specifically described; be necessary to be pointed out that at this present embodiment only is used for the present invention is further specified; can not be interpreted as limiting the scope of the invention; the person skilled in the art of this area can make some nonessential improvement and adjustment according to the content of foregoing invention.
Embodiment 1
With the glass fibre is base material, uses the acetone oil removing, and washes with distilled water, immerses concentration and is in 1.5% the silane coupler solution, flooded 10 minutes, and filtered, oven dry, the concentration that immerses 60 ℃ is that 50% salpeter solution roughening treatment was handled 30 minutes, washing, and immersing concentration is 10g/L SnCl 22H 2Carry out sensitization in O and the 20g/L HCl mixing solutions and handle, immersing concentration is 0.3g/L PdCl 2With carry out activation treatment in the 1.5mL/L HCl mixing solutions.Immersed in 90 ℃ of plating baths plating then 40 minutes, electroplate liquid formulation is tin chloride 40g/L, nickelous chloride 15g/L, inferior sodium phosphate 60g/L, Trisodium Citrate 90g/L, pH value 4.2.Obtain the zinc-plated nickel glass fibre of surface chemistry, with 100 ℃ with its oven dry after, use microscopic examination, the coating densification.
Embodiment 2
With the glass fibre is base material, uses the acetone oil removing, and washes with distilled water, immerses concentration and is in 2% the silane coupler solution, flooded 8 minutes, and filtered, oven dry, the concentration that immerses 55 ℃ is that 60% salpeter solution roughening treatment was handled 35 minutes, washing, and immersing concentration is 12g/L SnCl 22H 2Carry out sensitization in O and the 25g/L HCl mixing solutions and handle, immersing concentration is 0.2g/L PdCl 2With carry out activation treatment in the 2mL/L HCl mixing solutions.Immersed in 90 ℃ of plating baths plating then 60 minutes, electroplate liquid formulation is tin chloride 45g/L, nickelous chloride 20g/L, and inferior sodium phosphate 65g/L, Trisodium Citrate 95g/L, pH value 5, bake out temperature is 95 ℃.Obtain the zinc-plated glass fibre of surface chemistry, with 95 ℃ with its oven dry after, use microscopic examination, the coating densification.
Embodiment 3
With the glass fibre is base material, uses the acetone oil removing, and washes with distilled water, immerses concentration and is in 1% the silane coupler solution, flooded 15 minutes, and filtered, oven dry, the concentration that immerses 50 ℃ is that 55% salpeter solution roughening treatment was handled 40 minutes, washing, and immersing concentration is 8g/L SnCl 22H 2Carry out sensitization in O and the 15g/L HCl mixing solutions and handle, immersion concentration is 0.5g/LPdCl 2With carry out activation treatment in the 2mL/L HCl mixing solutions.Immersed in 93 ℃ of plating baths plating then 60 minutes, electroplate liquid formulation is tin chloride 50g/L, nickelous chloride 15g/L, inferior sodium phosphate 70g/L, Trisodium Citrate 95g/L, pH value 4.5.Bake out temperature is 100 ℃.Obtain the zinc-plated nickel glass fibre of surface chemistry, with 100 ℃ with its oven dry after, use microscopic examination, the coating densification.

Claims (3)

1. a fiberglass surfacing tin-nickel plating prescription is characterized in that with the glass fibre being matrix, and it is carried out tin-nickel plating, and the electroplate liquid formulation of tin-nickel plating is as follows:
Tin chloride 30~60g/L
Nickelous chloride 10~30g/L
Inferior sodium phosphate 40~80g/L
Trisodium Citrate 70~100g/L.
2. a kind of fiberglass surfacing chemical plating stannum nickel preprocessing technology according to claim 1, technology comprises pre-treatment such as glass fibre oil removing, alligatoring, sensitization, activation, it is characterized in that the pretreatment technology step is as follows:
(1) uses the acetone oil removing, and wash with distilled water;
(2) it is in 0.5~5% the silane coupler solution, flood 2-20 minute that the glass fibre step (1) handled immerses concentration, filters, and dries;
(3) the glass fibre immersion concentration of step (2) being handled is that the salpeter solution of 40-65% carries out roughening treatment processing 10~60 minutes, and the temperature maintenance of salpeter solution is at 40~80 ℃;
(4) it is 5~20g/L SnCl that the glass fibre of step (3) being handled immerses concentration 22H 2Carrying out sensitization in O and the 10~30g/L HCl mixing solutions handles;
(5) glass fibre that step (4) was handled is at 0.1~2g/L PdCl 2With carry out activation treatment in 1~20mL/L HCl mixing solutions.
3. according to claim 1 and 2 described a kind of fiberglass surfacing tin-nickel plating process, it is characterized in that fiberglass surfacing tin-nickel plating process step is as follows:
(1) by the described tin-nickel plating prescription of claim 1, uses the dissolved in distilled water tin chloride respectively, nickelous chloride, inferior sodium phosphate and Trisodium Citrate;
(2) consoluet tin chloride and nickel chloride solution are mixed after, join in the sodium citrate solution, stir;
(3) the ortho phosphorous acid sodium solution is slowly added the solution that step (2) is prepared, and dilution cause volume required, with salt acid for adjusting pH value to 3~6;
(4) glass fibre after will handling by the described pretreatment technology of claim 2 is put into the plating bath that step (3) prepared and is carried out tin-nickel plating, 80~100 ℃ of plating temperatures, plating time 0.5~5 hour.
(5) with above-mentioned prepared zinc-plated nickel glass fibre oven dry, 60~100 ℃ of bake out temperatures.
CN201010103214A 2010-02-01 2010-02-01 Tin-nickel chemical plating prescription and process on surface of glass fiber Pending CN101760734A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106119817A (en) * 2016-06-28 2016-11-16 西安理工大学 A kind of method of W fiber surface chemical deposition morphology controllable nickel dam
CN107164950A (en) * 2017-06-08 2017-09-15 中北大学 Fabric surface coats the preparation method of metal
CN111153639A (en) * 2020-03-01 2020-05-15 苏州巴涛信息科技有限公司 Radiation-proof concrete for preventing high-temperature fusion penetration and preparation method thereof
CN114105494A (en) * 2021-10-22 2022-03-01 北京科技大学 Coupling agent compounded ionic nickel palladium-free activation solution and method for preparing conductive basalt fiber

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106119817A (en) * 2016-06-28 2016-11-16 西安理工大学 A kind of method of W fiber surface chemical deposition morphology controllable nickel dam
CN106119817B (en) * 2016-06-28 2019-02-01 西安理工大学 A kind of method of W fiber surface chemical deposition morphology controllable nickel layer
CN107164950A (en) * 2017-06-08 2017-09-15 中北大学 Fabric surface coats the preparation method of metal
CN111153639A (en) * 2020-03-01 2020-05-15 苏州巴涛信息科技有限公司 Radiation-proof concrete for preventing high-temperature fusion penetration and preparation method thereof
CN114105494A (en) * 2021-10-22 2022-03-01 北京科技大学 Coupling agent compounded ionic nickel palladium-free activation solution and method for preparing conductive basalt fiber
CN114105494B (en) * 2021-10-22 2022-10-04 北京科技大学 Coupling agent compounded ionic nickel palladium-free activation solution and method for preparing conductive basalt fiber

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Open date: 20100630