CN103757617A - Ni-Cu-La-B quaternary alloy plating solution and method for chemically plating glass fibers by using same - Google Patents
Ni-Cu-La-B quaternary alloy plating solution and method for chemically plating glass fibers by using same Download PDFInfo
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Abstract
The invention discloses a Ni-Cu-La-B quaternary alloy plating solution. The Ni-Cu-La-B quaternary alloy plating solution comprises the following components: 20-40g/L of nickel chloride, 10-20g/L of copper sulfate, 0.5-10 g/L of lanthanum sulfate, 0.5-3 g/L of sodium borohydride, 40-50g/L of potassium sodium tartrate, 15-30g/L of ethylenediamine and 35-60g/L of sodium hydroxide. A method for chemically plating the glass fibers by using the Ni-Cu-La-B quaternary alloy plating solution comprises the following steps: using sodium borohydride as a reducing agent, adding the water-soluble lanthanum sulfate, and chemically plating the glass fibers by using the Ni-Cu-La-B quaternary alloy plating solution under the conditions of strong base and low temperature; plating layers are Ni-Cu-La-B alloy plating layers, wherein the content of boron is low (only about 0.5-5wt%), the content of nickel in the plating layers is high; the plating layers have good bonding force, electrical conductivity and wear resistance. Through observation with microscopes, the plating layers of the Ni-Cu-La-B quaternary alloy plated glass fibers prepared by using the method are compact; testing with an X-ray energy dispersive spectrometer shows that the surface chemistry components of the Ni-Cu-La-B quaternary alloy plated glass fibers contain 15-50wt% of Ni, 2-15wt% of Cu, 0.5-5wt% of La and 0.5-5wt% of B. The electric conducting glass fibers can be applied to the special fields of electromagnetic wave shielding, microwave absorption, invisibility, anti-static electricity and the like.
Description
Technical field
The present invention relates to electroless plating technology field, relate in particular to a kind of Ni-Cu-La-B quad alloy plating solution and for the method for glass fibre electroless plating.
Background technology
High speed development along with modern science and technology, a kind ofly by people, be called " stealthy killer " electromagnetic radiation pollution and day by day receive the concern of all circles, the impact that the electromagnetic interference that electromagnetic radiation causes, electromagnetic information are divulged a secret and electromagnetic environmental pollution brings economic construction, national defense safety and social life is more and more serious, and electromagnetic radiation pollution has become large public hazards of society.Adopting electromagnetic wave screen paint is a kind of method of effective control electromagnetic radiation pollution to disturbing the stray electrical magnetic wave of the normal work of electronic and electrical equipment to carry out electromagnetic wave shielding processing.For electromagnetic wave screen paint, the cost of conductive filler material and conductivity, proportion etc. have become the key factor of its cost performance of restriction and application thereof.Though the electroconductibility of the metals such as traditional gold and silver, aluminium, nickel, copper is good, excessive due to its high cost, proportion, greatly limited its marketing and used.
Electroless plating is that a kind of environmental protection, cost are lower, application surface metalation method of modifying more widely, utilize coating prepared by electroless plating technology evenly, firmly and composition be easy to control, electroless plating has become one of conventional technology of preparing of novel electromagnetic shielding compounded mix.At present, take plastics, fabric, fiber, glass microballon, timber, metal or mineral crystal whisker etc. is matrix, with electroless plating technology preparation, has successfully prepared various new electromagnetic shielding complex conductive fillers.
Glass fibre is a kind of ceramic of excellent performance, its insulativity, thermotolerance and erosion resistance are good, physical strength is high, strongthener in Chang Zuowei matrix material, electrically insulating material and heat-insulating material and circuit base material etc., be widely used in the many necks of national economy such as building, traffic, electronics, electric, chemical industry, metallurgy, environmental protection, national defence.Glass fibre is crisp, wear resistance and electroconductibility poor, reduced to a certain extent the cost performance of glass fibre, limit its range of application.To glass fibre chemical plating metal, can prepare electroconductive glass fibre.The principle of fiberglass surfacing chemical plating metal is: take glass fibre as matrix, utilize reductive agent that GOLD FROM PLATING SOLUTION (is for example belonged to ion, nickel, copper metal ion) etc. chemical reduction be the fiberglass surfacing of catalytic activity, in the situation that not having extrinsic current to pass through, make it to form electroconductive coating, thereby obtain plating metal on surface (for example, ambrose alloy) glass fibre.
At present, about fiberglass surfacing electroless plating multicomponent alloy technology disclosed patent mainly contain: 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 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 solution is comprised 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 adding appropriate La in chemical plating fluid
2o
3, in obtained alloy layer, phosphorus content is 1.8%～17%.
China's patent applied for 200710017926.1 relates to a kind of glass fibre Electroless Plating Ni-Co-Fe-La-P quinary alloy plating solution and preparation method thereof, its plating solution is comprised 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 adding appropriate La in chemical plating fluid
2o
3, in obtained alloy layer, phosphorus content is 3%～17%.
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 solution is comprised 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 adding appropriate La in chemical plating fluid
2o
3, in obtained alloy layer, phosphorus content is 6%～23%.
Through retrieval, do not find patent application or the bibliographical information of glass fibre Electroless Plating Ni-Cu-La-B quad alloy plating solution and preparation method thereof.
Plating Ni-Cu-La-B glass fibre can be used as the functional stuffing of electrically conducting coating, for electromagnetic wave shielding, suction ripple, stealthy, antistatic and heating field.Fiberglass surfacing Electroless Plating Ni-Cu-La-B technology is expected to for improving the added value of glass fibre, for improving the comprehensive exploitation of non-metallic material and utilizing level that a kind of new technological method is provided.
It is reductive agent that traditional glass fibre electroless plating technology be take inferior sodium phosphate (having another name called sodium hypophosphite), and inferior sodium phosphate has certain toxicity, and under normal pressure, heating evaporation ortho phosphorous acid sodium solution can be blasted; In electroless plating, there is phosphorus to separate out with the codeposition of phosphorus and nickel and form the nickel-phosphorus alloy coating that the high and phosphorus of phosphorus content is disperse state, increased coating fragility and reduced binding force of cladding material and electroconductibility, thereby having affected quality of coating.The La adding in chemical plating fluid
2o
3water insoluble, reduced the effect of rare earth in electroless plating.
Summary of the invention
The object of this invention is to provide a kind of Ni-Cu-La-B quad alloy plating solution and for the method for glass fibre electroless plating.Mainly that glass fibre is after the pre-treatment such as oil removing, alligatoring, sensitization, activation, utilize reductive agent that nickel, copper, the reduction of lanthanum ion chemistry in solution are being to the fiberglass surfacing of catalytic activity, in the situation that not having extrinsic current to pass through, make it to form metal plating, thereby make surface containing the electroconductive glass fibre of Ni-Cu-La-B, improve the conductivity of glass fibre.
The technical scheme that the present invention takes is:
Ni-Cu-La-B quad alloy plating solution of the present invention composed as follows:
Solvent is distilled water.
Preferred:
Solvent is distilled water.
Utilize quad alloy plating solution of the present invention to carry out the concrete steps of method of fiberglass surfacing electroless plating as follows:
(1) first by proportioning, take respectively nickelous chloride, copper sulfate, lanthanum sulfat, sodium borohydride, Seignette salt, quadrol, sodium hydroxide;
(2) nickelous chloride, copper sulfate and the lanthanum sulfat, Seignette salt, sodium hydroxide and the quadrol that step (1) are taken are put into container, and add distilled water, are uniformly mixed at normal temperatures with magnetic stirrer;
(3) solution that slowly adds step (2) to prepare inferior sodium borohydride, is stirred to dissolving, splashes into ammoniacal liquor and regulates pH value to 12～13.5, is made into chemical plating fluid;
(4) glass fibre is put into the chemical plating fluid that step (3) prepares and carried out Electroless Plating Ni-Cu-La-B, 60～90 ℃ of plating temperatures, plating time 1～8h;
(5) above-mentioned prepared plating Ni-Cu-La-B glass fibre is dried, 80～100 ℃ of bake out temperatures, obtain plating Ni-Cu-La-B glass fibre.
In step (4), preferably 70～80 ℃ of plating temperatures.
In step (4), plating time is 3～6h preferably.
In step (5), preferably 80～90 ℃ of bake out temperatures.
Glass fibre in step (4) carries out pre-treatment before use, and pre-treatment step is as follows:
(1) use glass fibre is put into after 0.5～10% aqueous sodium carbonate soaks 8-24h and washed with distilled water, filter, dry;
(2) glass fibre of step (1) being processed immerses in the silane coupler solution that concentration is 0.5～5%, floods 2～20 minutes, filters, and dries;
(3) glass fibre of step (2) being processed immerses the salpeter solution that concentration is 40～65% and carries out roughening treatment processing 10～60 minutes, and the temperature of salpeter solution maintains 40～80 ℃;
(4) it is 5～20g/LSnCl that the glass fibre of step (3) being processed immerses concentration
22H
2in O and 10～30g/LHCl mixing solutions, carry out sensitization processing;
(5) glass fibre of step (4) being processed is at 0.1～2g/LPdCl
2with in 1～20mL/LHCl mixing solutions, carry out activation treatment.
The plating Ni-Cu-La-B glass fibre that utilizes method of the present invention to prepare is fine and close through microscopic examination coating, by X-ray energy spectrometer test surfaces chemical composition, containing Ni15～50wt%, Cu2～15wt%, La0.5～5wt%, B0.5～5wt%.The special dimensions such as this electroconductive glass fibre can be used for electromagnetic wave shielding, inhales ripple, stealthy and antistatic.
The present invention be take sodium borohydride as reductive agent, adds lanthanum sulfat soluble in water, carries out glass fibre Electroless Plating Ni-Cu-La-B quad alloy under strong basicity and cold condition; Coating is Ni-Cu-La-B alloy layer, the content low (being only 0.5%～5%) of boron, and coating nickel content is high, and binding force of cladding material, electroconductibility, wear resistance are good.
Positively effect of the present invention is as follows:
The present invention has following features:
1, the prepared Electroless Plating Ni-Cu-La-B glass fibre coating nickel content of the present invention is high, and binding force of cladding material, electroconductibility, wear resistance are good.
2, compare with the function solenoid filler such as conventional spherical, sheet, Electroless Plating Ni-Cu-La-B glass fibre is a kind of micron conductor fibers material, to improving coating electromagnetic wave shielding function, has good action.
3, the preparation of Electroless Plating Ni-Cu-La-B glass fibre is all carried out at low temperatures, and save energy is easy to use.
4, the preparation method of Electroless Plating Ni-Cu-La-B glass fibre simple, convenient, be easy to operate and control, use conventional equipment completely, investment is little, risk is less, is convenient to promote.
Embodiment
The following examples are to describe in further detail of the present invention.
Embodiment 1
Take glass fibre as base material, aqueous sodium carbonate with 1% soaked after 24 hours, and washed with distilled water, filtered, dry, in the silane coupler solution that immersion concentration is 1.5%, flood 10 minutes, filter, dry, the salpeter solution roughening treatment that the concentration that immerses 60 ℃ is 50% is processed 30 minutes, washing, and immersion concentration is 10g/LSnCl
22H
2in O and 20g/LHCl mixing solutions, carry out sensitization processing, immersion concentration is 0.3g/LPdCl
2with in 1.5mL/LHCl mixing solutions, carry out activation treatment.Then immerse in 60 ℃ of plating solutions plating 180 minutes, electroplate liquid formulation is nickelous chloride 35g/L, copper sulfate 15g/L, lanthanum sulfat 1g/L, sodium borohydride 1g/L, Seignette salt 45g/L, quadrol 18g/L, sodium hydroxide 45g/L, pH value 12.5.Obtain surface chemical plating Ni-Cu-La-B glass fibre, after being dried with 100 ℃, with microscopic examination, coating is fine and close.
Embodiment 2
Take glass fibre as base material, aqueous sodium carbonate with 1.5% soaked after 12 hours, and washed with distilled water, filtered, dry, in the silane coupler solution that immersion concentration is 1.5%, flood 10 minutes, filter, dry, the salpeter solution roughening treatment that the concentration that immerses 60 ℃ is 50% is processed 30 minutes, washing, and immersion concentration is 10g/LSnCl
22H
2in O and 20g/LHCl mixing solutions, carry out sensitization processing, immersion concentration is 0.3g/LPdCl
2with in 1.5mL/LHCl mixing solutions, carry out activation treatment.Then immerse in 70 ℃ of plating solutions plating 120 minutes, electroplate liquid formulation is nickelous chloride 30g/L, copper sulfate 20g/L, lanthanum sulfat 1.5g/L, sodium borohydride 0.8g/L, Seignette salt 40g/L, quadrol 25g/L, sodium hydroxide 50g/L, pH value 13.Obtain surface chemical plating Ni-Cu-La-B glass fibre, after being dried with 100 ℃, with microscopic examination, coating is fine and close.
Embodiment 3
Take glass fibre as base material, aqueous sodium carbonate with 1% soaked after 24 hours, and washed with distilled water, filtered, dry, in the silane coupler solution that immersion concentration is 1.5%, flood 10 minutes, filter, dry, the salpeter solution roughening treatment that the concentration that immerses 60 ℃ is 50% is processed 30 minutes, washing, and immersion concentration is 10g/LSnCl
22H
2in O and 20g/LHCl mixing solutions, carry out sensitization processing, immersion concentration is 0.3g/LPdCl
2with in 1.5mL/LHCl mixing solutions, carry out activation treatment.Then immerse in 60 ℃ of plating solutions plating 150 minutes, electroplate liquid formulation is nickelous chloride 40g/L, copper sulfate 20g/L, lanthanum sulfat 1g/L, sodium borohydride 2g/L, Seignette salt 50g/L, quadrol 30g/L, sodium hydroxide 50g/L, pH value 13.5.Obtain surface chemical plating Ni-Cu-La-B glass fibre, after being dried with 100 ℃, with microscopic examination, coating is fine and close.
Although illustrated and described embodiments of the invention, for the ordinary skill in the art, be appreciated that without departing from the principles and spirit of the present invention and can carry out multiple variation, modification, replacement and modification to these embodiment, scope of the present invention is limited by claims and equivalent thereof.
Claims (7)
1. a Ni-Cu-La-B quad alloy plating solution, is characterized in that: described Ni-Cu-La-B quad alloy plating solution composed as follows:
Solvent is distilled water.
2. Ni-Cu-La-B quad alloy plating solution as claimed in claim 1, is characterized in that: described Ni-Cu-La-B quad alloy plating solution composed as follows:
Solvent is distilled water.
3. utilize Ni-Cu-La-B quad alloy plating solution described in claim 1 or 2 to carry out a method for fiberglass surfacing electroless plating, it is characterized in that: the concrete steps of the method are as follows:
(1) first by proportioning, take respectively nickelous chloride, copper sulfate, lanthanum sulfat, sodium borohydride, Seignette salt, quadrol, sodium hydroxide;
(2) nickelous chloride, copper sulfate and the lanthanum sulfat, Seignette salt, sodium hydroxide and the quadrol that step (1) are taken are put into container, and add distilled water, are uniformly mixed at normal temperatures with magnetic stirrer;
(3) solution that slowly adds step (2) to prepare inferior sodium borohydride, is stirred to dissolving, splashes into ammoniacal liquor and regulates pH value to 12～13.5, is made into chemical plating fluid;
(4) glass fibre is put into the chemical plating fluid that step (3) prepares and carried out Electroless Plating Ni-Cu-La-B, 60～90 ℃ of plating temperatures, plating time 1～8h;
(5) above-mentioned prepared plating Ni-Cu-La-B glass fibre is dried, 80～100 ℃ of bake out temperatures, obtain plating Ni-Cu-La-B glass fibre.
4. method as claimed in claim 3, is characterized in that: the glass fibre in step (4) carries out pre-treatment before use, and pre-treatment step is as follows:
(1) glass fibre is put into after 0.5～10% aqueous sodium carbonate soaks 8-24h and washed with distilled water, filter, dry;
(2) glass fibre of step (1) being processed immerses in the silane coupler solution that concentration is 0.5～5%, floods 2～20 minutes, filters, and dries;
(3) glass fibre of step (2) being processed immerses the salpeter solution that concentration is 40～65% and carries out roughening treatment processing 10～60 minutes, and the temperature of salpeter solution maintains 40～80 ℃;
(4) it is 5～20g/LSnCl that the glass fibre of step (3) being processed immerses concentration
22H
2in O and 10～30g/LHCl mixing solutions, carry out sensitization processing;
(5) glass fibre of step (4) being processed is at 0.1～2g/LPdCl
2with in 1～20mL/LHCl mixing solutions, carry out activation treatment.
5. method as claimed in claim 3, is characterized in that: in step (4), and 60～90 ℃ of plating temperatures.
6. method as claimed in claim 3, is characterized in that: in step (4), and plating time 1～8h.
7. method as claimed in claim 3, is characterized in that: in step (5), and 80～100 ℃ of bake out temperatures.
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| CN105350044A (en) * | 2015-12-04 | 2016-02-24 | 太仓市建兴石英玻璃厂 | Electroplating pretreatment method for quartz glass |
| CN105834434A (en) * | 2016-04-27 | 2016-08-10 | 广东工业大学 | Chemical laser compound preparation method for copper micro-nano particles controllable in particle size distribution |
| CN106785556A (en) * | 2017-03-09 | 2017-05-31 | 维沃移动通信有限公司 | A kind of charging inlet, charging wire and mobile terminal |
| CN108342721A (en) * | 2018-03-06 | 2018-07-31 | 成都理工大学 | Fiberglass surfacing Electroless plating r-B quaternary alloy plating solutions and preparation method thereof |
| CN108588942A (en) * | 2018-04-10 | 2018-09-28 | 常熟市翔鹰特纤有限公司 | A kind of acrylic fibers copper facing-boron alloy electrically conductive filament and preparation method thereof |
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| CN105350044A (en) * | 2015-12-04 | 2016-02-24 | 太仓市建兴石英玻璃厂 | Electroplating pretreatment method for quartz glass |
| CN105834434A (en) * | 2016-04-27 | 2016-08-10 | 广东工业大学 | Chemical laser compound preparation method for copper micro-nano particles controllable in particle size distribution |
| CN105834434B (en) * | 2016-04-27 | 2017-12-05 | 广东工业大学 | A kind of chemical laser composite preparation process of the controllable copper micro-nano particle of particle diameter distribution |
| CN106785556A (en) * | 2017-03-09 | 2017-05-31 | 维沃移动通信有限公司 | A kind of charging inlet, charging wire and mobile terminal |
| CN106785556B (en) * | 2017-03-09 | 2019-04-12 | 维沃移动通信有限公司 | A kind of charging interface, charging cable and mobile terminal |
| CN108342721A (en) * | 2018-03-06 | 2018-07-31 | 成都理工大学 | Fiberglass surfacing Electroless plating r-B quaternary alloy plating solutions and preparation method thereof |
| CN108588942A (en) * | 2018-04-10 | 2018-09-28 | 常熟市翔鹰特纤有限公司 | A kind of acrylic fibers copper facing-boron alloy electrically conductive filament and preparation method thereof |
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