CN104195532A - Preparation method of graphite sheet surface chemical plating iron-nickel alloy layer - Google Patents
Preparation method of graphite sheet surface chemical plating iron-nickel alloy layer Download PDFInfo
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- CN104195532A CN104195532A CN201410315243.4A CN201410315243A CN104195532A CN 104195532 A CN104195532 A CN 104195532A CN 201410315243 A CN201410315243 A CN 201410315243A CN 104195532 A CN104195532 A CN 104195532A
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Abstract
The invention relates to a preparation method of a graphite sheet surface chemical plating iron-nickel alloy layer. The preparation method comprises the following steps of 1, carrying out degreasing treatment on a graphite sheet; 2, carrying out oxidation treatment on the graphite sheet subjected to degreasing treatment; 3, carrying out the following sensitized treatment on the graphite sheet by utilizing a stannous chloride solution; 4, carrying out activating treatment on the graphite sheet by utilizing a palladium chloride solution; 5, sequentially adding 8-10 parts of C6H5Na3O7.2H2O powder, 4-5 parts of NH4Cl2 powder, 3-6 parts of FeSO4.7H2O powder, 2-3 parts of NiSO4.6H2O powder and 2-4 parts of NaH2PO2.H2O powder into ultra-pure water according to the mass ratio so as to fully dissolve the powder, adopting a NaOH aqueous solution as a pH adjustment solution, and dropwise adding the pH adjustment solution with the pH being controlled in a range of 9-9.5 to prepare a plating solution for surface chemical plating of the graphite sheet; 6, carrying out chemical plating treatment on the graphite sheet subjected to preliminary treatment. The preparation method is convenient in manufacturing and simple in process, and a compact and uniform plating layer with controllable thickness can be obtained on the surface of the graphite sheet.
Description
Technical field
The invention belongs to electroless plating technology field, relate to a kind of preparation method in graphite flake surface chemical plating layer of iron-nickel alloy.
Background technology
When we stride into the electricization information age in big strides, electromagnetic radiation brings our life and the harm of producing more and more receives people's concern, therefore the material that preparation has a high-performance electromagnetic wave shielding solves the harm that present and following electromagnetic pollution brings, and has been instant thing.Wherein electromagnetic shielding filler is the main raw material(s) that forms high-performance electromagnetic wave shielding and absorbing material.It is that filler, carbon are filler and compound filler that the current filler for shielding material can be divided into metal.And now, single filler is difficult to meet the requirement under complex electromagnetic environment with good electrical magnetic shielding, thereby adopt compounded mix comprehensively the shielding character of multiple material obtain that excellent wideband shields and the performance such as physical mechanical, be satisfied with the demand of varying environment and application scenario
At carbon, be in filler, graphite flake has the premium propertiess such as density is little, cost is low, electric conductivity is high, good stability, has larger specific surface area simultaneously and makes it in the shielding material of preparation, more easily form conductive network, thereby overcome the deficiency that common carbon is filler.But compare with metallic substance, the electric conductivity of graphite flake need to improve.And at graphite flake surface clad layer, form compound filler, and not only can keep graphite flake advantage, also give filler more excellent conductivity simultaneously.As everyone knows, electromagnetic decay mainly relies on reflection, absorbs and repeatedly launches three kinds of modes, and simple conducting metal mainly relies on electromagnetic reflection loss, thereby reaches the effect of electromagnetic shielding.But in order to obtain more excellent effectiveness, it is inadequate relying on merely electromagnetic reflection.Iron-nickel alloy has good microwave absorbing property, and there is good electroconductibility, as prepared compound filler in graphite flake surface construction layer of iron-nickel alloy, and for electromagnetic shielding material, be expected to obtain the electromagnetic shielding filler that performance is more excellent, but yet there are no this type of relevant report.
At present, existing people, using nickel bag graphite sheet as electromagnetic shielding filler, has obtained good effectiveness, and has been applied in electronic product.With frequency change, its shielding material of preparing is better in Mid Frequency effect conventionally due to electromagnetic parameter (specific conductivity, magnetic permeability, specific inductivity etc.) for nickel plating filler, but not satisfactory at the capability of electromagnetic shielding of low-frequency range.In low-intensity magnetic field, layer of iron-nickel alloy has the good soft magnetic performances such as low coercive force, high magnetic permeability and polarizability, and magnetic property can regulate by changing composition and thermal treatment process etc., there is in addition low magnetostriction coefficient, can obtain larger magneto-impedance effect.The present invention is by the compounded mix of preparing in graphite flake surface chemical plating layer of iron-nickel alloy, not only make filler retain the performances such as the good electroconductibility of graphite flake and low thermal resistance, also, compared with there being higher magnetic permeability under low-intensity magnetic field, in low-frequency range electromagnetic shielding field, can be more widely used.
Method at graphite flake surface clad mainly contains electroless plating, vacuum evaporating, sputter plating and metal meltallizing etc. at present.Wherein electroless plating is easy to operate, technique is simple, covering power is strong, hardness is high, wear-resisting, corrosion-resistant, and can on the particle of any shape, carry out plating, can preparation even, tiny, to disperse composite granule, therefore very suitablely carries out the coated of metal level on graphite flake surface.
Summary of the invention
The object of the present invention is to provide a kind of preparation method in graphite flake surface chemical plating layer of iron-nickel alloy.The method is easy to operate, technique is simple, can obtain on graphite flake surface the controlled and fine and close uniform coating of thickness.By in graphite flake surface chemical plating layer of iron-nickel alloy, the material of acquisition has good electromagnetism over-all properties, is expected to obtain in low-frequency range electromagnetic shielding field application.
A preparation method for graphite flake surface chemical plating layer of iron-nickel alloy, comprises the following steps:
1) graphite flake is carried out to oil removal treatment
2) graphite flake through oil removal treatment is carried out to oxide treatment;
3) graphite flake being carried out to following sensitization processes: the stannous chloride solution that compound concentration is 15～20g/L, the ratio that is 0.1～0.2g:1000ml in mass volume ratio again adds Sn grain in solution, oxidized to prevent solution, process step 2) ratio that the graphite flake of processing is 0.2～0.5g:100ml according to mass volume ratio joins in the solution preparing, and fully stir and make to disperse in constant temperature blender with magnetic force, temperature is 50～65 ℃, time is 30～40min, and stirring velocity is 200～300r/min; Clean again, filtration and drying treatment;
4) graphite flake is carried out to activation treatment
Compound concentration is the palladium chloride solution of 0.25～0.5g/L, by step 3) in the graphite flake that obtains according to mass volume ratio, be 0.4～0.8g:100ml ratio adds in the solution preparing, and fully stir and make to disperse in constant temperature blender with magnetic force, temperature is 35～40 ℃, time is 15～20min, and stirring velocity is 200～300r/min; Clean again, filtration and drying treatment, complete the pre-treating technology of graphite flake;
5) plating solution of preparation graphite flake surface chemical plating
According to the quality proportioning of 8～10 parts, 4～5 parts, 3～6 parts, 2～3 parts and 2～4 parts by C
6h
5na
3o
72H
2o powder, NH
4cl
2powder, FeSO
47H
2o powder, NiSO
46H
2o powder and NaH
2pO
2h
2o powder, joins in ultrapure water successively, and powder is fully dissolved, and utilizes the NaOH aqueous solution as pH regulator liquid, drips pH regulator hydraulic control pH processed in 9～9.5 scope;
6) graphite flake through pre-treatment is carried out to electroless plating processing
Graphite flake adds in the plating solution preparing, and mechanical stirring under the water bath condition of 80 ℃, in whipping process, drips pH regulator liquid, and pH is stabilized in 9～9.5 scopes, and after reaction 30～40min, plating solution becomes reaction when light blue from mazarine and finishes; Clean, filtration and drying treatment, complete the electroless plating on graphite flake surface.
As preferred implementation, the preparation method of described graphite flake surface chemical plating layer of iron-nickel alloy, step 2 is wherein: the ratio that is 10～15g:100ml according to mass volume ratio is by K
2cr
2o
7powder is dissolved in the sulphuric acid soln that volume fraction is 200～300ml/L completely, by through step 1) graphite flake of oil removal treatment is 1～1.5g:100ml according to mass volume ratio ratio is distributed in the above-mentioned solution preparing, in constant temperature blender with magnetic force, fully stir and make to disperse, temperature is 50～60 ℃, time is 10～15min, and stirring velocity is 200～300r/min; Clean again, filtration and drying treatment.
The content of iron in layer of iron-nickel alloy that obtains can be controlled in 8～20% scopes.
Wherein the massfraction of the vitriol oil can be 96～98%; The massfraction of concentrated hydrochloric acid can be 34～36%.
Cost of the present invention is low, easy to operate, can realize continuous production, and coating is controlled and fine and close even, and the performances such as its iron nickel composition and magnetic all can regulate by changing processing condition.By regulating iron nickel ratio in plating solution, regulate and control the iron nickel content in iron-nickel magnetic layer, thereby the magnetospheric soft magnetic performance of regulation and control layer of iron-nickel alloy, can also control the content of phosphorus in iron-nickel magnetic layer by adjusting pH value, thereby meet the requirement of different performance in production technique.Not only bonding force is strong, hardness is high for gained graphite flake of the present invention and layer of iron-nickel alloy coating, wear resistance is good, and electromagnetism high comprehensive performance, being expected to obtain good application in low-frequency range electromagnetic shielding field, is a kind of chemical plating technology that can promote the use of in industrial production.
Accompanying drawing explanation
The stereoscan photograph of graphite flake before and after Fig. 1 pre-treating technology: (a) before pre-treating technology, (b) after pre-treating technology.
Optical microscope photograph after Fig. 2 graphite flake chemical plating iron nickel alloy layer: (a) * 500, (b) * 100.
Stereoscan photograph after Fig. 3 graphite flake chemical plating iron nickel alloy layer: (a) * 1000, (b) * 20000.
XRD figure spectrum after Fig. 4 graphite flake chemical plating iron nickel alloy layer.
Magnetic hysteresis loop figure after Fig. 5 graphite flake chemical plating iron nickel alloy layer.
Embodiment:
Below in conjunction with drawings and Examples, the present invention will be described.
Example 1
The pre-treating technology of 1 graphite flake
It is the graphite flake that 80～100um, thickness are 5～20um that 1.1 oil removing process are got 1g diameter, putting into 100ml massfraction is in the NaOH aqueous solution of 100g/L, and fully stir and make to disperse (temperature is 45 ℃, and the time is 2h, and stirring velocity is 300r/min) in constant temperature blender with magnetic force.After stirring finishes, by washed with de-ionized water 3～5 times, to neutral, filter, finally put into after the dry 4h of loft drier of 80 ℃ standby.
1.2 oxidizing procesies are prepared the H2SO4 solution that 100ml volume fractions are 250ml/L, add the K of 10g
2cr
2o
7, in room temperature (25 ℃), the lower 10min that stirs dissolves it completely.The graphite flake obtaining in step 1.1 is added in the solution preparing, and fully stir and make to disperse (temperature is 60 ℃, and the time is 10min, and stirring velocity is 300r/min) in constant temperature blender with magnetic force.After stirring finishes, by washed with de-ionized water 3～5 times, to neutral, filter, finally put into after the dry 4h of loft drier of 80 ℃ standby.
1.3 sensitization techniques are got the SnCl2 powder of 10g, join in the dense HCl of 25ml, and room temperature (25 ℃) is lower to be stirred until powder dissolves completely, solution colour becomes colorless transparent, the Sn grain that adds 0.2g, oxidized to prevent solution, then use deionized water constant volume to 500mL.The graphite flake obtaining in step 1.2 is added in the solution preparing, and fully stir and make to disperse (temperature is 60 ℃, and the time is 30min, and stirring velocity is 300r/min) in constant temperature blender with magnetic force.After stirring finishes, by washed with de-ionized water 3～5 times, to neutral, filter, finally put into after the dry 4h of loft drier of 80 ℃ standby.
1.4 activating process are got 0.05gPdCl
2powder, joins in the dense HCl of 2ml, uses deionized water constant volume to 200mL.The graphite flake obtaining in step 1.3 is put into the solution preparing, and fully stirred and make to disperse (temperature is 35 ℃, and the time is 20min, and stirring velocity is 300r/min) in constant temperature blender with magnetic force.After stirring finishes, by washed with de-ionized water 3～5 times, to neutral, filter, finally put into after the dry 4h of loft drier of 80 ℃ standby.Now completed the pre-treating technology of graphite flake.Graphite flake stereoscan photograph before and after pre-treating technology as shown in Figure 1.With respect to figure (a), from figure (b), can see that the graphite surface through pre-treatment has adsorbed comparatively dense nano-scale particle, this particle is active site Pd simple substance.
The electroless plating on 2 graphite flake surfaces
The configuration of 2.1 plating solutions takes respectively 10gC
6h
5na
3o
72H
2o, 5gNH
4cl
2, 3gFeSO
47H
2the NiSO of O, 3g
46H
2the NaH of O, 2.8g
2pO
2h
2o, is dissolved in appropriate ultrapure water successively, then adds ultrapure water and is settled to 100mL.The NaOH aqueous solution that preparation massfraction is 140g/L, as pH regulator liquid, drips pH regulator hydraulic control pH processed in 9 scope.Now completed the preparation of plating solution.
The chemical plating technology of 2.2 graphite flakes is got the graphite flake 0.2g obtaining in step 1.4, puts into the plating solution preparing, and is then placed in the water-bath of 80 ℃, mechanical stirring, and stirring velocity is 200r/min.In whipping process, drip pH regulator liquid, make pH be stabilized in 9 left and right.After reaction 40min, find that plating solution is become from mazarine light blue, now reaction finishes.Then use washed with de-ionized water 3～5 times, filter, take out after finally putting into the dry 4h of loft drier of 80 ℃, complete the electroless plating on graphite flake surface.The content of iron in layer of iron-nickel alloy that obtains reaches 10%.As shown in Figure 2, its stereoscan photograph as shown in Figure 3 for optical microscope photograph after chemical plating iron nickel alloy layer.
Example 2
The pre-treating technology of 1 graphite flake
It is the graphite flake that 80～100um, thickness are 5～20um that 1.1 oil removing process are got 1g diameter, putting into 100ml massfraction is in the NaOH aqueous solution of 80g/L, and fully stir and make to disperse (temperature is 40 ℃, and the time is 3h, and stirring velocity is 300r/min) in constant temperature blender with magnetic force.After stirring finishes, by washed with de-ionized water 3～5 times, to neutral, filter, finally put into after the dry 4h of loft drier of 80 ℃ standby.
1.2 oxidizing procesies are prepared the H2SO4 solution that 100ml volume fractions are 200ml/L, add the K of 15g
2cr
2o
7, in room temperature (25 ℃), the lower 10min that stirs dissolves it completely.The graphite flake obtaining in step 1.1 is added in the solution preparing, and fully stir and make to disperse (temperature is 50 ℃, and the time is 15min, and stirring velocity is 300r/min) in constant temperature blender with magnetic force.After stirring finishes, by washed with de-ionized water 3～5 times, to neutral, filter, finally put into after the dry 4h of loft drier of 80 ℃ standby.
1.3 sensitization techniques are got the SnCl of 8g
2powder, joins in the dense HCl of 20ml, and room temperature (25 ℃) is lower to be stirred until powder dissolves completely, and it is transparent that solution colour becomes colorless, and adds the Sn grain of 0.2g, oxidized to prevent solution, then uses deionized water constant volume to 500mL.The graphite flake obtaining in step 1.2 is added in the solution preparing, and fully stir and make to disperse (temperature is 55 ℃, and the time is 40min, and stirring velocity is 300r/min) in constant temperature blender with magnetic force.After stirring finishes, by washed with de-ionized water 3～5 times, to neutral, filter, finally put into after the dry 4h of loft drier of 80 ℃ standby.
1.4 activating process are got 0.08gPdCl
2powder, joins in the dense HCl of 3ml, uses deionized water constant volume to 200mL.The graphite flake obtaining in step 1.3 is put into the solution preparing, and fully stirred and make to disperse (temperature is 40 ℃, and the time is 15min, and stirring velocity is 300r/min) in constant temperature blender with magnetic force.After stirring finishes, by washed with de-ionized water 3～5 times, to neutral, filter, finally put into after the dry 4h of loft drier of 80 ℃ standby.Now completed the pre-treating technology of graphite flake.
The electroless plating on 2 graphite flake surfaces
The configuration of 2.1 plating solutions takes respectively 10gC
6h
5na
3o
72H
2o, 5gNH
4cl
2, 5gFeSO
47H
2o, 2.5gNiSO
46H
2the NaH of O, 3g
2pO
2h
2o, is dissolved in appropriate ultrapure water successively, then adds ultrapure water and is settled to 100mL.The NaOH aqueous solution that preparation massfraction is 140g/L, as pH regulator liquid, drips pH regulator hydraulic control pH processed in 9.5 scope.Now completed the preparation of plating solution.
The chemical plating technology of 2.2 graphite flakes is got the graphite flake 0.2g obtaining in step 1.4, puts into the plating solution preparing, and is then placed in the water-bath of 80 ℃, mechanical stirring, and stirring velocity is 200r/min.In whipping process, drip pH regulator liquid, make pH be stabilized in 9.5 left and right.After reaction 30min, find that plating solution is become from mazarine light blue, now reaction finishes.Then use washed with de-ionized water 3～5 times, filter, take out after finally putting into the dry 4h of loft drier of 80 ℃, complete the electroless plating on graphite flake surface.The content of iron in layer of iron-nickel alloy that obtains has reached 14%.As shown in Figure 4, its magnetic hysteresis loop as shown in Figure 5 for XRD figure spectrum after chemical plating iron nickel alloy layer.
Claims (2)
1. a preparation method for graphite flake surface chemical plating layer of iron-nickel alloy, comprises the following steps:
1) graphite flake is carried out to oil removal treatment
2) graphite flake through oil removal treatment is carried out to oxide treatment;
3) graphite flake being carried out to following sensitization processes: the stannous chloride solution that compound concentration is 15～20g/L, the ratio that is 0.1～0.2g:1000ml in mass volume ratio again adds Sn grain in solution, oxidized to prevent solution, process step 2) ratio that the graphite flake of processing is 0.2～0.5g:100ml according to mass volume ratio joins in the solution preparing, and fully stir and make to disperse in constant temperature blender with magnetic force, temperature is 50～65 ℃, time is 30～40min, and stirring velocity is 200～300r/min; Clean again, filtration and drying treatment;
4) graphite flake is carried out to activation treatment
Compound concentration is the palladium chloride solution of 0.25～0.5g/L, by step 3) in the graphite flake that obtains according to mass volume ratio, be 0.4～0.8g:100ml ratio adds in the solution preparing, and fully stir and make to disperse in constant temperature blender with magnetic force, temperature is 35～40 ℃, time is 15～20min, and stirring velocity is 200～300r/min; Clean again, filtration and drying treatment, complete the pre-treating technology of graphite flake;
5) plating solution of preparation graphite flake surface chemical plating
According to the quality proportioning of 8～10 parts, 4～5 parts, 3～6 parts, 2～3 parts and 2～4 parts by C
6h
5na
3o
72H
2o powder, NH
4cl
2powder, FeSO
47H
2o powder, NiSO
46H
2o powder and N
ah
2pO
2h
2o powder, joins in ultrapure water successively, and powder is fully dissolved, and utilizes the NaOH aqueous solution as pH regulator liquid, drips pH regulator hydraulic control pH processed in 9～9.5 scope;
6) graphite flake through pre-treatment is carried out to electroless plating processing
Graphite flake adds in the plating solution preparing, and mechanical stirring under the water bath condition of 80 ℃, in whipping process, drips pH regulator liquid, and pH is stabilized in 9～9.5 scopes, and after reaction 30～40min, plating solution becomes reaction when light blue from mazarine and finishes; Clean, filtration and drying treatment, complete the electroless plating on graphite flake surface.
2. the preparation method of graphite flake surface chemical plating layer of iron-nickel alloy according to claim 1, step 2 is wherein: the ratio that is 10～15g:100ml according to mass volume ratio is by K
2cr
2o
7powder is dissolved in the sulphuric acid soln that volume fraction is 200～300ml/L completely, by through step 1) graphite flake of oil removal treatment is 1～1.5g:100ml according to mass volume ratio ratio is distributed in the above-mentioned solution preparing, in constant temperature blender with magnetic force, fully stir and make to disperse, temperature is 50～60 ℃, time is 10～15min, and stirring velocity is 200～300r/min; Clean again, filtration and drying treatment.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104477892A (en) * | 2014-12-12 | 2015-04-01 | 盐城市新能源化学储能与动力电源研究中心 | Preparation method of flake graphene and flake graphene device prepared by same |
| CN106220247A (en) * | 2016-07-21 | 2016-12-14 | 天津大学 | Needle-like ferroso-ferric oxide cladding iron-nickel alloy/graphite flake absorbing material preparation method |
| CN111408713A (en) * | 2020-03-17 | 2020-07-14 | 苏州逸峰新材料科技有限公司 | Preparation method of nickel-coated graphite composite powder material with high coating rate |
| CN115415519A (en) * | 2022-10-11 | 2022-12-02 | 雅安百图高新材料股份有限公司 | Chemical nickel plating solution of graphite micropowder and method for judging nickel plating reaction end point |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104477892A (en) * | 2014-12-12 | 2015-04-01 | 盐城市新能源化学储能与动力电源研究中心 | Preparation method of flake graphene and flake graphene device prepared by same |
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| CN106220247A (en) * | 2016-07-21 | 2016-12-14 | 天津大学 | Needle-like ferroso-ferric oxide cladding iron-nickel alloy/graphite flake absorbing material preparation method |
| CN111408713A (en) * | 2020-03-17 | 2020-07-14 | 苏州逸峰新材料科技有限公司 | Preparation method of nickel-coated graphite composite powder material with high coating rate |
| CN115415519A (en) * | 2022-10-11 | 2022-12-02 | 雅安百图高新材料股份有限公司 | Chemical nickel plating solution of graphite micropowder and method for judging nickel plating reaction end point |
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Application publication date: 20141210 |