CN108130567B - A kind of method of aqueous solution plating gallium nickel alloy - Google Patents
A kind of method of aqueous solution plating gallium nickel alloy Download PDFInfo
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- CN108130567B CN108130567B CN201711404956.8A CN201711404956A CN108130567B CN 108130567 B CN108130567 B CN 108130567B CN 201711404956 A CN201711404956 A CN 201711404956A CN 108130567 B CN108130567 B CN 108130567B
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/56—Electroplating: Baths therefor from solutions of alloys
Abstract
The present invention relates to a kind of methods of aqueous solution plating gallium nickel alloy, include the following steps: for hydrated sulfuric acid gallium and hydration nickel sulfate to be dissolved in the water, dodecyl sodium sulfate or neopelex is added, obtaining gallium concentration is 47g/L to 55g/L, nickel concentration is the plating solution of 7.5g/L to 9g/L, and the mass ratio of gallium element and nickel element is 5.2:1 to 7.3:1；Using copper sheet, zinc metal sheet, aluminium flake or nickel sheet as working electrode, using platinized platinum or glass-carbon electrode as auxiliary electrode, plating solution is placed in electrolytic cell, working electrode and auxiliary electrode are mounted in electrolytic cell and are connected with electrochemical workstation or potentiostat；It is electroplated using potentiostatic electrolysis, plating obtains gallium nickel alloy coating on the working electrode (s.The method of aqueous solution plating gallium nickel alloy according to the present invention, carries out, the simple and effective fine and close gallium nickel alloy coating that can be obtained with metallic luster under room temperature open environment.
Description
Technical field
The present invention relates to the preparations of the electrochemistry of gallium nickel alloy coating, relate more specifically to a kind of aqueous solution plating gallium nickel alloy
Method.
Background technique
Gallium (Ga) is a kind of silvery white non-ferrous metal, density 5.904g/cm3.29.78 DEG C of fusing point.2403 DEG C of boiling point, freezing point is very
It is low.It is mainly used for semi-conductor industry, light emitting diode and GaAs laser diode；Natural gallium is practiced shooting nuclear reaction through proton simultaneously
It obtains68Ge, will68Ge separates available68The daughter of Ge decay68Ga carries out nuclear medicine application, and therefore, gallium is also that production is put
Injectivity isotope68The primary raw material of Ge,68The main application of Ge has: 1) with its daughter68Ga(t1/2=68min, 89% β+, 3%
1077keV γ) balance when, it can be used as proton source, the correction as attenuation correction and PET/MRI scanner；2) it can be used as one
Kind radiopharmaceutical preparation68Ga generator；3)68The half-life period of Ge is 68min, can be with polypeptide and other small molecule medicines
The pharmacokinetics of object matches；In addition, it is newest studies have shown that gallium nickel intermetallic compound (gallium nickel alloy macroscopically may be used
Be called the solid solution of two kinds of metals, it is microcosmic on can be described as the intermetallic compound of gallium nickel, be the compound being keyed by metal,
Therefore resulting gallium nickel alloy be electroplated be equal to gallium nickel intermetallic compound) for catalyze and synthesize gas methanol be better than it is traditional
Cu/ZnO/Al2O3Catalyst, not only methanol yield with higher, can also substantially reduce the generation of carbon monoxide.
In order to produce radioactive isotope68Target piece needed for Ge is related to bombarding gallium target using high energy proton beam, hair
Raw nuclear reaction can produce radionuclide68Ge.Electro-deposition targetry is the important means for preparing gallium target.Since the fusing point of gallium is low,
It can liquefy completely during proton beam is practiced shooting, to make gallium target keep complete physical aspect, it is necessary in the form of gallium nickel alloy
Target processed.
Electro-deposition legal system gallium nickel alloy target piece mainly uses gallium chloride-chlorination nickel plating bath or sulfuric acid dissolution three to aoxidize at present
Two galliums, it is miscible to add gallium sulfate, with ammonium hydroxide tune pH to 1.5.Wherein, gallium chloride-chlorination nickel plating bath electro-deposition gallium nickel alloy
Method needs that hydrochloric acid is added, and to obtain to surface has the gallium nickel alloy coating of metallic luster that electroplating temperature must be added to at least 80
DEG C high temperature, which can be such that aqueous solution largely evaporates, and cathode-current density greatlys improve, due to joined hydrochloric acid, thus
Keep evolving hydrogen reaction very violent, therefore obtained gallium nickel alloy coating metal luster is poor, character is highly unstable, reproducibility
Difference, and with the extension of electroplating time, the evaporation of water, the concentration of gallium and nickel can improve in plating solution, when reaching certain high concentration
When you can't get fine and close gallium nickel alloy coatings.In addition, the method for sulfuric acid dissolution gallic oxide electro-deposition gallium nickel alloy, by
The concentrated sulfuric acid is slightly soluble in gallic oxide, it is very difficult to be dissolved, lower three oxygen of sulfuric acid dissolution with 27wt% of 220 DEG C of 500rpm stirrings
Change two gallium 48h dissolution rates no more than 50wt%, furthermore, gallium sulfate and ammonium hydroxide are easily changed into gel when adjusting pH with ammonium hydroxide, from
And plating solution is scrapped, the failure for causing plating solution to prepare.In the preparation of gallium nickel alloy catalyst, existing patent is by using ion
Gallium nickel alloy is electroplated in liquid electrolyte, but ionic liquid itself is expensive, and the water imbibition of glyoxaline ion liquid is strong, needs
It to be electroplated in anhydrous glove box, increase production cost, and be not easy to electroplating operations.In short, lack simply has at present
The electro-deposition method of effect prepares gallium nickel alloy.
Summary of the invention
In order to solve the problems of above-mentioned electro-deposition gallium nickel alloy of the existing technology, the present invention is intended to provide one
The method of kind aqueous solution plating gallium nickel alloy.
The method of aqueous solution plating gallium nickel alloy of the present invention, includes the following steps: S1, by hydrated sulfuric acid gallium and water
Close nickel sulfate to be dissolved in the water, dodecyl sodium sulfate or neopelex be added, obtain gallium concentration be 47g/L extremely
55g/L, nickel concentration are the plating solution of 7.5g/L to 9g/L, and the mass ratio of gallium element and nickel element is 5.2:1 to 7.3:1；S2, with copper
Plating solution is placed in electrolytic cell using platinized platinum or glass-carbon electrode as auxiliary electrode as working electrode by piece, zinc metal sheet, aluminium flake or nickel sheet
In, working electrode and auxiliary electrode are mounted in electrolytic cell and are connected with electrochemical workstation or potentiostat；S3, using perseverance
Potential electrolysis method is electroplated, and plating obtains gallium nickel alloy coating on the working electrode (s.
Preferably, the mass ratio of the gallium element in step S1 and nickel element is 6.1:1 to 6.3:1.
Hydrated sulfuric acid gallium and hydration nickel sulfate in the step S1 are dissolved in the water under conditions of room temperature is to 60 DEG C.It answers
The understanding, if temperature is excessively high, the evaporation of the water in plating solution is accelerated, and causes concentration in final dissolved ion bigger than normal；If
Temperature is too low, and solution rate reduces, so that dissolution time is greatly extended.
Water in the step S1 is deionized water, and resistivity is 18.2M Ω cm.
The concentration of dodecyl sodium sulfate or neopelex in the plating solution in the step S1 is 0.06g/L
To 0.09g/L.
The mass ratio of gallium element and nickel element is 6:1 in the step S1.
The gallium concentration of plating solution in the step S1 is 50.57g/L, nickel concentration 8.26g/L, wherein gallium element and nickel
The mass ratio of element is 6.1:1.
The step S1 specifically: weigh 18 water conjunction gallium sulfate and hydration nickel sulfate is placed in a beaker, deionization is added
It is stirred after water, adds dodecyl sodium sulfate and stirring makes it completely dissolved, obtain plating solution with deionized water constant volume.
The mounting height of working electrode and auxiliary electrode in the step S2 is consistent and to just.
The distance between working electrode and auxiliary electrode in the step S2 are 0.5cm to 5cm.It should connect, if
This, will be so that resistance increases apart from excessive, and the energy consumption of gallium Nickel alloy electroplating process is increase accordingly；If this apart from too small, will make
The bubble generated on auxiliary electrode is obtained to have an impact the coating on working electrode.
The step S2 further includes providing reference electrode.
The distance of reference electrode to working electrode in the step S2 is 1mm to 3mm.It should be understood that if the distance
It is excessive, the working electrode potential measured by reference electrode will be made inaccurate；It, will be so that practical behaviour if this is apart from too small
It is easy to make reference electrode touch working electrode and influence to be electroplated during making.
Working electrode in the step S2 is by polishing, polishing and carrying out washing treatment.Preferably, which includes using
Acetone is cleaned by ultrasonic working electrode 15min to remove grease stain, is rinsed after taking out working electrode with deionized water.
In the step S3, it under conditions of bath temperature is maintained at 20 DEG C to 30 DEG C, is electroplated on the working electrode (s
To gallium nickel alloy coating.It should be understood that coating deposition rate is too fast if temperature is excessively high, coating blackening, adhesive force is very poor；Such as
Fruit temperature is too low, and depositing current density is too small, and electrodeposition time is greatly extended.
In the step S3, the plating control of Electric potentials of working electrode is between -0.7V to -1.2V.Although every kind of metal
Electro-deposition has the sedimentation potential of oneself, however, it is to be understood that by that control of Electric potentials will be electroplated within the above range, it can be true
It protects and obtains excellent adhesive force and lustrous surface.If overtension, will lead to that metal deposit is too fast, the performance pattern of coating and
Adhesive force will all deteriorate；If brownout, will lead to gallium nickel alloy can not be deposited or deposit slowly.Preferably, whole
Keep current potential constant in a electroplating process.
In the step S3, electroplating time is 15min to 4h.In addition, the electroplating process is under conditions of magnetic agitation
It carries out.Preferably, the revolving speed of the magnetic agitation is 500rpm.
In the step S3, working electrode is removed after the completion of plating, is rinsed with deionized water and natural air drying obtains
Gallium nickel alloy coating.
The method of aqueous solution plating gallium nickel alloy according to the present invention, carries out under room temperature open environment, without heating plating
Liquid, the simple and effective fine and close gallium nickel alloy coating that can be obtained with metallic luster greatly simplifie plating gallium nickel alloy
Condition has saved the energy, reduces costs, wherein practice have shown that, dodecyl sodium sulfate or neopelex add
Add, gallium concentration is 47g/L to 55g/L, nickel concentration be the plating solution of 7.5g/L to 9g/L, working electrode material selection, each other
It complements each other, reduces destruction of the liberation of hydrogen side reaction to coating surface, finally ensure to realize that normal-temperature water solutions obtain densification
There is the gallium nickel alloy coating of metallic luster.It particularly, can by addition dodecyl sodium sulfate or neopelex
Electrode-solution interface tension is reduced, is belonged to for the first time in fact in the application of plating gallium nickel alloy, so that the bubble that side reaction generates
It is unlikely to attachment to grow up on the working electrode (s and coating is caused to deteriorate, reduces even if obtaining bubble and avoid being attached to working electrode
On.Particularly, by the way that working electrode is selected specifically to copper electrode, zinc electrode, aluminium electrode or nickel electrode, so that hydrogen is working
Precipitation on electrode is not especially violent, therefore side reaction is small, is conducive to the plating of gallium nickel alloy.In addition, according to the present invention
Aqueous solution plating gallium nickel alloy method, mixed aqueous solution itself pH of gallium sulfate and nickel sulfate is about 1.5, without adjusting plating
Liquid pH enormously simplifies process compared to sulfuric acid dissolution gallic oxide method.And, the results showed that, the coating that the present invention obtains
In the content of gallium reach 60%, make its surface that there is metallic luster.Further, gallium nickel is electroplated in aqueous solution according to the present invention
The method of alloy can be greatly reduced compared to using ionic liquid as solvent using the deionized water being easily obtained as solvent
Cost.
Detailed description of the invention
Fig. 1 is the three-electrode system plating gallium nickel alloy schematic device of embodiment according to the present invention 1；
Fig. 2 is the three-electrode system plating gallium nickel alloy schematic device of embodiment according to the present invention 2；
Fig. 3 is the surface microscopic topographic of the gallium nickel alloy of embodiment according to the present invention 1；
Fig. 4 is the photo in kind of the gallium nickel alloy of embodiment according to the present invention 1.
Specific embodiment
With reference to the accompanying drawing, presently preferred embodiments of the present invention is provided, and is described in detail.
Embodiment 1
Weigh 13.9g 18 water respectively and close gallium sulfate and 1.84g hydration nickel sulfate and be placed in a beaker, be added about 30ml go from
Sub- water, and magnetic agitation obtains the electroplate liquid of clear to being completely dissolved at 25 DEG C, adds about 3mg dodecyl sulphur
Sour sodium and stir make it completely dissolved, plating solution is finally settled to 50ml with deionized water again, at this point, gallium concentration be 50.57g/
The mass ratio of L, nickel concentration 8.26g/L, gallium element and nickel element is 6.1:1.Then, take 40ml plating solution electrolytic cell 2 (referring to figure
1) in.
Take 1cm2Platinized platinum be auxiliary electrode, take 1cm2Copper sheet as working electrode 4 (referring to Fig. 1), polish and polish copper
Electrode slice, then grease stain is removed with acetone ultrasonic cleaning copper electrode piece 15min, it is rinsed after taking out electrode slice with deionized water, then
Three electrodes are mounted in electrolytic cell 2 (referring to Fig. 1), are working electrode 4, auxiliary electrode 3 and reference electrode 5, three electrodes respectively
It is connected respectively with electrochemical workstation 1 (referring to Fig. 1) the corresponding interface, working electrode 4 and the height of auxiliary electrode 3 are consistent and to just,
Spacing 1.5cm, reference electrode 5 abut working electrode, spacing 3mm.
Electrochemical workstation 1 is opened, is opened magnetic stirring apparatus 7 (referring to Fig. 1), adjusting 6 revolving speed of stirrer is 500rpm, room
Temperature is lower to be electroplated gallium nickel alloy, working electrode potential selection -1V using potentiostatic electrolysis on working electrode 4, and electroplating time is
80min removes working electrode piece after the completion of plating, is rinsed with deionized water and natural air drying obtains gallium nickel alloy coating.
Fig. 1 is the three-electrode system plating gallium nickel alloy schematic device of the present embodiment, and Fig. 3 is obtained according to the present embodiment
Gallium nickel alloy amplification 1000 times after surface microscopic topographic, show the available surface compact of the electro-plating method gallium nickel close
Gold plate；Fig. 4 is the photo in kind of the gallium nickel alloy obtained according to the present embodiment, shows that coating surface has metallic luster.Under
Table 1 is the EDS elemental analysis of the gallium nickel alloy obtained according to the present embodiment as a result, showing that the content of the gallium in coating reaches 60%
More than:
Table 1
| Element | Line type | Apparent concentration | K ratio | Wt% | Wt%Sigma | Standard sample label | Manufacturer's standard |
| C | K linear system | 0.74 | 0.00742 | 8.31 | 0.48 | C | It is |
| Ni | K linear system | 16.78 | 0.16781 | 14.30 | 0.22 | Ni | It is |
| Cu | K linear system | 16.10 | 0.16096 | 14.35 | 0.25 | Cu | It is |
| Ga | L linear system | 32.84 | 0.30787 | 63.04 | 0.43 | GaP | It is |
| Total amount: | 100.00 |
Embodiment 2
Part identical with above-described embodiment 1, details are not described herein.Unlike above-described embodiment 1, the electrification of Fig. 1
It learns work station 1 to be replaced with the potentiostat of Fig. 2, so as to not have to the reference electrode 5 of Fig. 1, auxiliary electrode 3 is connecing potentiostat just
Pole, working electrode 4 connect the cathode of potentiostat, and potentiostat applies the current potential of 1V.
Embodiment 3
18 water conjunction gallium sulfate is weighed respectively and hydration nickel sulfate is placed in a beaker, addition about 30ml deionized water, and
Magnetic agitation obtains the electroplate liquid of clear to being completely dissolved at 30 DEG C, and adding dodecyl sodium sulfate and stirring makes it
Be completely dissolved, plating solution be finally settled to 50ml with deionized water again, at this point, gallium concentration be 47g/L, nickel concentration 7.5g/L,
The mass ratio of gallium element and nickel element is 6.3:1.Dodecyl sodium sulfate is 0.06g/L.Then, 40ml plating solution electrolytic cell 2 is taken
In (referring to Fig. 1).
Take 1cm2Platinized platinum be auxiliary electrode, take 1cm2Zinc metal sheet as working electrode 4 (referring to Fig. 1), polish and polish copper
Electrode slice, then grease stain is removed with acetone ultrasonic cleaning copper electrode piece 15min, it is rinsed after taking out electrode slice with deionized water, then
Three electrodes are mounted in electrolytic cell 2 (referring to Fig. 1), are working electrode 4, auxiliary electrode 3 and reference electrode 5, three electrodes respectively
It is connected respectively with electrochemical workstation 1 (referring to Fig. 1) the corresponding interface, working electrode 4 and the height of auxiliary electrode 3 are consistent and to just,
Spacing 0.5cm, reference electrode 5 abut working electrode, spacing 1mm.
Open electrochemical workstation 1, open magnetic stirring apparatus 7 (referring to Fig. 1), adjustings 6 revolving speed of stirrer be 500rpm, 20
Gallium nickel alloy, working electrode potential selection -0.7V, electroplating time are electroplated on working electrode 4 using potentiostatic electrolysis at DEG C
For 15min, working electrode piece is removed after the completion of plating, is rinsed with deionized water and natural air drying obtains gallium nickel alloy coating.
Embodiment 4
18 water conjunction gallium sulfate is weighed respectively and hydration nickel sulfate is placed in a beaker, addition about 30ml deionized water, and
Magnetic agitation obtains the electroplate liquid of clear to being completely dissolved at 60 DEG C, and adding neopelex and stirring makes
It is completely dissolved, and plating solution is finally settled to 50ml with deionized water again, at this point, gallium concentration be 55g/L, nickel concentration 9g/L,
The mass ratio of gallium element and nickel element is 6.1:1.Neopelex is 0.09g/L.Then, 40ml plating solution electrolytic cell is taken
In 2 (referring to Fig. 1).
Take 1cm2Glass-carbon electrode be auxiliary electrode, take 1cm2Aluminium flake as working electrode 4 (referring to Fig. 1), polish and throw
Light copper electrode piece, then grease stain is removed with acetone ultrasonic cleaning copper electrode piece 15min, it is rinsed after taking out electrode slice with deionized water,
Then three electrodes are mounted in electrolytic cell 2 (referring to Fig. 1), are working electrode 4, auxiliary electrode 3 and reference electrode 5 respectively, three
Electrode is connected with electrochemical workstation 1 (referring to Fig. 1) the corresponding interface respectively, and working electrode 4 and 3 height of auxiliary electrode are consistent and right
Just, spacing 5cm, reference electrode 5 abut working electrode, spacing 3mm.
Open electrochemical workstation 1, open magnetic stirring apparatus 7 (referring to Fig. 1), adjustings 6 revolving speed of stirrer be 500rpm, 30
Gallium nickel alloy, working electrode potential selection -1.2V, electroplating time are electroplated on working electrode 4 using potentiostatic electrolysis at DEG C
For 4min, working electrode piece is removed after the completion of plating, is rinsed with deionized water and natural air drying obtains gallium nickel alloy coating.
Above-described, only presently preferred embodiments of the present invention, the range being not intended to limit the invention, of the invention is upper
Stating embodiment can also make a variety of changes.Made by i.e. all claims applied according to the present invention and description
Simply, equivalent changes and modifications fall within the claims of the invention patent.The not detailed description of the present invention is
Routine techniques content.
Claims (7)
1. a kind of method of aqueous solution plating gallium nickel alloy, which comprises the steps of:
Hydrated sulfuric acid gallium and hydration nickel sulfate are dissolved in the water by S1, and the dodecane that concentration is 0.06g/L to 0.09g/L is added
Base sodium sulfonate or neopelex, obtaining gallium concentration is 47g/L to 55g/L, and nickel concentration is the plating of 7.5g/L to 9g/L
The mass ratio of liquid, gallium element and nickel element is 5.2:1 to 7.3:1；
S2, using copper sheet, zinc metal sheet, aluminium flake or nickel sheet as working electrode, using platinized platinum or glass-carbon electrode as auxiliary electrode, by plating solution
Be placed in electrolytic cell, by working electrode and auxiliary electrode be mounted in electrolytic cell and with electrochemical workstation or potentiostat phase
Even；
S3 is electroplated using potentiostatic electrolysis, under conditions of bath temperature is maintained at 20 DEG C to 30 DEG C, in working electrode
Upper plating obtains gallium nickel alloy coating.
2. the method according to claim 1, wherein hydrated sulfuric acid gallium and hydration nickel sulfate in the step S1
It is dissolved in deionized water under conditions of room temperature is to 60 DEG C, the resistivity of deionized water is 18.2M Ω cm.
3. the method according to claim 1, wherein the step S1 specifically: weigh 18 water and close gallium sulfate
It is placed in a beaker with hydration nickel sulfate, is stirred after deionized water is added, adding dodecyl sodium sulfate and stirring makes it completely
Dissolution, obtains plating solution with deionized water constant volume.
4. the method according to claim 1, wherein the peace of working electrode and auxiliary electrode in the step S2
Dress height is consistent and to just, and the distance between working electrode and auxiliary electrode are 0.5cm to 5cm.
5. reference electrode arrives the method according to claim 1, wherein using reference electrode in the step S2
The distance of working electrode is 1mm to 3mm.
6. the method according to claim 1, wherein in the step S3, the plating current potential control of working electrode
System is between -0.7V to -1.2V.
7. the method according to claim 1, wherein in the step S3, electroplating time is 15min to 4h.
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