CN108660484A - A method of preparing zinc indium alloy powder using electrochemical co-deposition - Google Patents
A method of preparing zinc indium alloy powder using electrochemical co-deposition Download PDFInfo
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- CN108660484A CN108660484A CN201810598702.2A CN201810598702A CN108660484A CN 108660484 A CN108660484 A CN 108660484A CN 201810598702 A CN201810598702 A CN 201810598702A CN 108660484 A CN108660484 A CN 108660484A
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Abstract
A method of zinc indium alloy powder being prepared using electrochemical co-deposition, the present invention relates to the preparation methods of zinc indium alloy powder.The present invention is to solve the technical issues of being unevenly distributed of indium in the zinc load of zinc silver oxide cell.This method：One, with ZnSO4、In2(SO4)3、Na2SO4, EDTA and citric acid prepare deposition liquid；Two, using copper sheet as cathode, depositing system is built as anode using high-purity zine plate；Three, it is deposited under galvanostatic conditions；Four, gained powder under vacuum on copper sheet is dried, obtains zinc indium alloy powder.There is the zinc indium alloy powder of the present invention dendritic structure, indium to be evenly distributed, the zinc silver oxide cell that can be used for preparing.
Description
Technical field
The present invention relates to the preparation methods of zinc indium alloy powder.
Background technology
Zinc-silver oxide battery be it is a kind of there is the higher electrochmical power source than energy and power density, there is stable put
The advantages that piezoelectric voltage, good, nontoxic safety, is applied to civilian and national defence space industry.But zinc-silver oxide battery follows
Ring performance limits its application field, and the stability of zinc electrode has a major impact the cycle performance of zinc-silver oxide battery, zinc
Cathode will appear the feelings of zinc electrode deformation, zinc electrode dendrite, the self-corrosion of zinc electrode, the passivation of zinc electrode in alkaline electrolyte
Shape, these problems will influence the capacity and cycle life of battery, in order to solve the problems, such as zinc electrode these, typically using addition
The method of agent, these additives include：Metal (mercury, lead, tin, indium etc.) and its metal oxide (Bi2O3、SnO2、Ga2O3Deng),
Hydroxide (Ca (OH)2、In(OH)3、Ba(OH)2、Mg(OH)2Deng) and organic molecule (dodecyl benzene sulfonate, dodecane
Base sulfate) etc..After additive is added in zinc electrode, additive can make the corrosion of zinc electrode and overpotential of hydrogen evolution increase, and inhibit
The self-corrosion of zinc electrode and liberation of hydrogen；Additive can make zinc electrode in cyclic process, can make current distribution evenly, inhibit zinc
The generation of dendrite in deposition process.In zinc-silver oxide battery cyclic process, additive can inhibit the deformation of zinc electrode, branch
Brilliant, passivation, self-corrosion, improve the utilization rate of zinc electrode active material.In these additives, other than metal, other additions
The electric conductivity of agent is relatively low, and metal is selected to have the conductivity increased as additive, and mercury, lead, indium in these metallic additions
It, can be as the selection of additive with higher overpotential of hydrogen evolution.But mercury, lead have pollution, gradually due to toxic to environment
It is forbidden to use by people.And indium due to higher overpotential of hydrogen evolution, good electric conductivity, the chemical property of stabilization, to ring
The advantageous properties such as border close friend, thus select indium be added to as additive improved in zinc electrode zinc electrode liberation of hydrogen it is excessively electric, suppression
The self-corrosion of zinc electrode processed and the generation of hydrogen.The mode of zinc electrode is added using indium as additive at present to be mechanical mixture or be total to
Molten and surface cladding, but electrode prepared by these methods, indium are unevenly distributed in zinc electrode, the cycle life of battery still compared with
It is low.
Master's thesis《Zinc indium alloy electro-deposition rule and its application study in high energy alkaline Mn cell》One is disclosed herein
One kind is in hydrosulphate system, and the method for depositing indium or zinc indium alloy layer on copper current collector surface by galvanoplastic should
The copper current collector for plating indium or zinc indium alloy has preferable electrochemical stability in alkaline system.Its plating solution basic composition is
Indium sulfate 8-12g/L, zinc sulfate 18-26g/L are made of based on EDTA the organic compound of hydroxyl, carboxyl, amido
Compound complex agent 60-70g/L, additive 2-5g/L.Since sedimentary is deposited on collector, indium is distributed not in zinc electrode
Uniformly.The technical solution is directly to prepare zinc-silver alloy powder by the method for electro-deposition, and the powder is directly as zinc-silver oxide cell
The active material of zinc electrode, and be not to deposit on a current collector, and indium is generally evenly distributed in entire zinc electricity as additive
In pole；Said program is only distributed on a current collector, and indium is unevenly distributed in zinc electrode.
Invention content
The present invention is to solve the technical issues of being unevenly distributed of indium in the zinc load of zinc-silver oxide battery, and provide
A method of preparing zinc indium alloy powder using electrochemical co-deposition
The method for preparing zinc indium alloy powder using electrochemical co-deposition of the present invention, carries out according to the following steps：
One, ZnSO is pressed4A concentration of 20~40g/L, In2(SO4)3A concentration of 2~6g/L, Na2SO4A concentration of 10~
A concentration of 35~45g/L of 20g/L, EDTA, a concentration of 4~8g/L of citric acid, by ZnSO4、In2(SO4)3、Na2SO4、EDTA
It is added to the water dissolving with citric acid, and it is 4~6 to adjust pH, obtains deposition liquid；
Two, using copper sheet as cathode, using high-purity zine plate as anode, copper sheet is connected with zine plate with conducting wire with power supply, simultaneously
Copper sheet is immersed in zine plate in deposition liquid and keeps being 3~6cm at a distance from the two poles of the earth；Obtain depositing system；
Three, power supply is opened, is deposited under galvanostatic conditions, wherein current density is 50~150mA/cm2, sedimentation time is
5~10min；
Four, gained powder on copper sheet is dried in vacuo at 40~60 DEG C, obtains zinc indium alloy powder.
The present invention obtains electronics in cathode using different kinds of ions and occurs to restore the electrochemical co-deposition method deposited, copper-based
The zinc indium alloy powder with dendritic structure is obtained on plate, indium realizes the uniform of atomic level with zinc in the zinc indium alloy powder
Distribution reaches oneself for the formation and zinc electrode for inhibiting zinc dendrite to make zinc load equably be redistributed in cyclic process
Corrode liberation of hydrogen, to improve cathode active material utilization rate and discharge performance purpose.While this dendritic structure
Zinc indium alloy powder has larger specific surface area, can reduce the internal resistance of cell, improve the discharge capability of battery.The zinc of the present invention
The zinc-silver oxide battery that indium alloy powder can be used for preparing.
Description of the drawings
Fig. 1 is the XRD diffraction patterns of zinc indium alloy in embodiment 1；
Fig. 2 is the SEM figures of zinc indium alloy in embodiment 1；
Fig. 3 is Zn-ef ficiency mapping in zinc indium alloy in embodiment 1；
Fig. 4 is phosphide element mapping in zinc indium alloy in embodiment 1；
Fig. 5 is the linear polarisation curves of deposition zinc powder, coating zinc powder, zinc indium alloy in embodiment 1；
Fig. 6 is the XRD diffraction patterns of zinc indium alloy in embodiment 2；
Fig. 7 is the XRD diffraction patterns of zinc indium alloy in embodiment 3.
Specific implementation mode
Specific implementation mode one：The method for preparing zinc indium alloy powder using electrochemical co-deposition of present embodiment, is pressed
Following steps carry out：
One, ZnSO is pressed4A concentration of 20~40g/L, In2(SO4)3A concentration of 2~6g/L, Na2SO4A concentration of 10~
A concentration of 35~45g/L of 20g/L, EDTA, a concentration of 4~8g/L of citric acid, by ZnSO4、In2(SO4)3、Na2SO4、EDTA
It is added to the water dissolving with citric acid, and it is 4~6 to adjust pH, obtains deposition liquid；
Two, using copper sheet as cathode, using high-purity zine plate as anode, copper sheet is connected with zine plate with conducting wire with power supply, simultaneously
Copper sheet is immersed in zine plate in deposition liquid and keeps being 3~6cm at a distance from the two poles of the earth；Obtain depositing system；
Three, power supply is opened, is deposited under galvanostatic conditions, wherein current density is 50~150mA/cm2, sedimentation time is
5~10min；
Four, gained powder on copper sheet is dried in vacuo at 40~60 DEG C, obtains zinc indium alloy powder.
Specific implementation mode two：The present embodiment is different from the first embodiment in that：In deposition liquid in step 1
ZnSO4A concentration of 25g/L, In2(SO4)3A concentration of 5g/L, Na2SO4A concentration of 15g/L, EDTA a concentration of 40g/L,
A concentration of 5g/L of citric acid, pH 5.It is other same as the specific embodiment one.
Present embodiment is by adding Na2SO4, the conductive capability for improving deposition liquid is strong, increases cathodic polarization so that electrification
It learns and is co-deposited anti-smoothly generation, obtain powdered zinc indium alloy.
Specific implementation mode three：The present embodiment is different from the first and the second embodiment in that：Described in step 2
The quality percent purity of high-purity zine plate is more than 99.99%.It is other the same as one or two specific embodiments.
High-purity zine plate of present embodiment is as sacrificing positive pole.
Specific implementation mode four：Unlike one of present embodiment and specific implementation mode one to three：It will in step 2
Copper sheet and the zine plate of high-purity are by pretreated, and specific preprocessing process is：The zine plate of copper sheet and high-purity is put into
To being impregnated in the KOH solution of a concentration of 1~1.2mol/L, to remove the oil stain of material surface, then wash with distilled water；Again
They are respectively put into the hydrochloric acid solution of 1~1.2mol/L, remove the oxide of material surface, then use distilled water flushing,
To remove the Liquid Residue of material surface.It is other identical as one of specific implementation mode one to three.
Specific implementation mode five：Unlike one of present embodiment and specific implementation mode one to four：It is electric in step 3
Current density is 100mA/cm2, sedimentation time 10min.It is other identical as one of specific implementation mode one to four.
Beneficial effects of the present invention are verified with the following examples：
Embodiment 1：The method for preparing zinc indium alloy powder using electrochemical co-deposition of the present embodiment, according to the following steps into
Row：
One, ZnSO is pressed4A concentration of 20g/L, In2(SO4)3A concentration of 5g/L, Na2SO4A concentration of 10g/L, EDTA
A concentration of 40g/L, citric acid a concentration of 5g/L, by ZnSO4、In2(SO4)3、Na2SO4, EDTA and citric acid be added to
It is dissolved in ionized water, and it is 4 to adjust pH, obtains deposition liquid；
Two, the zine plate for the high-purity that copper sheet and quality percent purity are 99.99% is put into 1mol/L KOH solutions
10min is impregnated, the oil stain of material surface is removed, then wash with distilled water 3 times；They are respectively put into 1mol/L hydrochloric acid again
10min is impregnated in solution, removes the oxide of material surface；With distilled water flushing 3 times, to remove the Liquid Residue of material surface；
Using copper sheet as cathode, using high-purity zine plate as anode, copper sheet is connected with zine plate with conducting wire with power supply, while by copper sheet and zinc
It is 5cm that plate, which is immersed in deposition liquid and keeps the distance at the two poles of the earth, is used in combination clip to fix, obtains depositing system；
Two, power supply is opened, with 100mA/cm2Current density carry out galvanostatic deposition 10min；
Three, the alloy distilled water flushing for obtaining deposition removes deposition liquid Liquid Residue, is put into vacuum drying chamber, 60
It is 12 hours dry at DEG C, obtain zinc indium alloy powder.
The XRD spectrum for the zinc indium alloy powder that the present embodiment obtains is as shown in Figure 1, it will be seen from figure 1 that obtained heavy
Product object is zinc indium alloy.
The SEM for the zinc indium alloy powder that the present embodiment obtains schemes as shown in Fig. 2, figure it is seen that the present embodiment obtains
Zinc indium alloy powder present dendroid, size is at 50~100 μm.
With the elemental distribution for the zinc indium alloy powder that energy disperse spectroscopy (EDS) analysis the present embodiment obtains, Fig. 3 closes for zinc indium
The mapping of Zn-ef ficiency in bronze end, Fig. 4 are the mapping of phosphide element in zinc indium alloy powder, can from Fig. 3 and Fig. 4
Go out phosphide element to be generally evenly distributed in zinc indium alloy.Indium in the zinc indium alloy powder that the present embodiment obtains can be calculated simultaneously
Mass percentage is about 5.07%.
It remakes a contrast test 1 and prepares deposition zinc powder, the contrast test is as different from Example 1：Step 1 is sunk
In is not added in hydrops2(SO4)3, that is, press ZnSO4A concentration of 20g/L, Na2SO4A concentration of 10g/L, EDTA a concentration of 40g/
L, a concentration of 5g/L of citric acid, by ZnSO4、Na2SO4, EDTA and citric acid be add to deionized water dissolving, and adjust pH
It is 4, obtains deposition liquid；It is other same as Example 1, obtain deposition zinc powder as a comparison；
It remakes a contrast test 2 and prepares coating zinc powder, the step of contrast test is as follows：
One, the deposition zinc powder tabletting that will be obtained in contrast test 1 obtains deposition zinc powder piece.
Two, ZnSO4A concentration of 20g/L, In2(SO4)3A concentration of 5g/L, Na2SO4A concentration of 10g/L, EDTA
A concentration of 5g/L of a concentration of 40g/L, citric acid, by ZnSO4、In2(SO4)3、Na2SO4, EDTA and citric acid be added to from
It is dissolved in sub- water, and it is 4 to adjust pH, obtains deposition liquid；
Two, copper sheet and deposition zinc powder piece are put into 1mol/L KOH solutions and impregnate 10min, remove the oil of material surface
Stain, then wash with distilled water 3 times；They are respectively put into 1mol/L hydrochloric acid solutions again and impregnates 10min, removes material table
The oxide in face；With distilled water flushing 3 times, to remove the Liquid Residue of material surface；Using copper sheet as cathode, to deposit zinc powder piece
For anode, copper sheet is connected with deposition zinc powder piece with conducting wire with power supply, while copper sheet and deposition zinc powder piece are immersed in deposition
It in liquid and keeps the distance at the two poles of the earth for 5cm, is used in combination clip to fix, obtains depositing system；
Two, power supply is opened, with 10mA/cm2Current density carry out galvanostatic deposition 10min；
Three, the alloy distilled water flushing for obtaining deposition removes deposition liquid Liquid Residue, is put into vacuum drying chamber, 60
It is 12 hours dry at DEG C, obtain coating zinc powder.
By deposition zinc powder prepared by zinc indium alloy prepared by the present embodiment 1, contrast test 1 and plating prepared by contrast test 2
Layer zinc powder tests linear polarisation curves under the same conditions, and obtained linear polarisation curves figure is as shown in figure 5, can be with from Fig. 5
Find out, under same potential, the liberation of hydrogen current density for depositing zinc powder is more than the liberation of hydrogen current density of coating zinc powder, coating zinc powder
Liberation of hydrogen current density is more than the liberation of hydrogen current density of zinc indium alloy, this illustrates that zinc indium alloy helps to inhibit the hair of evolving hydrogen reaction
Raw, coating zinc powder inhibits liberation of hydrogen effect also better than deposition zinc powder.
Embodiment 2：The method for preparing zinc indium alloy powder using electrochemical co-deposition of the present embodiment, according to the following steps into
Row：
One, ZnSO is pressed4A concentration of 30g/L, In2(SO4)3A concentration of 4g/L, Na2SO4A concentration of 12g/L, EDTA
A concentration of 40g/L, citric acid a concentration of 6g/L, by ZnSO4、In2(SO4)3、Na2SO4, EDTA and citric acid be added to
It is dissolved in ionized water, and it is 4.5 to adjust pH, obtains deposition liquid；
Two, the zine plate for the high-purity that copper sheet and quality percent purity are 99.99% is put into 1.1mol/L KOH solutions
Middle immersion 10min, removes the oil stain of material surface, then wash with distilled water 3 times；They are respectively put into 1mol/L salt again
10min is impregnated in acid solution, removes the oxide of material surface；With distilled water flushing 3 times, to remove the residual of material surface
Liquid；Using copper sheet as cathode, using high-purity zine plate as anode, copper sheet is connected with zine plate with conducting wire with power supply, while by copper sheet
It is immersed in deposition liquid with zine plate and keeps being 5cm at a distance from the two poles of the earth；It is used in combination clip to fix, obtains depositing system；
Two, power supply is opened, with 120mA/cm2Current density carry out galvanostatic deposition 10min；
Three, the alloy distilled water flushing for obtaining deposition removes deposition liquid Liquid Residue, is put into vacuum drying chamber, 60
It is 12 hours dry at DEG C, obtain zinc indium alloy powder.
The XRD spectrum for the zinc indium alloy powder that the present embodiment obtains is as shown in fig. 6, from fig. 6, it can be seen that obtained heavy
Product object is zinc indium alloy.
With the Elemental redistribution for the zinc indium alloy powder that energy disperse spectroscopy (EDS) analysis the present embodiment obtains, it is equal to measure phosphide element
It is even to be distributed in zinc indium alloy.The mass percentage of indium in the zinc indium alloy powder that the present embodiment obtains can be calculated simultaneously
About 3.59%.
Embodiment 3：The method for preparing zinc indium alloy powder using electrochemical co-deposition of the present embodiment, according to the following steps into
Row：
One, ZnSO is pressed4A concentration of 35g/L, In2(SO4)3A concentration of 2g/L, Na2SO4A concentration of 15g/L, EDTA
A concentration of 40g/L, citric acid a concentration of 6g/L, by ZnSO4、In2(SO4)3、Na2SO4, EDTA and citric acid be added to
It is dissolved in ionized water, and it is 5 to adjust pH, obtains deposition liquid；
Two, the zine plate for the high-purity that copper sheet and quality percent purity are 99.99% is put into 1.1mol/L KOH solutions
Middle immersion 10min, removes the oil stain of material surface, then wash with distilled water 3 times；They are respectively put into 1mol/L salt again
10min is impregnated in acid solution, removes the oxide of material surface；With distilled water flushing 3 times, to remove the residual of material surface
Liquid；Using copper sheet as cathode, using high-purity zine plate as anode, copper sheet is connected with zine plate with conducting wire with power supply, while by copper sheet
It is immersed in deposition liquid with zine plate and keeps being 5cm at a distance from the two poles of the earth；It is used in combination clip to fix, obtains depositing system；
Two, power supply is opened, with 150mA/cm2Current density carry out galvanostatic deposition 10min；
Three, the alloy distilled water flushing for obtaining deposition removes deposition liquid Liquid Residue, is put into vacuum drying chamber, 60
It is 12 hours dry at DEG C, obtain zinc indium alloy powder.
The XRD spectrum for the zinc indium alloy powder that the present embodiment obtains is as shown in fig. 7, from figure 7 it can be seen that obtained heavy
Product object is zinc indium alloy.
With the Elemental redistribution for the zinc indium alloy powder that energy disperse spectroscopy (EDS) analysis the present embodiment obtains, it is equal to measure phosphide element
It is even to be distributed in zinc indium alloy.The mass percentage of indium in the zinc indium alloy powder that the present embodiment obtains can be calculated simultaneously
About 2.78%.
Claims (5)
1. a kind of method preparing zinc indium alloy powder using electrochemical co-deposition, it is characterised in that this method according to the following steps into
Row：
One, ZnSO is pressed4A concentration of 20~40g/L, In2(SO4)3A concentration of 2~6g/L, Na2SO4A concentration of 10~20g/
L, a concentration of 4~8g/L of a concentration of 35~45g/L of EDTA, citric acid, by ZnSO4、In2(SO4)3、Na2SO4, EDTA and lemon
Lemon acid is added to the water dissolving, and it is 4~6 to adjust pH, obtains deposition liquid；
Two, using copper sheet as cathode, using high-purity zine plate as anode, copper sheet is connected with zine plate with conducting wire with power supply, while by copper
It is 3~6cm at a distance from the two poles of the earth that piece, which is immersed in deposition liquid and is kept with zine plate,；Obtain depositing system；
Three, power supply is opened, is deposited under galvanostatic conditions, wherein current density is 50~150mA/cm2, sedimentation time be 5~
10min；
Four, gained powder on copper sheet is dried in vacuo at 40~60 DEG C, obtains zinc indium alloy powder.
2. a kind of method preparing zinc indium alloy powder using electrochemical co-deposition according to claim 1, feature exist
ZnSO in deposition liquid in step 14A concentration of 25g/L, In2(SO4)3A concentration of 5g/L, Na2SO4A concentration of 15g/
L, a concentration of 5g/L of a concentration of 40g/L of EDTA, citric acid, pH 5.
3. a kind of method preparing zinc indium alloy powder using electrochemical co-deposition according to claim 1, feature exist
The quality percent purity of high-purity zine plate described in step 2 is more than 99.99%.
4. a kind of method preparing zinc indium alloy powder using electrochemical co-deposition according to claim 1, feature exist
By the zine plate of copper sheet and high-purity it is by pretreated in step 2, specific preprocessing process is：By copper sheet and high-purity
The zine plate of degree, which is put into the KOH solution of a concentration of 1~1.2mol/L, to be impregnated, to remove the oil stain of material surface, then with steaming
Distilled water is cleaned；They are respectively put into the hydrochloric acid solution of 1~1.2mol/L again, removes the oxide of material surface, then
With distilled water flushing, to remove the Liquid Residue of material surface.
5. a kind of method preparing zinc indium alloy powder using electrochemical co-deposition according to claim 1, feature exist
Current density is 100mA/cm in step 32, sedimentation time 10min.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2023167960A1 (en) * | 2022-03-04 | 2023-09-07 | Battelle Memorial Institute | Indium zinc-based alloy anodes forming porous structure for aqueous zinc batteries |
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| CN101451255A (en) * | 2007-08-28 | 2009-06-10 | 罗门哈斯电子材料有限公司 | Electrochemically deposited indium composites |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101451255A (en) * | 2007-08-28 | 2009-06-10 | 罗门哈斯电子材料有限公司 | Electrochemically deposited indium composites |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2023167960A1 (en) * | 2022-03-04 | 2023-09-07 | Battelle Memorial Institute | Indium zinc-based alloy anodes forming porous structure for aqueous zinc batteries |
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