CN108660484B - Method for preparing zinc-indium alloy powder by utilizing electrochemical codeposition - Google Patents

Method for preparing zinc-indium alloy powder by utilizing electrochemical codeposition Download PDF

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CN108660484B
CN108660484B CN201810598702.2A CN201810598702A CN108660484B CN 108660484 B CN108660484 B CN 108660484B CN 201810598702 A CN201810598702 A CN 201810598702A CN 108660484 B CN108660484 B CN 108660484B
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姜再兴
邱胜友
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Harbin Institute of Technology
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Abstract

The invention discloses a method for preparing zinc-indium alloy powder by utilizing electrochemical codeposition, and relates to a preparation method of zinc-indium alloy powder. The invention aims to solve the problem of zinc-oxidationThe indium in the zinc cathode of the silver battery is not uniformly distributed. The method comprises the following steps: one, by ZnSO4、In2(SO4)3、Na2SO4Preparing a deposition solution from EDTA and citric acid; secondly, a deposition system is built by taking the copper sheet as a cathode and taking the high-purity zinc plate as an anode; thirdly, depositing under the condition of constant current; and fourthly, drying the powder obtained on the copper sheet in vacuum to obtain zinc-indium alloy powder. The zinc-indium alloy powder has a dendritic structure, indium is uniformly distributed, and the zinc-indium alloy powder can be used for preparing zinc-silver oxide batteries.

Description

Method for preparing zinc-indium alloy powder by utilizing electrochemical codeposition
Technical Field
The invention relates to a preparation method of zinc-indium alloy powder.
Background
The zinc-silver oxide battery is a chemical power supply with higher specific energy and power density, has the advantages of stable discharge voltage, good safety, no toxicity, no harm and the like, and is applied to the fields of civil use and national defense aerospace. However, the cycle performance of the zinc-silver oxide battery limits the application field, the stability of the zinc electrode has an important influence on the cycle performance of the zinc-silver oxide battery, the zinc electrode deformation, zinc electrode dendrite, zinc electrode self-corrosion and zinc electrode passivation of the zinc electrode can occur in the alkaline electrolyte of the zinc cathode, and the problems affect the capacity and cycle life of the battery, and in order to solve the problems of the zinc electrode, the method of adopting additives is generally adopted, and the additives comprise: metals (mercury, lead, tin, indium, etc.) and their metal oxides (Bi)2O3、SnO2、Ga2O3Etc.), hydroxides (Ca (OH)2、In(OH)3、Ba(OH)2、Mg(OH)2Etc.) and organic molecules (dodecylbenzene sulfonate, dodecyl sulfate), etc. After the additive is added into the zinc electrode, the additive can increase the corrosion and hydrogen evolution overpotential of the zinc electrode and inhibit the self-corrosion and hydrogen evolution of the zinc electrode; the additive can make the current distribution more uniform during the circulation process of the zinc electrode, and inhibit the generation of dendritic crystals during the deposition process of zinc. In the circulation process of the zinc-silver oxide battery, the additive can inhibit the deformation, dendrite, passivation and self-corrosion of the zinc electrode, and improve the utilization rate of active substances of the zinc electrode. Among these additives, metals other than metals have low conductivity, and metals selected as additives have high conductivity, whereas mercury, lead, and indium among these metal additives have high hydrogen evolution overpotentials and can be selected as additives. However, mercury and lead are toxicThe use of the product is gradually prohibited due to environmental pollution. The indium has excellent properties such as higher hydrogen evolution overpotential, good conductivity, stable chemical property, environmental friendliness and the like, so that the indium is selected as an additive to be added into the zinc electrode to improve the hydrogen evolution overpotential of the zinc electrode and inhibit the self-corrosion of the zinc electrode and the generation of hydrogen. At present, the mode of adding indium as an additive into a zinc electrode is mechanical mixing or eutectic melting and surface coating, but the indium of the electrodes prepared by the methods is unevenly distributed in the zinc electrode, and the cycle life of the battery is still low.
The Master thesis, namely the zinc-indium alloy electrodeposition rule and application research thereof in a high-energy alkaline manganese battery, discloses a method for depositing an indium or zinc-indium alloy layer on the surface of a copper current collector in an acidic sulfate system by an electroplating method, wherein the copper current collector plated with indium or zinc-indium alloy has better electrochemical stability in an alkaline system. The basic composition of the plating solution is 8-12g/L of indium sulfate, 18-26g/L of zinc sulfate, 60-70g/L of composite complexing agent which mainly comprises EDTA and is composed of organic compounds containing hydroxyl, carboxyl and amino, and 2-5g/L of additive. Since the deposited layer is deposited on the current collector, the indium is not uniformly distributed in the zinc electrode. The technical scheme is that zinc-silver alloy powder is directly prepared by an electrodeposition method, the powder is directly used as an active substance of a zinc electrode of a zinc-silver battery, is not deposited on a current collector, and indium as an additive is uniformly distributed in the whole zinc electrode; the scheme is only distributed on the current collector, and the indium is unevenly distributed in the zinc electrode.
Disclosure of Invention
The invention aims to solve the technical problem of uneven distribution of indium in a zinc cathode of a zinc-silver oxide battery, and provides a method for preparing zinc-indium alloy powder by utilizing electrochemical codeposition
The method for preparing the zinc-indium alloy powder by utilizing the electrochemical codeposition comprises the following steps of:
one, one and one ZnSO4Has a concentration of 20 to 40g/L, In2(SO4)3Has a concentration of 2 to 6g/L, Na2SO4The concentration of (b) is 35 to up to 20g/L, EDTA45g/L, the concentration of citric acid is 4-8 g/L, and ZnSO is added4、In2(SO4)3、Na2SO4Adding EDTA and citric acid into water for dissolving, and adjusting the pH value to be 4-6 to obtain a deposition solution;
secondly, connecting the copper sheet and the zinc plate with a power supply by using the copper sheet as a cathode and the high-purity zinc plate as an anode through a lead, and simultaneously immersing the copper sheet and the zinc plate into a deposition solution while keeping the distance between the copper sheet and the zinc plate at 3-6 cm; obtaining a deposition system;
thirdly, turning on a power supply, and depositing under the condition of constant current, wherein the current density is 50-150 mA/cm2The deposition time is 5-10 min;
fourthly, drying the powder obtained on the copper sheet in vacuum at the temperature of 40-60 ℃ to obtain the zinc-indium alloy powder.
The invention utilizes an electrochemical codeposition method that various ions obtain electrons at a cathode to generate reduction deposition to obtain zinc-indium alloy powder with a dendritic structure on a copper substrate, and indium and zinc in the zinc-indium alloy powder are uniformly distributed at an atomic level, so that a zinc cathode is uniformly redistributed in a circulating process, and the purposes of inhibiting the formation of zinc dendrites and the self-corrosion hydrogen evolution of a zinc electrode and improving the utilization rate and the discharge performance of active substances of the cathode are achieved. Meanwhile, the zinc-indium alloy powder with the dendritic structure has a large specific surface area, so that the internal resistance of the battery can be reduced, and the discharge capacity of the battery can be improved. The zinc-indium alloy powder of the invention can be used for preparing zinc-silver oxide batteries.
Drawings
FIG. 1 is an XRD diffractogram of the zinc-indium alloy of example 1;
FIG. 2 is an SEM photograph of the zinc-indium alloy of example 1;
FIG. 3 is a surface distribution diagram of Zn element in the Zn-in alloy of example 1;
FIG. 4 is a distribution diagram of the surface distribution of indium in the zinc-indium alloy in example 1;
FIG. 5 is a linear polarization curve of the zinc powder deposited, zinc coated, and zinc-indium alloy of example 1;
FIG. 6 is an XRD diffractogram of the zinc-indium alloy of example 2;
FIG. 7 is an XRD diffractogram of the zinc-indium alloy of example 3.
Detailed Description
The first embodiment is as follows: the method for preparing the zinc-indium alloy powder by utilizing the electrochemical codeposition comprises the following steps of:
one, one and one ZnSO4Has a concentration of 20 to 40g/L, In2(SO4)3Has a concentration of 2 to 6g/L, Na2SO4The concentration of the zinc oxide is 35-45 g/L with the concentration of 10-20 g/L, EDTA, the concentration of the citric acid is 4-8 g/L, and ZnSO is added4、In2(SO4)3、Na2SO4Adding EDTA and citric acid into water for dissolving, and adjusting the pH value to be 4-6 to obtain a deposition solution;
secondly, connecting the copper sheet and the zinc plate with a power supply by using the copper sheet as a cathode and the high-purity zinc plate as an anode through a lead, and simultaneously immersing the copper sheet and the zinc plate into a deposition solution while keeping the distance between the copper sheet and the zinc plate at 3-6 cm; obtaining a deposition system;
thirdly, turning on a power supply, and depositing under the condition of constant current, wherein the current density is 50-150 mA/cm2The deposition time is 5-10 min;
fourthly, drying the powder obtained on the copper sheet in vacuum at the temperature of 40-60 ℃ to obtain the zinc-indium alloy powder.
The second embodiment is as follows: the first difference between the present embodiment and the specific embodiment is: ZnSO in the deposition solution in the first step4Has a concentration of 25g/L, In2(SO4)3Has a concentration of 5g/L, Na2SO4Has a concentration of 15g/L, EDTA of 40g/L, a concentration of citric acid of 5g/L and a pH of 5. The rest is the same as the first embodiment.
In this embodiment, Na is added2SO4The method improves the conductivity of the deposition solution, increases the cathode polarization, enables electrochemical codeposition to occur smoothly, and obtains the powdery zinc-indium alloy.
The third concrete implementation mode: the present embodiment differs from the first or second embodiment in that: and the mass percent purity of the high-purity zinc plate in the step two is more than 99.99%. The other is the same as in the first or second embodiment.
The high purity zinc plate of the present embodiment serves as a sacrificial anode.
The fourth concrete implementation mode: the difference between this embodiment mode and one of the first to third embodiment modes is: in the second step, the copper sheet and the high-purity zinc plate are pretreated, and the specific pretreatment process is as follows: soaking a copper sheet and a high-purity zinc plate in a KOH solution with the concentration of 1-1.2 mol/L to remove oil stains on the surface of the material, and then cleaning with distilled water; and respectively putting the materials into 1-1.2 mol/L hydrochloric acid solution to remove oxides on the surface of the materials, and then washing the materials with distilled water to remove residual liquid on the surface of the materials. The others are the same as in one of the first to third embodiments.
The fifth concrete implementation mode: the difference between this embodiment and one of the first to fourth embodiments is: the current density in the third step is 100mA/cm2The deposition time was 10 min. The other is the same as one of the first to fourth embodiments.
The following examples are used to demonstrate the beneficial effects of the present invention:
example 1: the method for preparing the zinc-indium alloy powder by using the electrochemical codeposition comprises the following steps:
one, one and one ZnSO4Has a concentration of 20g/L, In2(SO4)3Has a concentration of 5g/L, Na2SO4The concentration of (1) is 10g/L, EDTA, the concentration of (40 g/L), the concentration of citric acid is 5g/L, and ZnSO is added4、In2(SO4)3、Na2SO4EDTA and citric acid are added into deionized water to be dissolved, and the pH value is adjusted to 4, so as to obtain deposition liquid;
secondly, putting the copper sheet and the high-purity zinc plate with the mass percentage purity of 99.99% into a 1mol/L KOH solution for soaking for 10min, removing oil stains on the surface of the material, and then cleaning for 3 times by using distilled water; then putting the materials into 1mol/L hydrochloric acid solution respectively to be soaked for 10min, and removing oxides on the surface of the materials; washing with distilled water for 3 times to remove residual liquid on the surface of the material; taking a copper sheet as a cathode, taking a high-purity zinc plate as an anode, connecting the copper sheet and the zinc plate with a power supply through a lead, simultaneously immersing the copper sheet and the zinc plate into a deposition solution, keeping the distance between the copper sheet and the zinc plate to be 5cm, and fixing the copper sheet and the zinc plate by using a clamp to obtain a deposition system;
secondly, turning on the power supply at 100mA/cm2Constant current deposition is carried out for 10min at the current density;
and thirdly, washing the alloy obtained by deposition with distilled water, removing residual liquid of the deposition liquid, putting the alloy into a vacuum drying oven, and drying the alloy for 12 hours at the temperature of 60 ℃ to obtain zinc-indium alloy powder.
The XRD pattern of the zinc-indium alloy powder obtained in this example is shown in fig. 1, and it can be seen from fig. 1 that the obtained deposit is a zinc-indium alloy.
The SEM image of the zinc-indium alloy powder obtained in the present example is shown in FIG. 2, and it can be seen from FIG. 2 that the zinc-indium alloy powder obtained in the present example is dendritic and has a size of 50 to 100 μm.
The elemental distribution of the zinc-indium alloy powder obtained in this example was analyzed by an energy spectrometer (EDS), fig. 3 is a surface distribution diagram of zinc element in the zinc-indium alloy powder, fig. 4 is a surface distribution diagram of indium element in the zinc-indium alloy powder, and it can be seen from fig. 3 and 4 that indium element is uniformly distributed in the zinc-indium alloy. Meanwhile, the mass percentage of indium in the zinc-indium alloy powder obtained in the embodiment can be calculated to be about 5.07%.
A further comparative test 1 was carried out to prepare a deposited zinc powder, which differs from example 1 in that: in is not added into the deposition solution In the first step2(SO4)3I.e. according to ZnSO4Has a concentration of 20g/L, Na2SO4The concentration of (1) is 10g/L, EDTA, the concentration of (40 g/L), the concentration of citric acid is 5g/L, and ZnSO is added4、Na2SO4EDTA and citric acid are added into deionized water to be dissolved, and the pH value is adjusted to 4, so as to obtain deposition liquid; otherwise the same as in example 1, a comparative deposited zinc powder was obtained;
a comparative test 2 was carried out to prepare a zinc-coated powder, the steps of which were as follows:
firstly, the deposited zinc powder obtained in the comparative test 1 is tabletted to obtain a deposited zinc powder tablet.
Di, ZnSO4Has a concentration of 20g/L, In2(SO4)3Has a concentration of 5g/L, Na2SO4The concentration of (1) is 10g/L, EDTA, the concentration of (40 g/L), the concentration of citric acid is 5g/L, and ZnSO is added4、In2(SO4)3、Na2SO4EDTA and citric acid are added into deionized water to be dissolved, and the pH value is adjusted to 4, so as to obtain deposition liquid;
secondly, putting the copper sheet and the deposited zinc powder sheet into a 1mol/L KOH solution for soaking for 10min, removing oil stains on the surface of the material, and then cleaning for 3 times by using distilled water; then putting the materials into 1mol/L hydrochloric acid solution respectively to be soaked for 10min, and removing oxides on the surface of the materials; washing with distilled water for 3 times to remove residual liquid on the surface of the material; taking a copper sheet as a cathode and a deposited zinc powder sheet as an anode, connecting the copper sheet and the deposited zinc powder sheet with a power supply through a lead, simultaneously immersing the copper sheet and the deposited zinc powder sheet into a deposition solution, keeping the distance between the two electrodes to be 5cm, and fixing the two electrodes through a clamp to obtain a deposition system;
secondly, turning on the power supply at 10mA/cm2Constant current deposition is carried out for 10min at the current density;
and thirdly, washing the alloy obtained by deposition with distilled water, removing residual liquid of the deposition liquid, putting the alloy into a vacuum drying oven, and drying the alloy for 12 hours at the temperature of 60 ℃ to obtain the coating zinc powder.
The zinc-indium alloy prepared in this example 1, the deposited zinc powder prepared in the comparative experiment 1, and the coated zinc powder prepared in the comparative experiment 2 were tested for a linear polarization curve under the same conditions, and the obtained linear polarization curve is shown in fig. 5, and it can be seen from fig. 5 that, under the same potential, the hydrogen evolution current density of the deposited zinc powder is greater than that of the coated zinc powder, and the hydrogen evolution current density of the coated zinc powder is greater than that of the zinc-indium alloy, which indicates that the zinc-indium alloy is helpful for suppressing the occurrence of a hydrogen evolution reaction, and the hydrogen evolution suppressing effect of the coated zinc powder is better than that of the deposited zinc powder.
Example 2: the method for preparing the zinc-indium alloy powder by using the electrochemical codeposition comprises the following steps:
one, one and one ZnSO4The concentration of (A) is 30g/L,In2(SO4)3Has a concentration of 4g/L, Na2SO4The concentration of (1) is 12g/L, EDTA, the concentration of (2) is 40g/L, the concentration of citric acid is 6g/L, and ZnSO is added4、In2(SO4)3、Na2SO4EDTA and citric acid are added into deionized water to be dissolved, and the pH value is adjusted to 4.5, so as to obtain deposition liquid;
secondly, putting the copper sheet and the high-purity zinc plate with the mass percentage purity of 99.99% into a 1.1mol/L KOH solution for soaking for 10min, removing oil stains on the surface of the material, and then cleaning for 3 times by using distilled water; then putting the materials into 1mol/L hydrochloric acid solution respectively to be soaked for 10min, and removing oxides on the surface of the materials; washing with distilled water for 3 times to remove residual liquid on the surface of the material; taking a copper sheet as a cathode and a high-purity zinc plate as an anode, connecting the copper sheet and the zinc plate with a power supply by using a lead, and simultaneously immersing the copper sheet and the zinc plate into a deposition solution and keeping the distance between the copper sheet and the zinc plate to be 5 cm; fixing the substrate by a clamp to obtain a deposition system;
secondly, turning on the power supply at 120mA/cm2Constant current deposition is carried out for 10min at the current density;
and thirdly, washing the alloy obtained by deposition with distilled water, removing residual liquid of the deposition liquid, putting the alloy into a vacuum drying oven, and drying the alloy for 12 hours at the temperature of 60 ℃ to obtain zinc-indium alloy powder.
The XRD pattern of the zinc-indium alloy powder obtained in this example is shown in fig. 6, and it can be seen from fig. 6 that the obtained deposit is a zinc-indium alloy.
The elemental distribution of the zinc-indium alloy powder obtained in this example was analyzed by an energy spectrometer (EDS), and it was found that the indium element was uniformly distributed in the zinc-indium alloy. Meanwhile, the mass percentage of indium in the zinc-indium alloy powder obtained in the embodiment can be calculated to be about 3.59%.
Example 3: the method for preparing the zinc-indium alloy powder by using the electrochemical codeposition comprises the following steps:
one, one and one ZnSO4Has a concentration of 35g/L, In2(SO4)3Has a concentration of 2g/L, Na2SO4The concentration of (A) is 15g/L, EDTA, the concentration is 40g/L, and the lemon isThe acid concentration is 6g/L, and ZnSO is added4、In2(SO4)3、Na2SO4EDTA and citric acid are added into deionized water to be dissolved, and the pH value is adjusted to 5, so as to obtain deposition liquid;
secondly, putting the copper sheet and the high-purity zinc plate with the mass percentage purity of 99.99% into a 1.1mol/L KOH solution for soaking for 10min, removing oil stains on the surface of the material, and then cleaning for 3 times by using distilled water; then putting the materials into 1mol/L hydrochloric acid solution respectively to be soaked for 10min, and removing oxides on the surface of the materials; washing with distilled water for 3 times to remove residual liquid on the surface of the material; taking a copper sheet as a cathode and a high-purity zinc plate as an anode, connecting the copper sheet and the zinc plate with a power supply by using a lead, and simultaneously immersing the copper sheet and the zinc plate into a deposition solution and keeping the distance between the copper sheet and the zinc plate to be 5 cm; fixing the substrate by a clamp to obtain a deposition system;
secondly, turning on the power supply at 150mA/cm2Constant current deposition is carried out for 10min at the current density;
and thirdly, washing the alloy obtained by deposition with distilled water, removing residual liquid of the deposition liquid, putting the alloy into a vacuum drying oven, and drying the alloy for 12 hours at the temperature of 60 ℃ to obtain zinc-indium alloy powder.
The XRD pattern of the zinc-indium alloy powder obtained in this example is shown in fig. 7, and it can be seen from fig. 7 that the obtained deposit is a zinc-indium alloy.
The elemental distribution of the zinc-indium alloy powder obtained in this example was analyzed by an energy spectrometer (EDS), and it was found that the indium element was uniformly distributed in the zinc-indium alloy. Meanwhile, the mass percentage of indium in the zinc-indium alloy powder obtained in the embodiment can be calculated to be about 2.78%.

Claims (3)

1. A method for preparing zinc-indium alloy powder by utilizing electrochemical codeposition is characterized by comprising the following steps:
one, one and one ZnSO4Has a concentration of 20 to 40g/L, In2(SO4)3Has a concentration of 2 to 6g/L, Na2SO4The concentration of the zinc oxide is 35-45 g/L with the concentration of 10-20 g/L, EDTA, the concentration of the citric acid is 4-8 g/L, and ZnSO is added4、In2(SO4)3、Na2SO4Adding EDTA and citric acid into water for dissolving, and adjusting the pH value to be 4-6 to obtain a deposition solution;
secondly, connecting the copper sheet and the zinc plate with a power supply by using the copper sheet as a cathode and the high-purity zinc plate as an anode through a lead, and simultaneously immersing the copper sheet and the zinc plate into a deposition solution while keeping the distance between the copper sheet and the zinc plate at 3-6 cm; obtaining a deposition system; the mass percentage purity of the high-purity zinc plate is more than 99.99 percent;
thirdly, turning on a power supply, and depositing under the condition of constant current, wherein the current density is 100-150 mA/cm2The deposition time is 5-10 min;
fourthly, drying the powder obtained on the copper sheet in vacuum at the temperature of 40-60 ℃ to obtain the zinc-indium alloy powder.
2. The method for preparing the Zn-in alloy powder by electrochemical co-deposition as claimed in claim 1, wherein ZnSO in the deposition solution in the first step4Has a concentration of 25g/L, In2(SO4)3Has a concentration of 5g/L, Na2SO4Has a concentration of 15g/L, EDTA of 40g/L, a concentration of citric acid of 5g/L and a pH of 5.
3. The method for preparing the Zn-in alloy powder by electrochemical co-deposition as claimed in claim 1, wherein the copper sheet and the high purity zinc plate in the second step are pre-treated, and the specific pre-treatment process is as follows: soaking a copper sheet and a high-purity zinc plate in a KOH solution with the concentration of 1-1.2 mol/L to remove oil stains on the surface of the material, and then cleaning with distilled water; and respectively putting the materials into 1-1.2 mol/L hydrochloric acid solution to remove oxides on the surface of the materials, and then washing the materials with distilled water to remove residual liquid on the surface of the materials.
CN201810598702.2A 2018-06-12 2018-06-12 Method for preparing zinc-indium alloy powder by utilizing electrochemical codeposition Active CN108660484B (en)

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