CN101144176A - Method for reducing metal and alloy hydroxide gel by hydrogen separated from electrochemistry cathode - Google Patents
Method for reducing metal and alloy hydroxide gel by hydrogen separated from electrochemistry cathode Download PDFInfo
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Abstract
The present invention discloses a method for reducing metal hydroxide gel and metal hydroxide-carbon gel and alloy gel and alloy hydroxide-carbon gel through electrochemical cathodic hydrogen evolution in potassium chloride aqueous solution, and directly further forming and preparing electrode materials of metal and metal-carbon and alloy and alloy-carbon. The electrode prepared by the method can obtain composition of metal: carbon or alloy: carbon with definite proportion, thereby the electrode composition is stable. The tin-carbon gel and tin-cobalt-carbon gel of the present invention is prepared by a definite proportion chemical precipitation method, and overcomes the disadvantage that the coating element content can not be accurately controlled if an electrochemical deposition method is adulterated. The experimental battery consisting of the tin-carbon anode and the lithium sheet cathode prepared with the process has 20 times circulation time and specific capacity of up to 327.4 mAh/g under 0.2 C charging and discharging current; the prepared experimental battery consisting of the tin-cobalt-carbon anode and the lithium sheet cathode has 50 times circulation time specific capacity of up to 278.5 mAh/g under 0.3 C charging and discharging current.
Description
(1) technical field:
The present invention relates to a kind of electrode materials, specifically, be meant a kind of employing electrochemistry cathode hydrogen evolution reducing metal hydroxide gel and metal hydroxides one carbon gel and alloy hydroxide gel and alloy hydroxide-carbon gel in potassium chloride solution, directly prepare the method for metal and metal-carbon and alloy and alloy-carbon electrode material in the moulding of Copper Foil collector previous step.
(2) background technology:
As electrode materials, its preparation method has machine-alloying, sputtering method, electrochemical deposition method etc. with the metal or alloy of doping carbon.The machine-alloying preparation time is long, and it is very difficult to obtain nano-scale level particle; Sputtering method is subjected to the control of working spaces's size, is difficult to use in the actual production line; Though the structure of matter that electrochemical deposition method can the depositing nano size, but adulterated carbon is to be composited by being mingled with by the metal or alloy that carbon particles in the electrolytic solution and galvanic deposit go out in the coating, be difficult to accurately control the content and the distribution of carbon particles in the coating, directly have influence on the circulation ratio of electrode materials performance.
Electrochemistry cathode hydrogen evolution reducing metal hydroxide gel and metal hydroxides-carbon gel and alloy hydroxide gel and alloy hydroxide-carbon gel, directly the method for preparing metal and metal-carbon and alloy and alloy-carbon electrode material in the moulding of Copper Foil collector previous step be with:
1. potassium chloride solution+metal hydroxides gel
2. potassium chloride solution+alloy hydroxide gel
3. potassium chloride solution+metal hydroxides wraps up the colloidal particle of carbon particulate
4. potassium chloride solution+alloy hydroxide wraps up the colloidal particle of carbon particulate
Be deposit solution, utilize electrochemistry cathode hydrogen evolution reduction gel, directly prepare the method for metal and metal-carbon and alloy and alloy-carbon electrode material in the moulding of Copper Foil collector previous step.The advantage of this method is that used gel is to prepare than chemical precipitation method by fixed in the electrolytic solution, and it has guaranteed to obtain definite material composition at electrode surface in the follow-up cathode hydrogen evolution reduction process.Decide to be meant that than chemical precipitation method the mass ratio of the solute of calculating by the mole densitometer is configured solution, obtains sedimentary gel with chemical method then.
(3) summary of the invention:
The objective of the invention is to propose a kind of method for preparing metal and metal-carbon and alloy and alloy-carbon electrode material, be to adopt electro-deposition techniques in potassium chloride solution, to come reducing metal hydroxide gel and metal hydroxides-carbon gel and alloy hydroxide gel and alloy hydroxide-carbon gel, directly prepare the method for metal and metal-carbon and alloy and alloy-carbon electrode material in the moulding of Copper Foil collector previous step by cathode hydrogen evolution.Owing to used gel in the electrolytic solution is to prepare with chemical precipitation method after calculating each composition by fixed, it has guaranteed to obtain definite material composition at electrode surface in the follow-up cathode hydrogen evolution reduction process.Tin-carbon dioxide process carbon electrode that the present invention obtains is anodal and the pour lithium slice negative pole is formed simulated battery, under the 0.2C charge-discharge magnification, and 20 circulation times, specific storage can reach 327.4mAh/g, (mAh represents MAH, and g represents gram).
Tin-Cobalt-carbon dioxide process carbon electrode that the present invention obtains is the anodal simulated battery of forming with lithium sheet negative pole, under the 0.3C charging and discharging currents, and 50 circulation times, specific storage can reach 278.5mAh/g.
The method of the present invention a kind of electrochemistry cathode hydrogen evolution reducing metal and alloy hydroxide gel, it adopts electrochemistry cathode hydrogen evolution reducing metal hydroxide gel and metal hydroxides-carbon gel in potassium chloride solution, directly prepare the method for metal and metal-carbon electrode materials, comprise the following steps: in the moulding of Copper Foil collector previous step
The first step: decide to prepare metal hydroxides gel or metal hydroxides-carbon gel, at first the solution of preparation preparation gel than chemical precipitation method:
(1) solvent is distilled water or deionized water, and solute is tin chloride or tin sulphate, and concentration is at 0.01～5mol/L;
(2) solvent is distilled water or deionized water, and solute is tin chloride or tin sulphate, and concentration is at 0.01～5mol/L, and a certain amount of graphite or carbon black or other carbon particles are placed solution,
It is carried out ultrasonic concussion 30-120 minute; Above solution is under magnetic agitation, and dropping ammonia can obtain coagulant liquid, washs 3-10 time under the whizzer effect through deionized water, makes gel;
Second step: cathode hydrogen evolution reducing metal hydroxide gel and metal hydroxides-carbon gel is metal and metal-carbon;
At first prepare electric depositing solution:
Solvent is distilled water or deionized water, and solute is a conductive agent Repone K, and concentration adds the gel that the first step makes at 0.1～5mol/L, adds hydrochloric acid or sulfuric acid or ammoniacal liquor adjust pH 3-9;
Remove the zone of oxidation on cathode base surface, and carry out the matrix surface activation in dilute sulphuric acid, put into the electric depositing solution that has prepared through second step, big electric current carries out the cathode hydrogen evolution reduction.
The method of the present invention a kind of electrochemistry cathode hydrogen evolution reducing metal and alloy hydroxide gel, it adopts electrochemistry cathode hydrogen evolution reduction alloy hydroxide gel and alloy hydroxide-carbon gel in potassium chloride solution, directly prepare the method for alloy and alloy-carbon electrode material, comprise the following steps: in the moulding of Copper Foil collector previous step
The first step: decide to prepare alloy hydroxide gel or alloy hydroxide-carbon gel, at first the solution of preparation preparation gel than chemical precipitation method:
(1) solvent is distilled water or deionized water, and solute is chlorination Cobalt or sulfuric acid Cobalt or nitric acid Cobalt and tin chloride or tin sulphate, and concentration is at 0.01～5mol/L;
(2) solvent is distilled water or deionized water, and solute is chlorination Cobalt or sulfuric acid Cobalt or nitric acid Cobalt and tin chloride or tin sulphate, and concentration is at 0.01～5mol/L;
A certain amount of graphite or carbon black or other carbon particles are placed solution.It is carried out ultrasonic concussion 30-120 minute;
Above solution is under magnetic agitation, and dropping ammonia can obtain alloy gel liquid, washs 3-10 time under the whizzer effect through deionized water, makes alloy gel;
Second step: cathode hydrogen evolution reduction alloy hydroxide gel and alloy hydroxide-carbon gel are alloy and alloy-carbon;
At first prepare electric depositing solution;
Solvent is distilled water or deionized water, and solute is a conductive agent Repone K, and concentration adds the gel that the first step makes at 0.1～5mol/L, adds hydrochloric acid or sulfuric acid or ammoniacal liquor adjust pH 3-9;
Remove the zone of oxidation on cathode base surface, and carry out the matrix surface activation in dilute sulphuric acid, put into the electric depositing solution that has prepared through second step, big electric current carries out the cathode hydrogen evolution reduction.
Wherein, this decides to prepare than chemical precipitation method the gel of metal hydroxides-carbon or alloy hydroxide-carbon, and its carbon can be graphite, carbon black, hard carbon.
Wherein, the solute in this electric depositing solution is chlorination metal-salt or sulfuric acid metal-salt or nitric acid metal-salt, and concentration is at 0.01～5mol/L.
Wherein, conducting salt is chloride salts such as Repone K, sodium chloride in this electric depositing solution, and concentration is at 0.1～5mol/L.
Wherein, described matrix is meant the metal electrode that nickel foil, aluminium foil, Copper Foil, graphite, nickel plate or platinized platinum are made or is meant porous foam nickel, porous foam copper or porous foam aluminium.
Wherein, the current density of this galvanic deposit is 2-100A/dm
2
Advantage of the present invention: adopt and decide to prepare metal or alloy oxyhydroxide-carbon gel than chemical precipitation method, can accurately control each composition and content ratio in the gel, by follow-up in electrolyzer cathode hydrogen evolution reducing metal oxyhydroxide-carbon or alloy hydroxide-carbon gel be metal-carbon or alloy-carbon, guaranteed that electrode surface obtains material composition and the ratio of determining.This technological operation is easy, and is with low cost.Institute's coating surface that obtains is even, smooth, size, controllable shapes.The specific storage height of gained electrode materials, cycle performance is good.
(4) description of drawings:
Fig. 1 is the charge ratio capacity curve figure when embodiment 1.
Fig. 2 is the charge ratio capacity curve figure when embodiment 2.
(5) embodiment:
The present invention is described in further detail below in conjunction with embodiment.
The present invention is that a kind of employing is decided to prepare metal hydroxides gel and metal hydroxides-carbon gel and alloy hydroxide gel and alloy hydroxide-carbon gel than chemical precipitation method, directly prepares the method for metal and metal-carbon and alloy and alloy-carbon electrode material in the moulding of Copper Foil collector previous step by follow-up cathode hydrogen evolution reduction.Present method comprises the following steps:
The first step: decide to prepare metal hydroxides gel or metal hydroxides-carbon gel or alloy hydroxide gel or alloy hydroxide-carbon gel than chemical precipitation method,
At first preparation prepares the solution of gel:
1. solvent is distilled water or deionized water, and solute is tin chloride or tin sulphate, and concentration is at 0.01～5mol/L, and mol represents mole, and L represents to rise;
2. solvent is distilled water or deionized water, and solute is tin chloride or tin sulphate, and concentration is at 0.01～5mol/L,
A certain amount of graphite or carbon black or other carbon particles are placed solution, it is carried out ultrasonic concussion 30-120 minute;
3. solvent is distilled water or deionized water, and solute is tin chloride or tin sulphate, and concentration is at 0.01～5mol/L; Solute is chlorination Cobalt or sulfuric acid Cobalt or nitric acid Cobalt, and concentration is at 0.01～5mol/L;
4. solvent is distilled water or deionized water, and solute is tin chloride or tin sulphate, and concentration is at 0.01～5mol/L; Solute is chlorination Cobalt or sulfuric acid Cobalt or nitric acid Cobalt, and concentration is at 0.01～5mol/L; A certain amount of graphite or carbon black or other carbon particles are placed solution, it is carried out ultrasonic concussion 30-120 minute;
Above solution is under magnetic agitation, and dropping ammonia can obtain coagulant liquid, washs 3-10 time under the whizzer effect through deionized water, makes gel.
Second step: cathode hydrogen evolution reducing metal hydroxide gel and metal hydroxides-carbon gel and alloy hydroxide gel and alloy hydroxide-carbon gel is metal and metal-carbon and alloy and alloy-carbon,
At first prepare electrodeposit liquid;
Solvent is distilled water or deionized water, and solute is a conductive agent Repone K, and concentration adds the gel that the first step makes at 0.1～5mol/L, adds hydrochloric acid or sulfuric acid or ammoniacal liquor adjust pH 3-9;
Remove the zone of oxidation on cathode base surface, and carry out the matrix surface activation in dilute sulphuric acid, put into the electric depositing solution that has prepared through second step, big electric current carries out the cathode hydrogen evolution reduction;
In the present invention, matrix can be metal electrode or porous foam nickel, porous foam copper or the porous foam aluminium that nickel foil, aluminium foil, Copper Foil, graphite, carbon fiber, nickel plate or platinized platinum are made.
Embodiment 1
The first step: the solution of preparation preparation gel;
Its solution composition is:
Crystallization tin tetrachloride 1mol/L
Hard carbon 0.6 mol/L
After adding deionized water and treating tin tetrachloride dissolving, ultrasonic concussion 5min, under magnetic agitation, dropping ammonia treats that gel all generates then.
More than the gel that makes with deionized water centrifuge washing 5 times, take out gel and place beaker, add deionized water to 1 and rise scale, add 50gKC1, add ammoniacal liquor and transfer pH to 6.0.Make gel through electron probe test, the atomic ratio of Sn:C tabulates 1 as follows:
Table 1JXA8100 electron probe microanalysis (at%)
| Element | Gel (mean value) | Atomic ratio | Coating (mean value) | Atomic ratio |
| C | 34.2885 | 1 | 11.8309 | 1 |
| Sn | 65.6728 | 1.92 | 24.2490 | 2.05 |
| Cu (matrix) | 63.9200 |
In above-mentioned electrolytic solution, do negative electrode with Copper Foil, graphite is done anode, and current density is 25A/dm
2, galvanic deposit is 20 minutes under the magnetic agitation, takes out negative electrode, and washing dries up.Deposition layer is through electron probe test, and the atomic ratio of Sn:C sees Table 1, visible and gel component basically identical.
Use tabletting machine with the Sn-C negative electrode compression moulding of prepared by electrodeposition as positive pole, be negative pole with the lithium sheet, with the capillary polypropylene barrier film, electrolytic solution is 1M LiPF between positive pole and the negative pole
6/ EC+DMC (1: 1), M represents volumetric molar concentration.In being full of the glove box of argon gas, carry out the assembling of simulated battery.Adopt blue electric battery test system at room temperature to carry out the constant current charge-discharge test.The result shows that under the 0.2C charging and discharging currents specific discharge capacity can reach 327.4mAh/g in 20 circulations, sees Fig. 1.
The first step: preparation electric depositing solution;
Take by weighing six hydration cobalt chloride 0.009M (M represent mole) and add the 75ml deionized water dissolving, take by weighing the 0.02M hard carbon and add in the cobalt chloride solution, it is carried out ultrasonic concussion, treat that composition evenly after, under magnetic agitation, slowly dropping ammonia generates green precipitate.Take by weighing crystallization tin tetrachloride 0.011M and add the 100ml deionized water dissolving, it is added in the green gel, continue dropping ammonia 25ml, pH=8.5 makes required gel.More than the gel that makes with deionized water centrifuge washing 10 times, take out and place beaker, add deionized water to 1 and rise scale, add 50gKCl, transfer pH to 6.0 with ammoniacal liquor.
In above-mentioned electrolytic solution, do negative electrode with Copper Foil, graphite is done anode, and current density is 25A/dm
2, galvanic deposit is 20 minutes under the magnetic agitation, takes out negative electrode, and washing dries up.
Using the electrode compression moulding of tabletting machine with above prepared by electrodeposition, as positive pole, is negative pole with the Li sheet, and with the capillary polypropylene barrier film, electrolytic solution is 1M LiPF between positive pole and the negative pole
6/ EC+DMC (1: 1) carries out the assembling of simulated battery in being full of the glove box of argon gas.Adopt blue electric battery test system at room temperature to carry out the constant current charge-discharge test.The result shows under the 0.3C charging current, can reach 278.5/g 50 circulation back specific storagies, under the 0.5C charging current, can reach the 241.5/g (see figure 2) 50 circulation back specific storagies.
Claims (7)
1. the method for electrochemistry cathode hydrogen evolution reducing metal and alloy hydroxide gel, it is characterized in that: it adopts electrochemistry cathode hydrogen evolution reducing metal hydroxide gel and metal hydroxides-carbon gel in potassium chloride solution, directly prepare the method for metal and metal-carbon electrode materials, comprise the following steps: in the moulding of Copper Foil collector previous step
The first step:
Decide to prepare metal hydroxides gel or metal hydroxides-carbon gel, at first the solution of preparation preparation gel than chemical precipitation method:
(1) solvent is distilled water or deionized water, and solute is tin chloride or tin sulphate, and concentration is at 0.01～5mol/L;
(2) solvent is distilled water or deionized water, and solute is tin chloride or tin sulphate, and concentration is at 0.01～5mol/L, and a certain amount of graphite or carbon black or other carbon particles are placed solution, and it is carried out ultrasonic concussion 30-120 minute;
Above solution is under magnetic agitation, and dropping ammonia can obtain coagulant liquid, washs 3-10 time under the whizzer effect through deionized water, makes gel;
Second step: cathode hydrogen evolution reducing metal hydroxide gel and metal hydroxides-carbon gel is metal and metal-carbon;
At first prepare electric depositing solution:
Solvent is distilled water or deionized water, and solute is a conductive agent Repone K, and concentration adds the gel that the first step makes at 0.1～5mol/L, adds hydrochloric acid or sulfuric acid or ammoniacal liquor adjust pH 3-9;
Remove the zone of oxidation on cathode base surface, and carry out the matrix surface activation in dilute sulphuric acid, put into the electric depositing solution that has prepared through second step, big electric current carries out the cathode hydrogen evolution reduction.
2. the method for electrochemistry cathode hydrogen evolution reducing metal and alloy hydroxide gel, it is characterized in that: it adopts electrochemistry cathode hydrogen evolution reduction alloy hydroxide gel and alloy hydroxide-carbon gel in potassium chloride solution, directly prepare the method for alloy and alloy-carbon electrode material, comprise the following steps: in the moulding of Copper Foil collector previous step
The first step: decide to prepare alloy hydroxide gel or alloy hydroxide-carbon gel than chemical precipitation method,
At first preparation prepares the solution of gel:
(1) solvent is distilled water or deionized water, and solute is chlorination Cobalt or sulfuric acid Cobalt or nitric acid Cobalt and tin chloride or tin sulphate, and concentration is at 0.01～5mol/L;
(2) solvent is distilled water or deionized water, and solute is chlorination Cobalt or sulfuric acid Cobalt or nitric acid Cobalt and tin chloride or tin sulphate, and concentration is at 0.01～5mol/L;
A certain amount of graphite or carbon black or other carbon particles are placed solution.It is carried out ultrasonic concussion 30-120 minute;
Above solution is under magnetic agitation, and dropping ammonia can obtain alloy gel liquid, washs 3-10 time under the whizzer effect through deionized water, makes alloy gel;
Second step: cathode hydrogen evolution reduction alloy hydroxide gel and alloy hydroxide-carbon gel are alloy and alloy-carbon;
At first prepare electric depositing solution;
Solvent is distilled water or deionized water, and solute is a conductive agent Repone K, and concentration adds the gel that the first step makes at 0.1～5mol/L, adds hydrochloric acid or sulfuric acid or ammoniacal liquor adjust pH 3-9;
Remove the zone of oxidation on cathode base surface, and carry out the matrix surface activation in dilute sulphuric acid, put into the electric depositing solution that has prepared through second step, big electric current carries out the cathode hydrogen evolution reduction.
3. method according to claim 1 and 2 is characterized in that: this decides to prepare than chemical precipitation method the gel of metal hydroxides-carbon or alloy hydroxide-carbon, and its carbon can be graphite, carbon black, hard carbon.
4. method according to claim 1 and 2 is characterized in that: the solute in its electric depositing solution is chlorination metal-salt or sulfuric acid metal-salt or nitric acid metal-salt, and concentration is at 0.01～5mol/L.
5. method according to claim 4 is characterized in that: conducting salt is chloride salts such as Repone K, sodium chloride in its electric depositing solution, and concentration is at 0.1～5mol/L.
6. method according to claim 1 and 2 is characterized in that: described matrix is meant the metal electrode that nickel foil, aluminium foil, Copper Foil, graphite, nickel plate or platinized platinum are made or is meant porous foam nickel, porous foam copper or porous foam aluminium.
7. method according to claim 1 and 2 is characterized in that: the current density of its galvanic deposit is 2-100A/dm
2
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