CN1761087A - Method for treating surface of copper foil of affluxion body in lithium ion batteries - Google Patents
Method for treating surface of copper foil of affluxion body in lithium ion batteries Download PDFInfo
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- CN1761087A CN1761087A CNA2005101080057A CN200510108005A CN1761087A CN 1761087 A CN1761087 A CN 1761087A CN A2005101080057 A CNA2005101080057 A CN A2005101080057A CN 200510108005 A CN200510108005 A CN 200510108005A CN 1761087 A CN1761087 A CN 1761087A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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- Y02E60/10—Energy storage using batteries
Abstract
The method carries out coarsing, overlay and anticorrosive treatments for surface of copper foil with thickness less than or equal to 18 micro in order to raise cohesive force between copper foil and active materials. Coarsing treatment is that cathodal electrolysis is carried out for copper foil for 5-15s, in coarsing treating liquid composed of copper ion, vitriol, stannous ion and tungsten ion under conditioon of 15-40 deg.C, and certain current density; taking foil out, and using deionized water to wash the treated foil. Overlay treatment is that electrolysis is carried out for copper foil for 30-150s, in overlay treating liquid under condition of 15-40 deg.C, and certain current density. Anticorrosive treatment is carried out in BTA under 15-50 deg.C for 150-300s, and using deionized water to wash the treated foil. Then, drying the foil obtains dendritic structured copper foil in roughness larger than and equalto 0.25 micro, and less than and equal to 0.60 micro.
Description
Technical field
The present invention relates to a kind of process of surface treatment, more particularly, be meant a kind of surface treatment method of a kind of thickness≤18 μ m high-performance lithium batteries with copper foil of affluxion body to electrolytic copper foil.
Background technology
In recent years, miniaturization along with electronic instruments such as mobile phone, video camera, notebook computers, just need the secondary cell of high-energy-density, lithium rechargeable battery, have advantages such as high energy density, favorable charge-discharge cycle performance, discharge voltage plateau height, self-discharge rate are little, memory-less effect, thereby be widely used.
The manufacture process of the electrode plates of lithium ion battery is: obtain being used for the electrode appendix thing attached on positive pole or the negative pole after a certain proportion of positive pole or negative electrode active material, conductive agent, binding agent and solvent are fully mixed, then described electrode appendix thing is coated on collector aluminium foil (positive pole) or the Copper Foil (negative pole) equably, adopt then dry, obtain electrode plates after rolling, cut out division technique.Copper Foil is as the negative current collector material, and its performance directly affects the performance of lithium ion battery.
Undressed Copper Foil is because the surface is more smooth, roughness is low, and electrode appendix thing comes off easily when making electrode plates, and in the transportation use, therefore the perishable variable color of Copper Foil must carry out surface treatment to Copper Foil simultaneously.
Summary of the invention
The objective of the invention is to propose a kind ofly in the sulfuric acid solution of tin, tungsten and copper, to add thiocarbamide and the chloride ion additive carries out the surface-treated method to copper foil of affluxion body in lithium ion batteries, described surface treatment method is handled and antirust treatment process by roughening treatment, covering, make Copper Foil asperities shape evenly and be dendroid, has higher roughness 0.25 μ m≤Ra≤0.60 μ m, and roughened layer light, thereby improve the cohesive force of Copper Foil and active material, improve the better electric energy of lithium ion battery.
The present invention is a kind of surface treatment method of copper foil of affluxion body in lithium ion batteries, and this method may further comprise the steps:
(A) roughening treatment
The Copper Foil of thickness≤18 μ m is put into alligatoring electrolyte carry out the surface coarsening processing, wherein,
Alligatoring electrolyte is the copper ion by concentration 5～20g/l, the sulfuric acid of concentration 50～200g/l, and the tungsten ion of the stannous ion of concentration 0.1～5g/l and concentration 0.001～0.5g/l is formed;
The alligatoring electrolytic condition: in temperature is 15 ℃～40 ℃, and current density is 0.1～0.6A/cm
2Condition under carry out taking out behind 5～15s catholyte, and with washed with de-ionized water 1～5 time;
(B) cover processing
To put into covering electrolyte through the Copper Foil after (A) handles and cover processing; Wherein,
Covering electrolyte is to be the copper ion of 30～80g/l by concentration, and concentration is the sulfuric acid of 50～200g/l, and concentration is that the thiocarbamide of 0.0001～0.1g/l and chloride ion that concentration is 0.01～1g/l are formed;
Cover electrolytic condition: in temperature is 15 ℃～40 ℃, and current density is 0.01～0.3A/cm
2Condition under carry out taking out after 30～150s electrolysis, and with washed with de-ionized water 1～5 time;
(C) antirust processing
To put into antirust treatment fluid through the Copper Foil after (B) handles and carry out antirust processing; Wherein,
Antirust treatment fluid is that concentration is the BTA of 0.5～1.5g/l,
Antirust treatment conditions: be to carry out taking out after 150～300s processing of rust removing under 15 ℃～50 ℃ the condition in temperature, and water cleans 1～5 time, oven dry promptly obtains having the Copper Foil that roughness is 0.25 μ m≤Ra≤0.60 μ m then.
The surface treatment method of described copper foil of affluxion body in lithium ion batteries, the copper foil surface after roughening treatment forms dendritic structure.
The surface treatment method of described copper foil of affluxion body in lithium ion batteries, its antirust treatment fluid are that concentration is the BTA of 1.5g/l, and concentration is the Na of 3g/l
2MoO
42H
2O and concentration are the Na of 0.1g/l
2SiO
39H
2O.
The surface treatment method of described copper foil of affluxion body in lithium ion batteries, its antirust treatment fluid are that concentration is that BTA and the concentration of 1g/l is the Na of 20g/l
2MoO
42H
2O.
Advantage of the present invention: preparation roughening treatment liquid that (1) is an amount of and the condition of passing through the control roughening treatment, make the surface of Copper Foil have dendritic structure, the dendritic structure of this copper foil surface has improved the cohesive force of Copper Foil and active material effectively; (2) in covering processing, add the brightness that a certain amount of thiocarbamide and chloride ion additive have improved copper foil surface; (3) in antirust processing, add a certain amount of Na
2MoO
42H
2O and Na
2SiO
39H
2O or only add Na
2MoO
42H
2O can improve the inhibition cooperative effect of Copper Foil; (4) it is even to obtain the alligatoring shape through processing method of the present invention, and the roughness with better brightness and strong resistance to corrosion is the Copper Foil that is used for affluxion body in lithium ion batteries of 0.25 μ m≤Ra≤0.60 μ m.
Embodiment
The present invention is described in further detail below in conjunction with embodiment.
The present invention relates to a kind of surface treatment method,, reach the adhesion that improves Copper Foil and negative electrode active material by changing the roughness of copper foil surface to copper foil of affluxion body in lithium ion batteries.Comprise roughening treatment, cover and handle and antirust processing, roughening treatment is to be 5～20g/l at copper ion concentration, sulfuric acid concentration is 50～200g/l, stannous ion concentration 0.1～5g/1 and tungsten ion concentration are in the roughening treatment liquid of 0.001～0.5g/l composition, 15 ℃～40 ℃ of temperature, current density is 0.1～0.6A/cm
2Condition under carry out taking out behind 5～15s catholyte, and with washed with de-ionized water 1～5 time; Cover to handle is to be 30～80g/l at copper ion concentration, sulfuric acid concentration is 50～200g/l, thiourea concentration is that 0.0001～0.1g/l and chlorine ion concentration are that 15 ℃～40 ℃ of temperature, current density is 0.01～0.3A/cm in the covering treatment fluid of 0.01～1g/l composition
2Condition under carry out taking out after 30～150s electrolysis, and with washed with de-ionized water 1～5 time; Antirust processing generally is to carry out taking out after 150～300s processing of rust removing in temperature is 15 ℃～50 ℃ BTA, and water cleans 1～5 time, oven dry then, and the roughness that promptly obtains having dendritic structure is the Copper Foil of 0.25 μ m≤Ra≤0.60 μ m.In order to improve the resistance to corrosion of copper foil surface, antirust treatment fluid can be the BTA of 0.5～1.5g/l by concentration also, and concentration is the Na of 0.5～3g/l
2MoO
42H
2O and concentration are the Na of 0.005～0.1g/l
2SiO
39H
2O forms or is that BTA and the concentration of 0.5～1g/l is the Na of 3～20g/l by concentration
2MoO
42H
2O forms.
Embodiment one:
The thick Copper Foil of 18 μ m is placed in the alligatoring electrolyte, is 25 ℃ in temperature, and current density is 0.4A/cm
2Condition under, carry out taking out behind the catholyte of 10s, and with deionized water rinsing 1～5 time; Putting into then and cover electrolyte, is 25 ℃ in temperature, and current density is 0.1A/cm
2Condition under, carry out taking out behind the catholyte of 120s, and with deionized water rinsing 1～5 time; Putting into antirust treatment fluid then, is that take out the antirust processing back of carrying out 300s under 50 ℃ of conditions in temperature, and water cleans 1～5 time, and promptly obtaining the roughness that the surface has dendritic structure after the oven dry is the Copper Foil of Ra=0.44 μ m.
Described alligatoring electrolyte is the copper ion Cu by concentration 10g/l
2+, the sulfuric acid H of concentration 140g/l
2SO
4, the stannous ion Sn of concentration 0.25g/l
2+Tungsten ion W with concentration 0.03g/l
6+Form;
Described covering electrolyte is to be the copper ion Cu of 60g/l by concentration
2+With concentration be the sulfuric acid H of 150g/l
2SO
4, thiourea concentration is 0.0003g/l, chlorine ion concentration is that 0.03g/l forms, and covers and adds a certain amount of thiocarbamide and chloride ion in the electrolyte, can make copper foil surface obtain bright coating preferably;
Described antirust treatment fluid is that concentration is the BTA (benzotriazole) of 1.5g/l.
The Copper Foil for preparing is carried out the corrosivity experiment, and its result sees also shown in the table 1, and extent of corrosion is according to institute's corroded area metering, and corroded area is being the heavy corrosion variable color more than 40%, with symbol " zero " expression; Corroded area is significantly corrosion variable color 5%～40%, with symbol " ● " expression; Corroded area is below 5% being slight corrosion variable color, with symbol " △ " expression.Copper Foil without PROCESS FOR TREATMENT of the present invention, its surface roughness 0.12 μ m, in salt solution, soak after 32 hours and the heavy corrosion variable color occurs, occur significantly corrosion variable color in thermal oxidation (130 ℃ 2 hours) is handled, corrosion rate is 15.06A/cm in acid solution (mass percent concentration of pH=3 is 3% NaCl solution)
2Significantly corrosion variable color appears the Copper Foil after surface treatment method of the present invention is handled soaks 32 hours in salt solution after, occur significantly corrosion variable color in thermal oxidation (130 ℃ 2 hours) is handled, after treatment the corrosion rate of Copper Foil is 11.69A/cm in acid solution (mass percent concentration of pH=3 is 3% NaCl solution)
2
Embodiment two:
The thick Copper Foil of 18 μ m is placed in the alligatoring electrolyte, is 25 ℃ in temperature, and current density is 0.4A/cm
2Condition under, carry out taking out behind the catholyte of 10s, and with deionized water rinsing 1～5 time; Being placed on then in the covering electrolyte, is 25 ℃ in temperature, and current density is 0.1A/cm
2Condition under, carry out taking out behind the catholyte of 120s, and with deionized water rinsing 1～5 time; Putting into antirust treatment fluid then, is that take out the antirust processing back of carrying out 300s under 50 ℃ of conditions in temperature, and water cleans 1～5 time, and promptly obtaining the roughness that the surface has dendritic structure after the oven dry is the Copper Foil of Ra=0.47 μ m.
Described alligatoring electrolyte is the copper ion Cu by concentration 10g/l
2+, the sulfuric acid H of concentration 140g/l
2SO
4, the stannous ion Sn of concentration 0.5g/l
2+Tungsten ion W with concentration 0.03g/l
6+Form;
Described covering electrolyte is to be the copper ion Cu of 60g/l by concentration
2+, concentration is the sulfuric acid H of 150g/l
2SO
4, thiourea concentration is 0.0005g/l, chlorine ion concentration is that 0.04g/l forms;
Described antirust treatment fluid is that concentration is the BTA of 5g/l.
The Copper Foil for preparing is carried out the corrosivity experiment, its result sees also shown in the table 1, significantly corrosion variable color appears the Copper Foil after surface treatment method of the present invention is handled soaks 32 hours in salt solution after, the heavy corrosion variable color occurs in thermal oxidation (130 ℃ 2 hours) is handled, after treatment the corrosion rate of Copper Foil is 9.854A/cm in acid solution (mass percent concentration of pH=3 is 3% NaCl solution)
2
Embodiment three:
The thick Copper Foil of 18 μ m is placed in the alligatoring electrolyte, is 25 ℃ in temperature, and current density is 0.4A/cm
2Condition under, carry out taking out behind the catholyte of 10s, and with deionized water rinsing 1～5 time; Being placed on then in the covering electrolyte, is 25 ℃ in temperature, and current density is 0.1A/cm
2Condition under, carry out taking out behind the catholyte of 120s, and with deionized water rinsing 1～5 time; Putting into antirust treatment fluid then, is that take out the antirust processing back of carrying out 300s under 50 ℃ of conditions in temperature, and water cleans 1～5 time, and promptly obtaining the roughness that the surface has dendritic structure after the oven dry is the Copper Foil of Ra=0.42 μ m.
Described alligatoring electrolyte is the copper ion Cu by concentration 15g/l
2+, the sulfuric acid H of concentration 140g/l
2SO
4, the stannous ion Sn of concentration 0.5g/l
2+Tungsten ion W with concentration 0.05g/l
6+Form;
Described covering electrolyte is to be the copper ion Cu of 60g/l by concentration
2+, concentration is the sulfuric acid H of 150g/l
2SO
4, thiourea concentration is 0.0008g/l, chlorine ion concentration is that 0.04g/l forms;
Described antirust treatment fluid is that concentration is the BTA of 1.5g/l, and concentration is the Na of 3g/l
2MoO
42H
2O and concentration are the Na of 0.1g/l
2SiO
39H
2O.In general antirust treatment fluid BTA (benzotriazole), add a certain amount of Na
2MoO
4And Na
2SiO
3Can alleviate the inhibition cooperative effect of Copper Foil, improve the resistance to corrosion of Copper Foil.
The Copper Foil for preparing is carried out the corrosivity experiment, its result sees also shown in the table 1, significantly corrosion variable color appears the Copper Foil after surface treatment method of the present invention is handled soaks 32 hours in salt solution after, the heavy corrosion variable color occurs in thermal oxidation (130 ℃ 2 hours) is handled, after treatment the corrosion rate of Copper Foil is 13.23A/cm in acid solution (mass percent concentration of pH=3 is 3% NaCl solution)
2
Embodiment four:
The thick Copper Foil of 18 μ m is placed in the alligatoring electrolyte, is 25 ℃ in temperature, and current density is 0.4A/cm
2Condition under, carry out taking out behind the catholyte of 10s, and with deionized water rinsing 1～5 time; Being placed on then in the covering electrolyte, is 25 ℃ in temperature, and current density is 0.1A/cm
2Condition under, carry out taking out behind the catholyte of 120s, and with deionized water rinsing 1～5 time; Putting into antirust treatment fluid then, is that take out the antirust processing back of carrying out 300s under 50 ℃ of conditions in temperature, and water cleans 1～5 time, and promptly obtaining the roughness that the surface has dendritic structure after the oven dry is the Copper Foil of Ra=0.38 μ m.
Described alligatoring electrolyte is the copper ion Cu by concentration 15g/1
2+, the sulfuric acid H of concentration 140g/l
2SO
4, the stannous ion Sn of concentration 0.4g/l
2+Tungsten ion W with concentration 0.06g/l
6+Form;
Described covering electrolyte is to be the copper ion Cu of 60g/l by concentration
2+, concentration is the sulfuric acid H of 150g/l
2SO
4, thiourea concentration is 0.0008g/l, chlorine ion concentration is that 0.04g/l forms;
Described antirust treatment fluid is that concentration is that BTA and the concentration of 1g/l is the Na of 20g/l
2MoO
42H
2O.BTA and Na
2MoO
4In anti-copper material variable color, show good inhibition cooperative effect.
The Copper Foil for preparing is carried out the corrosivity experiment, its result sees also shown in the table 1, significantly corrosion variable color appears the Copper Foil after surface treatment method of the present invention is handled soaks 32 hours in salt solution after, the heavy corrosion variable color occurs in thermal oxidation (130 ℃ 2 hours) is handled, after treatment the corrosion rate of Copper Foil is 8.092A/cm in acid solution (mass percent concentration of pH=3 is 3% NaCl solution)
2
Embodiment five:
The thick Copper Foil of 18 μ m is placed in the alligatoring electrolyte, is 25 ℃ in temperature, and current density is 0.4A/cm
2Condition under, carry out taking out behind the catholyte of 10s, and with deionized water rinsing 1～5 time; Being placed on then in the covering electrolyte, is 25 ℃ in temperature, and current density is 0.1A/cm
2Condition under, carry out taking out behind the catholyte of 120s, and with deionized water rinsing 1～5 time; Then be placed in the antirust pretreatment fluid, in temperature is to take out behind the preliminary treatment 200s under 50 ℃ of conditions, and then put into antirust treatment fluid, in temperature is that take out the antirust processing back of carrying out 300s under 50 ℃ of conditions, and water cleans 1～5 time, and promptly obtaining the roughness that the surface has dendritic structure after the oven dry is the Copper Foil of Ra=0.50 μ m.
Described alligatoring electrolyte is the copper ion Cu by concentration 12g/l
2+, the sulfuric acid H of concentration 140g/l
2SO
4, the stannous ion Sn of concentration 0.8g/l
2+Tungsten ion W with concentration 0.03g/l
6+Form;
Described covering electrolyte is to be the copper ion Cu of 60g/l by concentration
2+, concentration is the sulfuric acid H of 150g/l
2SO
4, thiourea concentration is 0.0008g/l, chlorine ion concentration is that 0.04g/l forms;
Described antirust pretreatment fluid is that concentration is the oxalic acid of 40g/l, and concentration is the BTA of 0.2g/l and the H of 10ml/l
2O
2
Described antirust treatment fluid is that concentration is the BTA of 1.5g/l.
The Copper Foil for preparing is carried out the corrosivity experiment, its result sees also shown in the table 1, slight corrosion variable color appears the Copper Foil after surface treatment method of the present invention is handled soaks 32 hours in salt solution after, occur slight corrosion variable color in thermal oxidation (130 ℃ 2 hours) is handled, after treatment the corrosion rate of Copper Foil is 9.277A/cm in acid solution (mass percent concentration of pH=3 is 3% NaCl solution)
2
According to the present invention to being used for the surface treatment method of affluxion body in lithium ion batteries, thickness≤18 μ m high performance electrolytic copper foils, it is characterized in that having roughening treatment, cover and handle and antirust treatment process, has higher roughness 0.25 μ m≤Ra≤0.60 μ m, the asperities shape evenly and be dendritic structure (adopting ESEM equipment to observe), and matsurface light, rough layer has good adhesion, has good anti-rust properties simultaneously.
The corrosivity experimental result of each embodiment of table 1
| Copper Foil | Example one | Example two | Example three | Example four | Example five | |
| Roughness Ra (μ m) | 0.12 | 0.44 | 0.47 | 0.42 | 0.38 | 0.50 |
| Uniformity | Evenly | Evenly | Evenly | Evenly | Evenly | Evenly |
| Saline sook 32 hours | ○ | ● | ● | ● | ● | △ |
| Thermal oxidation test (130 ℃ 2 hours) | ● | ● | ○ | ○ | ○ | △ |
| Corrosion rate in the acid solution (A/cm) | 15.06 | 11.69 | 9.854 | 13.23 | 8.092 | 9.277 |
Claims (4)
1, a kind of surface treatment method of copper foil of affluxion body in lithium ion batteries is characterized in that may further comprise the steps:
(A) roughening treatment
The Copper Foil of thickness≤18 μ m is put into alligatoring electrolyte carry out the surface coarsening processing, wherein,
Alligatoring electrolyte is the copper ion by concentration 5～20g/l, the sulfuric acid of concentration 50～200g/l, and the tungsten ion of the stannous ion of concentration 0.1～5g/l and concentration 0.001～0.5g/l is formed;
The alligatoring electrolytic condition: in temperature is 15 ℃～40 ℃, and current density is 0.1～0.6A/cm
2Condition under carry out taking out behind 5～15s catholyte, and with washed with de-ionized water 1～5 time;
(B) cover processing
To put into covering electrolyte through the Copper Foil after (A) handles and cover processing; Wherein,
Covering electrolyte is to be the copper ion of 30～80g/l by concentration, and concentration is the sulfuric acid of 50～200g/l, and concentration is that the thiocarbamide of 0.0001～0.1g/l and chloride ion that concentration is 0.01～1g/l are formed;
Cover electrolytic condition: in temperature is 15 ℃～40 ℃, and current density is 0.01～0.3A/cm
2Condition under carry out taking out after 30～150s electrolysis, and with washed with de-ionized water 1～5 time;
(C) antirust processing
To put into antirust treatment fluid through the Copper Foil after (B) handles and carry out antirust processing; Wherein,
Antirust treatment fluid is that concentration is the BTA of 0.5～1.5g/l,
Antirust treatment conditions: be to carry out taking out after 150～300s processing of rust removing under 15 ℃～50 ℃ the condition in temperature, and water cleans 1～5 time, oven dry promptly obtains having the Copper Foil that roughness is 0.25 μ m≤Ra≤0.60 μ m then.
2, the surface treatment method of copper foil of affluxion body in lithium ion batteries according to claim 1 is characterized in that: the copper foil surface after roughening treatment forms dendritic structure.
3, the surface treatment method of copper foil of affluxion body in lithium ion batteries according to claim 1 is characterized in that: described antirust treatment fluid is that concentration is the BTA of 1.5g/l, and concentration is the Na of 3g/l
2MoO
42H
2O and concentration are the Na of 0.1g/l
2SiO
39H
2O.
4, the surface treatment method of copper foil of affluxion body in lithium ion batteries according to claim 1 is characterized in that: described antirust treatment fluid is that concentration is that BTA and the concentration of 1g/l is the Na of 20g/l
2MoO
42H
2O.
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