CN101656329A - Preparation method of inorganic aqueous solution lithium ion battery - Google Patents

Preparation method of inorganic aqueous solution lithium ion battery Download PDF

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Publication number
CN101656329A
CN101656329A CN200910023978A CN200910023978A CN101656329A CN 101656329 A CN101656329 A CN 101656329A CN 200910023978 A CN200910023978 A CN 200910023978A CN 200910023978 A CN200910023978 A CN 200910023978A CN 101656329 A CN101656329 A CN 101656329A
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ion battery
lithium ion
aqueous solution
preparation
furnace
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CN101656329B (en
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赵铭姝
郑青阳
汪飞
代维民
彭坤
宋晓平
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Xian Jiaotong University
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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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries
    • 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50—Manufacturing or production processes characterised by the final manufactured product

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Abstract

The invention discloses a preparation method of an inorganic aqueous solution lithium ion battery, comprising: 1. adopting inorganic lithium salt aqueous solution to replace common lithium salt organic binary (or multielement) electrolyte to design a novel lithium ion battery; and 2. adopting solid phase section calcination method to prepare lithium cobaltoxide and lithium vanadate battery materials, which feature easy control and simple operation. Compared with an organic electrolyte lithium ion battery, the aqueous solution lithium ion battery radically solves potential safety hazards, and is not required to be assembled in rigorously dry environment and protective atmosphere, electrolyte is cheap and electrical conductivity of ions is two orders of magnitude higher than that of organicelectrolyte; what is more important, the aqueous solution lithium ion battery is environment-friendly and is a real green energy battery. The voltage of the aqueous solution lithium ion battery givenin the invention is 1.0-1.2V, and the specific discharge capacity thereof is 95-110mAh*g<-1>.

Description

A kind of preparation method of inorganic aqueous solution lithium ion battery
Technical field
The invention belongs to material preparation method, particularly a kind of preparation method of inorganic aqueous solution lithium ion battery.
Background technology
As a class new type lithium ion secondary cell, the aqueous solution of employing inorganic lithium salt replaces the organic electrolyte of traditional lithium ion battery, fundamentally eliminated because of the reaction of organic electrolyte and electrode material and formed potential safety hazards such as burning that dendrite may cause, blast, had bigger competition potential in low-voltage battery (as lead-acid battery, alkaline Mn cell, nickel-cadmium cell, Ni-MH battery etc.) application.
Preparation method about cobalt acid lithium, lithium vanadate lithium ion battery material has had a lot of bibliographical informations, but, adopt chemical coprecipitation, sol-gal process, latex seasoning, ultrasonic wave sputtering method, high-temperature decomposition etc. for obtaining good dispersion, not having the battery material of reuniting more.Yet the operating process of these methods is more complicated all, and especially some technology is wayward, hinders its industrialization process.The most important thing is, can not realize continuous preparation, preparation process can cause in various degree pollution to environment.The advantage of solid phase multi-steps sintering method is pollution-free, reaction temperature and, temperature be easy to control, particle size be easy to control, course of reaction does not contain poisonous composition to the human body nonhazardous in the reaction system.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of inorganic aqueous solution lithium ion battery.The electrolyte cheapness of this method and ionic conductivity are than high two orders of magnitude of organic electrolyte, and aqueous solution lithium ion battery is environmentally friendly, are real green energy resource batteries.
Technical scheme of the present invention is achieved in that
1) preparation positive electrode:
Be in molar ratio (1.02～1.06): 1 takes by weighing Li 2CO 3And Co 2O 3Raw material is with the Li that takes by weighing 2CO 3And Co 2O 3Raw material is put into ball grinder, the agate mill ball of packing into, and ball milling 20-24 hour, obtain mixed-powder, its mould of packing into is placed press model machine, under the pressure of 15-20MPa, pressurize 10-15 minute, the demoulding obtained cylindrical piece; The cylindrical piece that obtains is placed porcelain boat, put into resistance wire horizontal pipe heating furnace, adopt following calcination process: with 3-5 ℃ of min -1Heating rate be heated to 300-350 ℃, be incubated 12-15 hour; Cool to room temperature with the furnace; Again with 3-5 ℃ of min -1Heating rate be heated to 750-800 ℃, be incubated 12-15 hour; Cool to room temperature with the furnace, obtain LiCoO 2Sample;
2) preparation negative material:
Choose Li 2CO 3And V 2O 5Be raw material, according to (1.02～1.06): 3 mol ratios claim sample, and above-mentioned raw materials is put into ball grinder, the agate mill ball of packing into, ball milling 20-24 hour, obtain mixed-powder, its mould of packing into is placed press model machine, under the pressure of 15-20MPa, pressurize 10-15 minute, the demoulding obtained cylindrical piece; The cylindrical piece that obtains is placed porcelain boat, put into resistance wire horizontal pipe heating furnace, adopt following calcination process: with 3-5 ℃ of min -1Heating rate be heated to 650-680 ℃, be incubated 10-12 hour; Cool to room temperature with the furnace; Again with 3-5 ℃ of min -1Heating rate be heated to 300-350 ℃, be incubated 8-10 hour; Cool to room temperature with the furnace, obtain LiV 3O 8Sample;
3) preparation technology of electrode slice:
A. with synthetic LiCoO 2Sample or LiV 3O 8Sample mixes with acetylene black respectively, obtains black powder, polyvinylidene fluoride is dissolved in the N-methyl pyrrolidone that dewaters then, obtains solution A, black powder is mixed obtaining black paste with solution A;
Wherein, LiCoO 2Sample or LiV 3O 8Sample is 80: 10: 10 or 85: 10: 5 with the mass ratio of acetylene black, polyvinylidene fluoride respectively;
B. black paste is coated on the nickel screen with doctor blade, under vacuum condition 85-100 ℃ dry 8-10 hour, obtain LiCoO respectively 2Positive electrical pole piece or LiV 3O 8The negative electricity pole piece;
4) with LiCoO 2Electrode slice is that water lithium electricity is anodal, LiV 3O 8Electrode slice is a negative pole, is contained in the saturated LiNO of 20ml 3In the beaker of electrolyte, the pH=5-6 of its electrolyte, positive/negative plate immerses, and keeps the spacing of 0.5-1cm, can obtain inorganic aqueous solution lithium ion battery.
Described resistance wire horizontal pipe heating furnace is a Fe-Cr-Al silk calandria stove.
The present invention one is that organic binary (or polynary) electrolyte that adopts the inorganic lithium salt aqueous solution to substitute lithium salts commonly used designs new type lithium ion battery, the 2nd, and adopt solid phase multi-steps sintering legal system to be equipped with cobalt acid lithium, lithium vanadate battery material, be easy to control, simple to operate.Compare with the organic electrolyte lithium ion battery, aqueous solution lithium ion battery has thoroughly solved potential safety hazard, needn't assembled battery under the drying of harshness and protective atmosphere, and electrolyte cheapness and ionic conductivity are than high two orders of magnitude of organic electrolyte.More importantly being that aqueous solution lithium ion battery is environmentally friendly, is real green energy resource battery.
The voltage of the aqueous solution lithium ion battery that the present invention provides is 1.0-1.2V, and specific discharge capacity is 95-110mAhg -1
Embodiment
Embodiment one:
The preparation positive electrode.Be 1.02: 1 raw materials weighing Li in molar ratio 2CO 3And Co 2O 3Above-mentioned raw materials puts it into ball grinder, and the agate mill ball of packing into placed the ball mill ball milling 20 hours, obtains mixed-powder, and its mould of packing into is placed press model machine, under the pressure of 15MPa, pressurize 10 minutes, the demoulding obtains cylindrical piece; Cylindrical piece is placed porcelain boat, put into resistance wire horizontal pipe heating furnace, adopt following calcination process: with 3 ℃ of min -1Heating rate be heated to 300 ℃, be incubated 12 hours; Cool to room temperature with the furnace; Again with 3 ℃ of min -1Heating rate be heated to 750 ℃, be incubated 12 hours; Cool to room temperature with the furnace, obtain LiCoO 2Sample.
The preparation negative material.Take by weighing raw material Li according to 1.02: 3 mol ratios 2CO 3And V 2O 5, above-mentioned raw materials is put into ball grinder, the agate mill ball of packing into placed the ball mill ball milling 20 hours, obtained mixed-powder, and its mould of packing into is placed press model machine, under the pressure of 15MPa, pressurize 10 minutes, the demoulding obtains cylindrical piece; Cylindrical piece is placed porcelain boat, put into resistance wire horizontal pipe heating furnace, adopt following calcination process: with 3 ℃ of min -1Heating rate be heated to 680 ℃, be incubated 10 hours; Cool to room temperature with the furnace; Again with 3 ℃ of min -1Heating rate be heated to 350 ℃, be incubated 8 hours; Cool to room temperature with the furnace, obtain LiV 3O 8Sample.
Kynoar (PVDF) is dissolved in the binding agent that is mixed with pulpous state in N methyl pyrrolidone (NMP) solution by the concentration of 0.2mol/l, again with active material LiCoO 2And LiV 3O 8Powder, conductive agent (acetylene black), binding agent mix by 80: 10: 10 (W/W), it are dissolved in the binding agent stir.Then it is applied on the pole piece, 100 ℃ of following vacuumize 10 hours obtains anodal and negative electricity pole piece.
The saturated LiNO of preparation 1M, pH=5 3Solution is the electrolyte of battery system.
Experimental cell is to carry out in a beaker that 20ml electrolyte is housed, and is assembled into the lithium ion battery of aqueous solution electrolysis liquid at last.The voltage of this water lithium electricity system is 1.0V, and specific discharge capacity is 95mAhg -1
Embodiment two:
The preparation positive electrode.Be 1.03: 1 raw materials weighing Li in molar ratio 2CO 3And Co 2O 3Above-mentioned raw materials puts it into ball grinder, and the agate mill ball of packing into placed the ball mill ball milling 24 hours, obtains mixed-powder, and its mould of packing into is placed press model machine, under the pressure of 20MPa, pressurize 15 minutes, the demoulding obtains cylindrical piece; Cylindrical piece is placed porcelain boat, put into resistance wire horizontal pipe heating furnace, adopt following calcination process: with 5 ℃ of min -1Heating rate be heated to 350 ℃, be incubated 12 hours; Cool to room temperature with the furnace; Again with 5 ℃ of min -1Heating rate be heated to 800 ℃, be incubated 12 hours; Cool to room temperature with the furnace, obtain LiCoO 2Sample.
The preparation negative material.Take by weighing raw material Li according to 1.03: 3 mol ratios 2CO 3And V 2O 5, above-mentioned raw materials is put into ball grinder, the agate mill ball of packing into placed the ball mill ball milling 24 hours, obtained mixed-powder, and its mould of packing into is placed press model machine, under the pressure of 20MPa, pressurize 15 minutes, the demoulding obtains cylindrical piece; Cylindrical piece is placed porcelain boat, put into resistance wire horizontal pipe heating furnace, adopt following calcination process: with 5 ℃ of min -1Heating rate be heated to 680 ℃, be incubated 12 hours; Cool to room temperature with the furnace; Again with 5 ℃ of min -1Heating rate be heated to 350 ℃, be incubated 10 hours; Cool to room temperature with the furnace, obtain LiV 3O 8Sample.
PVDF is dissolved in the binding agent that is mixed with pulpous state in the nmp solution by the concentration of 0.2mol/l, again with active material LiCoO 2And LiV 3O 8Powder, conductive agent (acetylene black), binding agent mix by 85: 10: 5 (W/W), it are dissolved in the binding agent stir.Then it is applied on the pole piece, 85 ℃ of following vacuumize 10 hours obtains anodal and negative electricity pole piece.
The saturated LiNO of preparation 1M 3Solution (pH=5.5) is the electrolyte of battery system.
Experimental cell is to carry out in a beaker that 20ml electrolyte is housed, and is assembled into the lithium ion battery of aqueous solution electrolysis liquid at last.The voltage of this water lithium electricity system is 1.0V, and specific discharge capacity is 100mAhg -1
Embodiment three
The preparation positive electrode.Be 1.05: 1 raw materials weighing Li in molar ratio 2CO 3And Co 2O 3Above-mentioned raw materials puts it into ball grinder, and the agate mill ball of packing into placed the ball mill ball milling 20 hours, obtains mixed-powder, and its mould of packing into is placed press model machine, under the pressure of 15MPa, pressurize 10 minutes, the demoulding obtains cylindrical piece; Cylindrical piece is placed porcelain boat, put into resistance wire horizontal pipe heating furnace, adopt following calcination process: with 3 ℃ of min -1Heating rate be heated to 300 ℃, be incubated 12 hours; Cool to room temperature with the furnace; Again with 3 ℃ of min -1Heating rate be heated to 750 ℃, be incubated 12 hours; Cool to room temperature with the furnace, obtain LiCoO 2Sample.
The preparation negative material.Take by weighing raw material Li according to 1.05: 3 mol ratios 2CO 3And V 2O 5, above-mentioned raw materials is put into ball grinder, the agate mill ball of packing into placed the ball mill ball milling 20 hours, obtained mixed-powder, and its mould of packing into is placed press model machine, under the pressure of 15MPa, pressurize 10 minutes, the demoulding obtains cylindrical piece; Cylindrical piece is placed porcelain boat, put into resistance wire horizontal pipe heating furnace, adopt following calcination process: with 3 ℃ of min -1Heating rate be heated to 650 ℃, be incubated 10 hours; Cool to room temperature with the furnace; Again with 3 ℃ of min -1Heating rate be heated to 300 ℃, be incubated 8 hours; Cool to room temperature with the furnace, obtain LiV 3O 8Sample.
PVDF is dissolved in the binding agent that is mixed with pulpous state in the nmp solution by the concentration of 0.2mol/l, again with active material LiCoO 2And LiV 3O 8Powder, conductive agent (acetylene black), binding agent mix by 80: 10: 10 (W/W), it are dissolved in the binding agent stir.Then it is applied on the pole piece, 100 ℃ of following vacuumize 10 hours obtains anodal and negative electricity pole piece.
The saturated LiNO of preparation 1M, pH=5.5 3Solution is the electrolyte of battery system.
Experimental cell is to carry out in a beaker that 20ml electrolyte is housed, and is assembled into the lithium ion battery of aqueous solution electrolysis liquid at last.The voltage of this water lithium electricity system is 1.2V, and specific discharge capacity is 105mAhg -1
Embodiment four
The preparation positive electrode.Be 1.06: 1 raw materials weighing Li in molar ratio 2CO 3And Co 2O 3Above-mentioned raw materials puts it into ball grinder, and the agate mill ball of packing into placed the ball mill ball milling 24 hours, obtains mixed-powder, and its mould of packing into is placed press model machine, under the pressure of 20MPa, pressurize 15 minutes, the demoulding obtains cylindrical piece; Cylindrical piece is placed porcelain boat, put into resistance wire horizontal pipe heating furnace, adopt following calcination process: with 5 ℃ of min -1Heating rate be heated to 350 ℃, be incubated 15 hours; Cool to room temperature with the furnace; Again with 5 ℃ of min -1Heating rate be heated to 800 ℃, be incubated 15 hours; Cool to room temperature with the furnace, obtain LiCoO 2Sample.
The preparation negative material.Take by weighing raw material Li according to 1.06: 3 mol ratios 2CO 3And V 2O 5, above-mentioned raw materials is put into ball grinder, the agate mill ball of packing into placed the ball mill ball milling 24 hours, obtained mixed-powder, and its mould of packing into is placed press model machine, under the pressure of 20MPa, pressurize 15 minutes, the demoulding obtains cylindrical piece; Cylindrical piece is placed porcelain boat, put into resistance wire horizontal pipe heating furnace, adopt following calcination process: with 5 ℃ of min -1Heating rate be heated to 680 ℃, be incubated 12 hours; Cool to room temperature with the furnace; Again with 5 ℃ of min -1Heating rate be heated to 350 ℃, be incubated 10 hours; Cool to room temperature with the furnace, obtain LiV 3O 8Sample.
PVDF is dissolved in the binding agent that is mixed with pulpous state in the nmp solution by the concentration of 0.2mol/l, again with active material LiCoO 2And LiV 3O 8Powder, conductive agent (acetylene black), binding agent mix by 85: 10: 5 (W/W), it are dissolved in the binding agent stir.Then it is applied on the pole piece, 90 ℃ of following vacuumize 10 hours obtains anodal and negative electricity pole piece.
The saturated LiNO of preparation 1M, pH=6 3Solution is the electrolyte of battery system.
Experimental cell is to carry out in a beaker that 20ml electrolyte is housed, and is assembled into the lithium ion battery of aqueous solution electrolysis liquid at last.The voltage of this water lithium electricity system is 1.2V, and specific discharge capacity is 110mAhg -1

Claims (2)

1. the preparation method of an inorganic aqueous solution lithium ion battery is characterized in that:
1) preparation positive electrode:
Be in molar ratio (1.02～1.06): 1 takes by weighing Li 2CO 3And Co 2O 3Raw material is with the Li that takes by weighing 2CO 3And Co 2O 3Raw material is put into ball grinder, the agate mill ball of packing into, and ball milling 20-24 hour, obtain mixed-powder, its mould of packing into is placed press model machine, under the pressure of 15-20MPa, pressurize 10-15 minute, the demoulding obtained cylindrical piece; The cylindrical piece that obtains is placed porcelain boat, put into resistance wire horizontal pipe heating furnace, adopt following calcination process: with 3-5 ℃ of min -1Heating rate be heated to 300-350 ℃, be incubated 12-15 hour; Cool to room temperature with the furnace; Again with 3-5 ℃ of min -1Heating rate be heated to 750-800 ℃, be incubated 12-15 hour; Cool to room temperature with the furnace, obtain LiCoO 2Sample;
2) preparation negative material:
Choose Li 2CO 3And V 2O 5Be raw material, according to (1.02～1.06): 3 mol ratios claim sample, and above-mentioned raw materials is put into ball grinder, the agate mill ball of packing into, ball milling 20-24 hour, obtain mixed-powder, its mould of packing into is placed press model machine, under the pressure of 15-20MPa, pressurize 10-15 minute, the demoulding obtained cylindrical piece; The cylindrical piece that obtains is placed porcelain boat, put into resistance wire horizontal pipe heating furnace, adopt following calcination process: with 3-5 ℃ of min -1Heating rate be heated to 650-680 ℃, be incubated 10-12 hour; Cool to room temperature with the furnace; Again with 3-5 ℃ of min -1Heating rate be heated to 300-350 ℃, be incubated 8-10 hour; Cool to room temperature with the furnace, obtain LiV 3O 8Sample;
3) preparation technology of electrode slice:
A. with synthetic LiCoO 2Sample or LiV 3O 8Sample mixes with acetylene black respectively, obtains black powder, polyvinylidene fluoride is dissolved in the N-methyl pyrrolidone that dewaters then, obtains solution A, black powder is mixed obtaining black paste with solution A;
Wherein, LiCoO 2Sample or LiV 3O 8Sample is 80: 10: 10 or 85: 10: 5 with the mass ratio of acetylene black, polyvinylidene fluoride respectively;
B. black paste is coated on the nickel screen with doctor blade, under vacuum condition 85-100 ℃ dry 8-10 hour, obtain LiCoO respectively 2Positive electrical pole piece or LiV 3O 8The negative electricity pole piece;
4) with LiCoO 2Electrode slice is that water lithium electricity is anodal, LiV 3O 8Electrode slice is a negative pole, is contained in the saturated LiNO of 20ml 3In the beaker of electrolyte, the pH=5-6 of its electrolyte, positive/negative plate immerses, and keeps the spacing of 0.5-1cm, can obtain inorganic aqueous solution lithium ion battery.
According to the preparation method of the described a kind of inorganic aqueous solution lithium ion battery of claim 1, it is characterized in that 2, described resistance wire horizontal pipe heating furnace is a Fe-Cr-Al silk calandria stove.
CN2009100239789A 2009-09-22 2009-09-22 Preparation method of inorganic aqueous solution lithium ion battery Expired - Fee Related CN101656329B (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102185163A (en) * 2011-04-01 2011-09-14 西安交通大学 Method for preparing inorganic aqueous solution lithium ion battery system by using monocrystal LiMnO (lithium manganese oxide) nanowire
CN102610825A (en) * 2012-03-26 2012-07-25 四川省达州钢铁集团有限责任公司 Manufacturing method of cathode electrode plate for lithium battery
CN102610863A (en) * 2012-03-19 2012-07-25 西安交通大学 Method for assembling aqueous lithium-ion battery by aid of lithium iron manganese phosphate

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101262056A (en) * 2007-03-08 2008-09-10 复旦大学 A water solution chargeable lithium ion battery

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102185163A (en) * 2011-04-01 2011-09-14 西安交通大学 Method for preparing inorganic aqueous solution lithium ion battery system by using monocrystal LiMnO (lithium manganese oxide) nanowire
CN102610863A (en) * 2012-03-19 2012-07-25 西安交通大学 Method for assembling aqueous lithium-ion battery by aid of lithium iron manganese phosphate
CN102610825A (en) * 2012-03-26 2012-07-25 四川省达州钢铁集团有限责任公司 Manufacturing method of cathode electrode plate for lithium battery
CN102610825B (en) * 2012-03-26 2015-06-17 四川省达州钢铁集团有限责任公司 Manufacturing method of cathode electrode plate for lithium battery

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