CN109817938B - A kind of preparation method of iron-based negative electrode material - Google Patents
A kind of preparation method of iron-based negative electrode material Download PDFInfo
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 65
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 32
- 239000007773 negative electrode material Substances 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 238000007747 plating Methods 0.000 claims abstract description 40
- 239000000126 substance Substances 0.000 claims abstract description 20
- 239000000463 material Substances 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 13
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910001416 lithium ion Inorganic materials 0.000 claims abstract description 12
- 230000008569 process Effects 0.000 claims abstract description 9
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000000243 solution Substances 0.000 claims description 37
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 239000008367 deionised water Substances 0.000 claims description 14
- 229910021641 deionized water Inorganic materials 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 14
- JEIPFZHSYJVQDO-UHFFFAOYSA-N ferric oxide Chemical compound O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 14
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 8
- 230000004913 activation Effects 0.000 claims description 8
- 230000001235 sensitizing effect Effects 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical group OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims description 6
- 206010070834 Sensitisation Diseases 0.000 claims description 6
- 239000008139 complexing agent Substances 0.000 claims description 6
- 239000012153 distilled water Substances 0.000 claims description 6
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 6
- 230000008313 sensitization Effects 0.000 claims description 6
- 239000003381 stabilizer Substances 0.000 claims description 6
- 239000004094 surface-active agent Substances 0.000 claims description 6
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 150000003839 salts Chemical class 0.000 claims description 5
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 4
- 239000003638 chemical reducing agent Substances 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 230000007935 neutral effect Effects 0.000 claims description 4
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 4
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 4
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 4
- 238000003828 vacuum filtration Methods 0.000 claims description 4
- 239000012266 salt solution Substances 0.000 claims description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 2
- 239000003109 Disodium ethylene diamine tetraacetate Substances 0.000 claims description 2
- ZGTMUACCHSMWAC-UHFFFAOYSA-L EDTA disodium salt (anhydrous) Chemical compound [Na+].[Na+].OC(=O)CN(CC([O-])=O)CCN(CC(O)=O)CC([O-])=O ZGTMUACCHSMWAC-UHFFFAOYSA-L 0.000 claims description 2
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 2
- UYJXRRSPUVSSMN-UHFFFAOYSA-P ammonium sulfide Chemical compound [NH4+].[NH4+].[S-2] UYJXRRSPUVSSMN-UHFFFAOYSA-P 0.000 claims description 2
- 239000004202 carbamide Substances 0.000 claims description 2
- 235000019301 disodium ethylene diamine tetraacetate Nutrition 0.000 claims description 2
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 2
- 150000002505 iron Chemical class 0.000 claims description 2
- 150000002815 nickel Chemical class 0.000 claims description 2
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 2
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims description 2
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 2
- 239000001509 sodium citrate Substances 0.000 claims description 2
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 2
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 2
- 238000007772 electroless plating Methods 0.000 claims 3
- 238000007788 roughening Methods 0.000 claims 2
- 235000011114 ammonium hydroxide Nutrition 0.000 claims 1
- 238000005660 chlorination reaction Methods 0.000 claims 1
- 238000005238 degreasing Methods 0.000 claims 1
- 150000004687 hexahydrates Chemical class 0.000 claims 1
- 239000000203 mixture Substances 0.000 claims 1
- DAJSVUQLFFJUSX-UHFFFAOYSA-M sodium;dodecane-1-sulfonate Chemical compound [Na+].CCCCCCCCCCCCS([O-])(=O)=O DAJSVUQLFFJUSX-UHFFFAOYSA-M 0.000 claims 1
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 abstract description 12
- 239000002245 particle Substances 0.000 abstract description 3
- 239000011248 coating agent Substances 0.000 abstract description 2
- 238000000576 coating method Methods 0.000 abstract description 2
- 230000007797 corrosion Effects 0.000 abstract description 2
- 238000005260 corrosion Methods 0.000 abstract description 2
- 238000005516 engineering process Methods 0.000 abstract description 2
- 229910052759 nickel Inorganic materials 0.000 abstract description 2
- 238000007709 nanocrystallization Methods 0.000 abstract 1
- 230000003213 activating effect Effects 0.000 description 8
- 238000001354 calcination Methods 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- 229940044631 ferric chloride hexahydrate Drugs 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 238000001027 hydrothermal synthesis Methods 0.000 description 3
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000003139 buffering effect Effects 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009831 deintercalation Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000009830 intercalation Methods 0.000 description 1
- 230000002687 intercalation Effects 0.000 description 1
- 230000003446 memory effect Effects 0.000 description 1
- 230000020477 pH reduction Effects 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- 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
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- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention belongs to the technical field of lithium ion batteries, and particularly relates to a preparation method of an iron-based negative electrode material. The surface of the nano iron oxide is chemically plated with nickel, and the iron oxide particles are subjected to nanocrystallization, so that the contact area of the iron oxide can be increased, and the electrochemical performance is enhanced. Chemical plating is a surface technology which is simple and convenient to operate, can be deposited on the surface of an iron oxide material, is uniform in plating layer, and has good coating property, corrosion resistance and wear resistance. The surface of the iron-based negative electrode material is plated with a layer of substance with better conductivity by chemical plating, so that the conductivity of the material can be improved, the problem of volume expansion in the circulating process is solved, and the plating missing phenomenon is avoided by repeating the chemical plating process for 2-3 times, so that the electrochemical performance of the negative electrode material is further improved, and the high-performance iron-based negative electrode material is prepared.
Description
Technical Field
The invention belongs to the technical field of lithium ion batteries, and particularly relates to a preparation method of an iron-based negative electrode material.
Background
The lithium ion battery has the advantages of large energy density, high working voltage, small self-discharge, no memory effect, wide temperature range and the like, and becomes the secondary battery with the most excellent comprehensive performance at present. Compared with the traditional graphite negative electrode material (with the theoretical specific capacity of 372mAh/g), Fe2O3(the theoretical specific capacity is 1005mAh/g) has attracted high attention as the negative electrode material of the lithium ion battery. However, Fe is involved in the process of lithium ion intercalation and deintercalation2O3Pulverization and serious particle agglomeration occur, thereby causing the reduction of electron transmission and diffusion performance, too fast capacity attenuation, short cycle period,seriously affecting its further application as anode material in lithium ion batteries.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide a preparation method of an iron-based negative electrode material, which improves the conductivity of the material through surface chemical plating of the iron-based negative electrode material and inhibits the problem of volume expansion in the circulating process so as to prepare the high-performance iron-based negative electrode material.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of an iron-based negative electrode material comprises the following steps:
(1) taking an iron-based material, wherein the iron-based material is nano iron oxide powder; coarsening and sensitizing activation are carried out;
(2) preparing a plating solution: mixing the main salt solution and the complexing agent solution, sequentially adding the stabilizer and the surfactant, and uniformly mixing to obtain a plating solution; the main salt is nickel salt; the concentration of the main salt solution in the plating solution is 10-40g/L, the concentration of the complexing agent is 0.03-006mol/L, and the concentration of the stabilizing agent is (1-3) multiplied by 10-6mol/L, the concentration of the surfactant is (0.5-1.5) x 10- 6mol/L；
(3) Adding the activated iron-based material into a plating solution, adjusting the pH value of the plating solution to 12-13, slowly adding a reducing agent, and performing chemical plating, wherein the chemical plating temperature is 65-70 ℃, and the plating time is 70-120 min;
(4) and cleaning the iron-based material subjected to chemical plating with deionized water, and drying to obtain the iron-based lithium ion battery cathode material.
In the step (1), the preparation process of the nano iron oxide powder comprises the following steps: dissolving a certain amount of ferric chloride hexahydrate in deionized water, dropwise adding a sodium hydroxide solution, and adjusting the pH value of the system to be more than 10. Transferring the obtained product into a high-pressure reaction kettle, and carrying out hydrothermal reaction at 200 ℃ for 10 hours. And cooling, carrying out vacuum filtration, filtering to obtain a red product, washing the product with deionized water, and drying in a constant-temperature drying oven at 60 ℃ for 12 h. And taking out a sample obtained by drying, putting the sample into a clean crucible, and calcining the sample in a muffle furnace at 300 ℃ for 2 hours.
In the step (1), the coarsening process of the iron-based material comprises the following steps: performing coarsening and acidification treatment for 5min by using nitric acid solution with volume fraction of 10% while ultrasonically stirring, and washing to be neutral by using distilled water.
In the step (1), a sensitization activation fractional step method is adopted for sensitization activation of the iron-based material, and a sensitization liquid is prepared from 10g of a sensitizer, 40ml of concentrated hydrochloric acid and 1000ml of distilled water. Weighing a certain amount of deoiled powder into a quantitative sensitizing solution, sensitizing for 3-5 min under the ultrasonic stirring of 150W, taking out, and washing with distilled water until no chloride ion exists. The activating solution was prepared from 3.5g of silver nitrate +7g/L of aqueous solution of NaOH +100ml/L of aqueous ammonia. And (3) measuring a certain amount of activating liquid, adding the activating liquid into the sensitized powder, and activating for 10-15 min under the ultrasonic stirring of 150W.
In the step (2), the nickel salt is specifically one of nickel nitrate, nickel sulfate or nickel chloride.
In the step (2), the complexing agent is one of ethylenediamine, sodium citrate or disodium ethylenediamine tetraacetate, the stabilizer is one of thiourea, urea or ammonium sulfide, and the surfactant is one of sodium dodecyl sulfate, sodium dodecyl sulfate or sodium dodecyl benzene sulfonate.
In the step (3), the reducing agent is hydrazine hydrate, and the addition amount is 10-150ml/L of the plating solution.
In the step (4), the chemical plating times are 2-3 times so as to avoid the condition of plating leakage.
When the prepared iron-based negative electrode material is used as a lithium ion battery negative electrode, the current density is 100mA/g, the specific capacity is stabilized at 650-800mAh/g after 100 cycles, and the coulombic efficiency reaches 96-98%.
In the invention, the contact area of the iron oxide can be increased by nano-converting the iron oxide particles, and the electrochemical performance is enhanced. Chemical plating is a surface technology which is simple and convenient to operate, can be deposited on the surface of an iron oxide material, is uniform in plating layer, and has good coating property, corrosion resistance and wear resistance. Therefore, the surface of the iron-based negative electrode material is plated with a layer of substance with better conductivity by chemical plating, so that the conductivity of the material can be improved, the problem of volume expansion in the circulating process is solved, and the plating missing phenomenon is avoided by repeating the chemical plating process for 2-3 times, thereby further improving the electrochemical performance of the negative electrode material.
The invention has the beneficial effects that:
the invention adopts the surface chemical nickel plating of the nano iron oxide, even secondary chemical plating, thereby improving the conductivity of the material, buffering the problem of volume expansion of the iron-based negative electrode material in the circulating process and improving the electrochemical performance.
Detailed Description
The present invention will be described in further detail with reference to examples.
Example 1
(1) Dissolving a certain amount of ferric chloride hexahydrate in deionized water, dropwise adding a sodium hydroxide solution, and adjusting the pH value of the system to be more than 10. Transferring the obtained product into a high-pressure reaction kettle, and carrying out hydrothermal reaction at 200 ℃ for 10 hours. And cooling, carrying out vacuum filtration, filtering to obtain a red product, washing the product with deionized water, and drying in a constant-temperature drying oven at 60 ℃ for 12 h. And taking out a sample obtained by drying, putting the sample into a clean crucible, and calcining the sample in a muffle furnace at 300 ℃ for 2 hours. Obtaining nano iron oxide powder; (2) putting nano iron oxide powder into the coarsening solution of nitric acid, stirring at room temperature, cleaning to be neutral by deionized water, and then sensitizing and activating by adopting a sensitizing and activating step method; (3) mixing nickel sulfate solution and 0.05mol/L ethylenediamine solution, and sequentially adding 2 × 10-6mol/L Thiourea and 1X 10-6mol/L sodium dodecyl sulfate, wherein the concentration of the main salt is 20 g/L; (4) adding the product obtained in the step (2) into the plating solution prepared in the step (3), adjusting the pH value to 12, slowly adding a hydrazine hydrate solution, and performing chemical plating for 60min at 70 ℃, wherein the use amount of hydrazine hydrate is 50 ml/L; (5) washing with deionized water and drying; (6) and repeating the secondary chemical plating to obtain the iron-based negative electrode material. The negative electrode material is used as a lithium ion battery negative electrode, and after 100 cycles under the current density of 100mA/g, the specific capacity is stabilized at 655mAh/g, and the coulombic efficiency is 96.5%.
Example 2
(1) Dissolving a certain amount of ferric chloride hexahydrate in deionized water, dropwise adding a sodium hydroxide solution, and adjusting the pH value of the system to be more than 10. Transferring the obtained product into a high-pressure reaction kettle,carrying out hydrothermal reaction at 200 ℃ for 10 h. And cooling, carrying out vacuum filtration, filtering to obtain a red product, washing the product with deionized water, and drying in a constant-temperature drying oven at 60 ℃ for 12 h. And taking out a sample obtained by drying, putting the sample into a clean crucible, and calcining the sample in a muffle furnace at 300 ℃ for 2 hours. Obtaining nano iron oxide powder; (2) putting nano iron oxide powder into the coarsening solution of nitric acid, stirring at room temperature, cleaning to be neutral by deionized water, and then sensitizing and activating by adopting a sensitizing and activating step method; (3) mixing nickel sulfate solution and 0.05mol/L ethylenediamine solution, and sequentially adding 2 × 10-6mol/L Thiourea and 1X 10-6mol/L sodium dodecyl sulfate, wherein the concentration of the main salt is 30 g/L; (4) adding the product obtained in the step (2) into the plating solution prepared in the step (3), adjusting the pH value to 13, slowly adding a hydrazine hydrate solution, and performing chemical plating for 60min at 65 ℃, wherein the use amount of hydrazine hydrate is 50 ml/L; (5) washing with deionized water and drying; (6) and repeating the secondary chemical plating to obtain the iron-based negative electrode material. The negative electrode material is used as a lithium ion battery negative electrode, and after 100 cycles under the current density of 100mA/g, the specific capacity is stabilized at 780mAh/g, and the coulombic efficiency is 97.55%.
Claims (4)
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| CN101302613A (en) * | 2008-01-16 | 2008-11-12 | 哈尔滨工业大学 | Nickel plating solution and nickel plating method for inorganic oxide powder |
| CN106601993A (en) * | 2016-12-29 | 2017-04-26 | 深圳市沃特玛电池有限公司 | Lithium ion battery negative electrode plate and preparation method therefor |
| CN108270011A (en) * | 2018-01-26 | 2018-07-10 | 山东大学 | A kind of lithium ion battery negative material and preparation method thereof |
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| DE2422577C3 (en) * | 1974-05-09 | 1979-10-11 | Deutsche Automobilgesellschaft Mbh, 3000 Hannover | Rechargeable galvanic cell and method of operating this cell |
| JP3151801B2 (en) * | 1995-06-19 | 2001-04-03 | 住友電気工業株式会社 | Battery electrode substrate and method of manufacturing the same |
| US5851599A (en) * | 1995-09-28 | 1998-12-22 | Sumitomo Electric Industries Co., Ltd. | Battery electrode substrate and process for producing the same |
| CN1319191C (en) * | 2005-09-06 | 2007-05-30 | 天津力神电池股份有限公司 | Method for preparing negative pole material of lithium ion cell high-capacity tin composite |
| CN106299278A (en) * | 2016-08-31 | 2017-01-04 | 青岛文创科技有限公司 | A kind of ferrum magnesium ashbury metal lithium ion battery negative material |
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| CN101302613A (en) * | 2008-01-16 | 2008-11-12 | 哈尔滨工业大学 | Nickel plating solution and nickel plating method for inorganic oxide powder |
| CN106601993A (en) * | 2016-12-29 | 2017-04-26 | 深圳市沃特玛电池有限公司 | Lithium ion battery negative electrode plate and preparation method therefor |
| CN108270011A (en) * | 2018-01-26 | 2018-07-10 | 山东大学 | A kind of lithium ion battery negative material and preparation method thereof |
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