CN104577107A - Surface finish method of carbon fluoride material - Google Patents
Surface finish method of carbon fluoride material Download PDFInfo
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- CN104577107A CN104577107A CN201310478262.4A CN201310478262A CN104577107A CN 104577107 A CN104577107 A CN 104577107A CN 201310478262 A CN201310478262 A CN 201310478262A CN 104577107 A CN104577107 A CN 104577107A
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- carbon fluoride
- carbon material
- fluorinated carbon
- nanometer copper
- fluorocarbons
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/06—Electrodes for primary cells
- H01M4/08—Processes of manufacture
Abstract
The invention relates to a surface finish method of a carbon fluoride material. The method comprises the following steps: (1) mixing nanometer copper and carbon fluoride, then adding a solvent for ball milling so as to form a combined pulp; (2) drying the mixed pulp so as to form a mixture; (3) screening the mixture so as to obtain the powder mixture; (4) putting the powder mixture into an atmosphere oven so as to be calcined; (5) taking out the calcined powder mixture, lowering the temperature of the calcined powder mixture to the room temperature, and then screening the calcined powder mixture of which the temperature is lowered so as to form the carbon fluoride material modifies by the nanometer copper. According to the invention, the carbon fluoride and the nanometer copper with good conductivity are mixed, and after the mixture is calcined at a high temperature in an inert atmosphere, the nanometer copper reacts on the surface of the carbon fluoride, so that the phenomenon that the voltage of carbon fluoride is delayed is obviously improved, and high-ratio discharge and low temperature performance are greatly improved. The carbon fluoride with a finished surface, prepared by the method, is used as a positive material to be made into a lithium-carbon fluoride battery system, wherein the lithium-carbon fluoride battery system has the properties of high-ratio discharge and low temperature high-current discharge, so that the application range of the lithium-carbon fluoride battery system is extended.
Description
Technical field
The invention belongs to anode material of lithium battery technical field, particularly relate to a kind of surface modification method of fluorinated carbon material.
Background technology
Lithium metal one-shot battery is of a great variety, there is higher specific energy and operating voltage, the comparatively ripe system of current development mainly contains lithium-manganese dioxide battery, lithium-thionyl chloride battery, lithium-sulfur dioxide battery etc., and energy density generally can reach 250-350Wh/kg.In recent years, lithium-fluorocarbons battery receives much concern because having higher energy density.But, due to delayed serious, the large multiplying power discharging property of fluorinated carbon material initial voltage be not very well, the problem such as heat release and expansion, eventually reduce the effect of battery low-temperature high-current discharge, have a strong impact on the large multiplying power discharging property of battery, greatly limit the technical development of lithium-fluorocarbons battery.
Disclose a kind of lithium battery fluorocarbons positive electrode fluorocarbons patent of invention at present, wherein fluorocarbons is fluorographite CF
xwith carbon fluoride nano-tube CF
xmixture; Described fluorographite CF
xwith carbon fluoride nano-tube CF
xmass ratio range be 6:4 to 9.5:0.5.The present invention adopts the mixture of fluorographite and carbon fluoride nano-tube as battery fluorocarbons positive electrode, carbon fluoride nano-tube material is made to be dispersed in around fluorographite particle preferably, effectively eliminate the high agglomeration of carbon fluoride nano-tube material, improving the battery discharge initial stage there is obvious voltage delay phenomenon to some extent, the multiplying power discharging property of lithium-fluorocarbons battery system is increased, but the material due to the present invention's employing is fluoridizes series material, fundamentally do not solve the initial voltage hysteresis that fluorocarbons itself has, be difficult to the discharge-rate significantly improving lithium-fluorocarbons battery, have impact on the extensive use of fluorinated carbon material.
Summary of the invention
The present invention provides the voltage delay effectively reducing fluorocarbons for solving in known technology the technical problem that exists, improves the surface modification method of the large multiplying power discharging property of fluorocarbons and a kind of fluorinated carbon material of cryogenic property.
The present invention includes following technical scheme:
A surface modification method for fluorinated carbon material, is characterized in: comprise following preparation process:
Step 1. is by Nanometer Copper: the material of fluorocarbons=0.001-0.4:1 mass ratio is inserted in ball mill and mixed, then in ball mill with quality than fluorocarbons: the ratio of solvent=1:1-2 adds solvent; Turn/rotating speed batch mixing ball milling the 12-24h of min with 100-600, form mixed slurry;
Step 2. takes out mixed slurry, and the 10-20h that dries in the air in room temperature environment carries out drying, forms mixture;
Step 3. obtains mix powder after the mixture in step 2 is crossed 100-400 mesh sieve;
Mix powder is inserted in atmosphere furnace by step 4., and under inert atmosphere, atmosphere furnace is warming up to the constant temperature of 300-500 DEG C with the speed of 3-15 DEG C/min, carries out 1-24h calcining in constant temperature to mix powder;
Step 5. takes out the mix powder after calcining, after being down to room temperature, crosses 100-300 mesh sieve, namely form the fluorinated carbon material modified through Nanometer Copper with 2-15 DEG C/min speed.
The present invention can also adopt following technical measures:
Described solvent is a kind of in ethanol, ethylene glycol, isopropyl alcohol or water.
Described inert atmosphere is nitrogen or argon gas.
Add in mechanical milling process in described step 1 and have ball agate to grind pearl.
Ball mill in described step 1 is agate jar.
Described Nanometer Copper diameter is 10-100nm.
The advantage that the present invention has and good effect:
1, the present invention by fluorocarbons with there is good conductive nanometer copper mix, in inert atmosphere after high-temperature calcination, Nanometer Copper reacts on fluorocarbons surface, significantly improves fluorocarbons voltage delay phenomenon, and large multiplying power discharging and cryogenic property all improve a lot; The lithium that after the finishing prepared by the present invention, fluorocarbons is made into as positive electrode-fluorocarbons battery system has the performance of large multiplying power discharging, low-temperature high-current discharge, expands the range of application of lithium-fluorocarbons battery system.
2, the present invention is placed with ball agate mill pearl in the material of mechanical milling process, makes fluorocarbons more even with mixing of Nanometer Copper.
Accompanying drawing explanation
Fig. 1 is battery discharge curve comparison diagram prepared by the battery prepared of fluorinated carbon material after modifying in the embodiment of the present invention 1 and pure fluorinated carbon material;
Fig. 2 is battery discharge curve comparison diagram prepared by the battery prepared of fluorinated carbon material after modifying in the embodiment of the present invention 2 and pure fluorinated carbon material.
Detailed description of the invention
For summary of the invention of the present invention, Characteristic can be disclosed further, be also described in detail as follows by reference to the accompanying drawings especially exemplified by following instance.
A surface modification method for fluorinated carbon material, is characterized in: comprise following preparation process:
Step 1. is by Nanometer Copper: the material of fluorocarbons=0.001-0.4:1 mass ratio is inserted in ball mill and mixed, then in ball mill with quality than fluorocarbons: the ratio of solvent=1:1-2 adds solvent; Turn/rotating speed batch mixing ball milling the 12-24h of min with 100-600, form mixed slurry;
Step 2. takes out mixed slurry, and the 10-20h that dries in the air in room temperature environment carries out drying, forms mixture;
Step 3. obtains mix powder after the mixture in step 2 is crossed 100-400 mesh sieve;
Mix powder is inserted in atmosphere furnace by step 4., and under inert atmosphere, atmosphere furnace is warming up to the constant temperature of 300-500 DEG C with the speed of 3-15 DEG C/min, carries out 1-24h calcining in constant temperature to mix powder;
Step 5. takes out the mix powder after calcining, after being down to room temperature, crosses 100-300 mesh sieve, namely form the fluorinated carbon material modified through Nanometer Copper with 2-15 DEG C/min speed.
Described solvent is a kind of in ethanol, ethylene glycol, isopropyl alcohol or water.
Described inert atmosphere is nitrogen or argon gas.
Add in mechanical milling process in described step 1 and have ball agate to grind pearl.
Ball mill in described step 1 is agate jar.
Described Nanometer Copper diameter is 10-100nm.
Embodiment 1:
Step 1. gets the Nanometer Copper that 0.2g diameter is 10-100nm, 4g fluorocarbons adds in agate jar and mixes, then 6g ethanol is added, grinding pearl mass ratio according to fluorocarbons and ball agate is that the ratio of 1:10 is put into ball agate and ground pearl in agate jar, the diameter of ball agate mill pearl is 5-15mm, material ball milling mixing 12h under 300 turns/min condition in agate jar, forms mixed slurry; By ball milling, better by Nanometer Copper and fluorocarbons mixing, mixed effect can be improve.
Step 2. takes out the mixed slurry that step 1 is formed, and the 10h that dries in the air in room temperature environment carries out drying, forms mixture;
Step 3. obtains mix powder after the mixture in step 2 is crossed 300 mesh sieves;
Mix powder is inserted in atmosphere furnace by step 4., and under nitrogen atmosphere, atmosphere furnace is warming up to the constant temperature of 450 DEG C with the speed of 5 DEG C/min, to mix powder calcining 5h in constant temperature;
Step 5. takes out the mix powder after calcining, after being cooled to 25 DEG C of room temperatures, crosses 300 mesh sieves according to the speed of 2 DEG C/min, namely forms the fluorinated carbon material that the present invention modifies through Nanometer Copper.
Embodiment 2:
Step 1. gets the Nanometer Copper that 0.4g diameter is 20-40nm, 10g fluorocarbons adds in agate jar and mixes, then 14g ethanol is added, grinding pearl mass ratio according to fluorocarbons and ball agate is that the ratio of 1:15 is put into ball agate and ground pearl in agate jar, the diameter of ball agate mill pearl is 5-15mm, material ball milling mixing 12h under 200 turns/min condition in agate jar, forms mixed slurry; By ball milling, better by Nanometer Copper and fluorocarbons mixing, mixed effect can be added.
Step 2. takes out the mixed slurry that step 1 is formed, and the 10h that dries in the air in room temperature environment carries out drying, forms mixture;
Step 3. obtains mix powder after the mixture in step 2 is crossed 300 mesh sieves;
Mix powder is inserted in atmosphere furnace by step 4., and under argon gas atmosphere, atmosphere furnace is warming up to the constant temperature of 450 DEG C with the speed of 5 DEG C/min, to mix powder calcining 5h in constant temperature;
Step 5. takes out the mix powder after calcining, after being cooled to 25 DEG C of room temperatures, crosses 300 mesh sieves according to the speed of 10 DEG C/min, namely forms the fluorinated carbon material that the present invention modifies through Nanometer Copper.
Adopt embodiment 1 make through Nanometer Copper modify fluorinated carbon material as positive electrode, SP as conductive agent, pvdf as binding agent, according to quality than positive electrode: conductive agent: the ratio of binding agent=84:10:6 is uniformly mixed into anode sizing agent and is coated on aluminium foil in ball mill, carries out drying under 120 DEG C of conditions; Lithium metal, as negative electrode, carries out the assembling of one group of lithium battery in glove box.Adopt pure fluorocarbons as positive electrode again, all the other are identical with embodiment 1, carry out another group lithium battery assembling.Two groups of lithium batteries to carry out shown in Fig. 1 the discharge test under 25 DEG C of normal temperature, 0.1C condition simultaneously, and the lower curve in Fig. 1 is the discharge curve of the lithium battery that pure fluorocarbons is assembled into, upper curve is the discharge curve that the material adopting embodiment 1 to make is assembled into lithium battery; Obviously observe in Fig. 1, the lithium battery initial voltage that pure fluorocarbons is made is 2.30V, and adopt the lithium battery that the blended anode material in embodiment 1 is made, its initial minimum voltage is 2.49V, lagging voltage be improved significantly, and the battery made of fluorinated carbon material after adopting Nanometer Copper to modify, discharge voltage plateau there has also been and significantly improves, its voltage delay problem and voltage platform all be improved significantly, greatly improve the discharge performance of battery.
Adopt embodiment 2 make through Nanometer Copper modify fluorinated carbon material as positive electrode, SP as conductive agent, pvdf as binding agent, according to quality than positive electrode: conductive agent: the ratio of binding agent=84:10:6 is uniformly mixed into anode sizing agent and is coated on aluminium foil in ball mill, carries out drying under 120 DEG C of conditions; Lithium metal, as negative electrode, carries out the assembling of one group of lithium battery in glove box.Adopt pure fluorocarbons as positive electrode again, all the other are identical with embodiment 2, carry out another group lithium battery assembling.Two groups of lithium batteries to carry out shown in Fig. 2 the discharge test under 25 DEG C of normal temperature, 1C condition simultaneously, and the lower curve in Fig. 2 is the discharge curve of the lithium battery that pure fluorocarbons is assembled into, upper curve is the discharge curve that the material adopting embodiment 2 to make is assembled into lithium battery; Obviously observe in Fig. 2, the lithium battery initial voltage that pure fluorocarbons is made is about 1.8V, and under heavy-current discharge condition, voltage delay is obvious; Adopt the lithium battery that the blended anode material in embodiment 2 is made, its initial minimum voltage higher than 2.0V, lagging voltage be improved significantly, embodied through Nanometer Copper modify fluorocarbons, its electric conductivity and discharge platform are significantly improved, discharge performance be improved significantly.
Although be described the preferred embodiments of the present invention by reference to the accompanying drawings above; but the present invention is not limited to above-mentioned detailed description of the invention; above-mentioned detailed description of the invention is only schematic; be not restrictive; those of ordinary skill in the art is under enlightenment of the present invention; not departing under the ambit that present inventive concept and claim protect, a lot of form can also be made.These all belong within protection scope of the present invention.
Claims (6)
1. a surface modification method for fluorinated carbon material, is characterized in that: comprise following preparation process:
Step 1. is by Nanometer Copper: the material of fluorocarbons=0.001-0.4:1 mass ratio is inserted in ball mill and mixed, then in ball mill with quality than fluorocarbons: the ratio of solvent=1:1-2 adds solvent; Turn/rotating speed batch mixing ball milling the 12-24h of min with 100-600, form mixed slurry;
Step 2. takes out mixed slurry, and the 10-20h that dries in the air in room temperature environment carries out drying, forms mixture;
Step 3. obtains mix powder after the mixture in step 2 is crossed 100-400 mesh sieve;
Mix powder is inserted in atmosphere furnace by step 4., and under inert atmosphere, atmosphere furnace is warming up to the constant temperature of 300-500 DEG C with the speed of 3-15 DEG C/min, carries out 1-24h calcining in constant temperature to mix powder;
Step 5. takes out the mix powder after calcining, after being down to room temperature, crosses 100-300 mesh sieve, namely form the fluorinated carbon material modified through Nanometer Copper with 2-15 DEG C/min speed.
2. the surface modification method of a kind of fluorinated carbon material according to claim 1, is characterized in that: described solvent is the one in ethanol, ethylene glycol, isopropyl alcohol or water.
3. the surface modification method of a kind of fluorinated carbon material according to claim 1, is characterized in that: described inert atmosphere is nitrogen or argon gas.
4. the surface modification method of a kind of fluorinated carbon material according to claim 1, is characterized in that: add in the mechanical milling process in described step 1 and have ball agate to grind pearl.
5. the surface modification method of a kind of fluorinated carbon material according to claim 1, is characterized in that: the ball mill in described step 1 is agate jar.
6. the surface modification method of a kind of fluorinated carbon material according to claim 1, is characterized in that: described Nanometer Copper diameter is 10-100nm.
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Cited By (12)
Publication number | Priority date | Publication date | Assignee | Title |
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CN105655588A (en) * | 2016-04-08 | 2016-06-08 | 北京工业大学 | Silicon dioxide modified carbon fluoride material and preparation method thereof |
CN106229511A (en) * | 2016-10-13 | 2016-12-14 | 江苏超电新能源科技发展有限公司 | Surface modifying method of a kind of fluorinated carbon material and products thereof and application |
CN106384812A (en) * | 2016-10-13 | 2017-02-08 | 江苏超电新能源科技发展有限公司 | Surface-modified carbon fluoride material, and method and application thereof |
CN107910521A (en) * | 2017-11-10 | 2018-04-13 | 北京工业大学 | A kind of fluorinated carbon material, preparation and the application of ruthenium modification |
CN107968205A (en) * | 2017-12-06 | 2018-04-27 | 贵州梅岭电源有限公司 | A kind of method of the modified fluorinated carbon positive electrode of chemical reduction method |
CN109659515A (en) * | 2018-11-23 | 2019-04-19 | 贵州梅岭电源有限公司 | A kind of preparation method of the fluorination carbon electrode material of Ag C modification |
CN109698365A (en) * | 2018-12-05 | 2019-04-30 | 上海空间电源研究所 | A kind of lithium metal battery with elastic buffer structure |
CN109873137A (en) * | 2019-02-01 | 2019-06-11 | 贵州梅岭电源有限公司 | A kind of V2O5The preparation method of the fluorocarbons positive electrode of@C modification |
CN110783522A (en) * | 2018-11-23 | 2020-02-11 | 贵州梅岭电源有限公司 | Preparation method of nanomaterial-modified carbon fluoride electrode material |
WO2020034497A1 (en) * | 2018-08-17 | 2020-02-20 | 深圳南科新材科技有限公司 | Anti-wear additive, preparation method therefor, use thereof, and lubricating oil containing same |
CN112186139A (en) * | 2019-07-04 | 2021-01-05 | 上海大学 | Single-metal atom point modified carbon fluoride anode material and preparation method thereof |
CN114400305A (en) * | 2021-12-14 | 2022-04-26 | 中国电子科技集团公司第十八研究所 | Thermal battery high-voltage spherical carbon fluoride anode material and preparation method thereof |
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CN102473913A (en) * | 2009-07-21 | 2012-05-23 | 松下电器产业株式会社 | Lithium primary battery |
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Cited By (15)
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CN105655588B (en) * | 2016-04-08 | 2017-12-15 | 北京工业大学 | A kind of silica modified fluorinated carbon material and preparation method |
CN105655588A (en) * | 2016-04-08 | 2016-06-08 | 北京工业大学 | Silicon dioxide modified carbon fluoride material and preparation method thereof |
CN106384812B (en) * | 2016-10-13 | 2019-01-04 | 江苏超电新能源科技发展有限公司 | A kind of modified fluorinated carbon material in surface and its method and application |
CN106384812A (en) * | 2016-10-13 | 2017-02-08 | 江苏超电新能源科技发展有限公司 | Surface-modified carbon fluoride material, and method and application thereof |
CN106229511A (en) * | 2016-10-13 | 2016-12-14 | 江苏超电新能源科技发展有限公司 | Surface modifying method of a kind of fluorinated carbon material and products thereof and application |
CN107910521A (en) * | 2017-11-10 | 2018-04-13 | 北京工业大学 | A kind of fluorinated carbon material, preparation and the application of ruthenium modification |
CN107910521B (en) * | 2017-11-10 | 2021-03-16 | 北京工业大学 | Ruthenium-modified carbon fluoride material, preparation and application |
CN107968205A (en) * | 2017-12-06 | 2018-04-27 | 贵州梅岭电源有限公司 | A kind of method of the modified fluorinated carbon positive electrode of chemical reduction method |
WO2020034497A1 (en) * | 2018-08-17 | 2020-02-20 | 深圳南科新材科技有限公司 | Anti-wear additive, preparation method therefor, use thereof, and lubricating oil containing same |
CN109659515A (en) * | 2018-11-23 | 2019-04-19 | 贵州梅岭电源有限公司 | A kind of preparation method of the fluorination carbon electrode material of Ag C modification |
CN110783522A (en) * | 2018-11-23 | 2020-02-11 | 贵州梅岭电源有限公司 | Preparation method of nanomaterial-modified carbon fluoride electrode material |
CN109698365A (en) * | 2018-12-05 | 2019-04-30 | 上海空间电源研究所 | A kind of lithium metal battery with elastic buffer structure |
CN109873137A (en) * | 2019-02-01 | 2019-06-11 | 贵州梅岭电源有限公司 | A kind of V2O5The preparation method of the fluorocarbons positive electrode of@C modification |
CN112186139A (en) * | 2019-07-04 | 2021-01-05 | 上海大学 | Single-metal atom point modified carbon fluoride anode material and preparation method thereof |
CN114400305A (en) * | 2021-12-14 | 2022-04-26 | 中国电子科技集团公司第十八研究所 | Thermal battery high-voltage spherical carbon fluoride anode material and preparation method thereof |
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