CN102324508A - The alloy that three-dimensional conductive structure is contained in a kind of inside coats negative material and preparation method thereof - Google Patents
The alloy that three-dimensional conductive structure is contained in a kind of inside coats negative material and preparation method thereof Download PDFInfo
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- CN102324508A CN102324508A CN201110270421A CN201110270421A CN102324508A CN 102324508 A CN102324508 A CN 102324508A CN 201110270421 A CN201110270421 A CN 201110270421A CN 201110270421 A CN201110270421 A CN 201110270421A CN 102324508 A CN102324508 A CN 102324508A
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Abstract
The present invention relates to a kind of inside and contain alloy coating negative material of three-dimensional conductive structure and preparation method thereof.The present invention is kernel with the nano-carbon material; Form conductor with nuclear with nanometer high conductive material clad nano material with carbon element; This conductor with nuclear shell and kernel form first conductive layer; With nano metal or metal oxide conductor with nuclear is coated once more, the housing that coats once more forms second conductive layer, promptly constitutes the negative material micro particles through twice coating; Second conductive layer and first conductive layer of this micro particles form three-dimensional conductive network jointly, do surface treatment and improve negative pole density with Graphene more at last.The lithium ion battery negative material of the present invention preparation is applied in the lithium ion battery, and its capacity can improve charging performance and be up to 20C greater than 500mAh/g, and discharge performance is up to 100C, and after the cycle-index 3000 times, efficient still is 80%.
Description
Technical field
The present invention relates to a kind of inside and contain the alloy coating negative material of three-dimensional conductive structure, particularly relate to a kind of nanometer high conductive material and nano metal or metallic compound lithium ion battery negative material of twice clad nano material with carbon element respectively that adopts.
Background technology
Lithium ion battery is a kind of novel chemical power source, embeds with two abilities respectively and the compound of deviating from lithium ion constitutes as both positive and negative polarity reversiblely.When battery charge, lithium ion takes off embedding and comes out from positive pole, in negative pole, embed; Lithium ion takes off embedding and comes out during discharge from negative pole, in positive pole, embeds.Since Japanese Sony company in 1991 is with the lithium ion battery commercialization; Lithium ion battery is high with its energy density, advantages such as operating voltage is high, load characteristic good, charging rate is fast, safety non-pollution, has obtained in fields such as mobile phone, micro-camera, palmtop PC, notebook computers rapidly using widely.
Graphene has the monolayer carbon atomic thickness, is a kind of novel carbonaceous material that bi-dimensional cellular shape lattice structure is arranged by carbon atom, is the basic composition unit of every other dimension carbonaceous material.Its thickness has only 0.335nm, be merely 200,000 of hair/, can be bundled into the fullerene of zero dimension, be curled into the CNT of one dimension, be piled into three-dimensional graphite.
Graphene has good mechanical, electricity, thermal property.It has highly stable structure.Each carbon atom is perfect in the Graphene lamella arranges, and when receiving external force, carbon atom can flexural deformation, need not arrange again, has kept its structural stability.On the Graphene plane, the arrangement of carbon atom makes its very rigid, and tensile strength can reach 50-200GPa, and modulus of elasticity can reach 1TPa, is the material of preparing in the world at present with high specific strength.
Graphene has excellent conducting performance as the material of Nobel prize for physics acquisition in 2010, and high rate performance is applied in the lithium ion battery negative material, can increase substantially the capacitance and the high rate charge-discharge performance of negative material.
The researcher of Princeton university (Princeton University) points out that a few days ago if adopt Graphene (graphene) electrode, as long as the charging interval of lithium battery can shorten to from 2 hours 10 minutes.This Graphene electrodes manufacturing technology newly developed; Be by the researcher Ilhan Aksay institute common exploitation of the Pacific Northwest National Laboratory under the USDOE (PNNL) with the Princeton University; And licensed to the Vorbeck Materials of manufacturer, prepared to push to commercialization.PNNL representes that the verified ultra-thin graphene platelet in this laboratory can be assembled into the electrode of lithium ion battery, and can significantly shorten the charging required time.
Summary of the invention
The alloy that the present invention provides a kind of inside to contain three-dimensional conductive structure coats negative material; With the nano-carbon material is kernel; Form conductor with nuclear with nanometer high conductive material clad nano material with carbon element, this conductor with nuclear shell and kernel form first conductive layer, with nano metal or metal oxide conductor with nuclear are coated once more; The housing that coats once more forms second conductive layer; Promptly constitute the negative material micro particles through twice coating, second conductive layer and first conductive layer of this micro particles form three-dimensional conductive network jointly, do surface treatment and improve negative pole density with Graphene more at last.
Described nano-carbon material is one or more in electrographite, native graphite, modified graphite, graphitized carbon fibre, petroleum coke, carbonaceous mesophase spherules, resin carbon, organic polymer RESEARCH OF PYROCARBON, carbon black, CNT, Graphene, fullerene, nano-sized carbon microballoon, the carbon fiber.
Described nanometer high conductive material is one or more of silver, copper, CNT.
Described nano metal or metallic compound are the metal or the metallic compound of nanometer metallic silver, copper, tin, aluminium, magnesium.
Described micro particles granularity is 2-100um.
Described Graphene thickness is 1-10nm, and the conductivity at room temperature rate is 800-1200S/cm.
The alloy that the present invention also provides a kind of inside to contain three-dimensional conductive structure coats the preparation method of negative material, and its step condition is:
The formation of (1) first conductive layer: the nano-carbon material of percentage by weight 20%～60% and the nanometer high conductive material of percentage by weight 40～80% are put into nanometer high pressure, high temperature vapor mixer simultaneously; The steam temperature scope is 100-600 ℃; With the high-temperature vapour is that carrier makes nano-carbon material mix with the nanometer high conductive material; In nanometer high pressure, high temperature vapor mixer, stir simultaneously, nanometer high pressure, high temperature vapor mixer heating rate is 100 ℃ of intensifications in per 1 hour, and temperature rises to 500-1000 ℃; Temperature retention time is 2～10 hours, and mixing speed is 60～300 rev/mins; Nanometer high pressure, high temperature vapor mixer temperature drops to 300 ℃-500 ℃, and pressure is 10
-5-10
-3Pa reacted 1～10 hour, made nano-carbon material clad nano high conductive material, and nano-carbon material and nanometer high conductive material form first conductive layer;
The formation of (2) second conductive layers: with the coating in the step (1) and nano metal or metallic compound according to percentage by weight 10%～50%: 50～90%; Put into nanometer high pressure, high temperature vapor mixer simultaneously; The steam temperature scope is 100-600 ℃, is that carrier makes coating mix with nano metal or metallic compound with the high-temperature vapour, in nanometer high pressure, high temperature vapor mixer, stirs simultaneously; Nanometer high pressure, high temperature vapor mixer heating rate is 200 ℃ of intensifications in per 1 hour; Temperature rises to 400-1000 ℃, and temperature retention time is 5～20 hours, and mixing speed is 60～300 rev/mins; Temperature of reaction kettle drops to 400 ℃-800 ℃, and pressure is 10
-5-10
-3Pa reacted 2～20 hours, coating is carried out secondary coat, and nano metal or metallic compound and first conductive layer form three-dimensional conductive network jointly.
(3) Graphene surface treatment: the material after secondary coated is put into the full-automatic Graphene trimmer of the third generation, and material and Graphene after the coating are integrated.
The present invention conducts electricity with three-dimensional how the Mi Hejin coating technology combines with Graphene negative terminal surface treatment technology; The lithium ion battery negative material of preparation; The inner three-dimensional conductive structure that forms; Fill up the slit of graphite layers again with Graphene, improve conductivity, cycle performance and the security performance of negative material.Material is applied in the lithium ion battery, and its capacity can improve charging performance and be up to 20C greater than 500mAh/g; Discharge performance is up to 100C, and after the cycle-index 3000 times, efficient still is 80%; Can make battery in a few minutes, accomplish charging fast, and fail safe improve greatly.
Embodiment
Embodiment one:
30 kilograms of nanometer native graphites and 70 kilograms of CNTs are put into nanometer high pressure, high temperature vapor mixer simultaneously; The steam temperature scope is 100-600 ℃, is that carrier makes CNT mix with the nanometer native graphite with the high-temperature vapour, in nanometer high pressure, high temperature vapor mixer, stirs simultaneously; Nanometer high pressure, high temperature vapor mixer heating rate is 100 ℃ of intensifications in per 1 hour; Temperature rises to 1000 ℃, and temperature retention time is 2 hours, and mixing speed is 100 rev/mins; Nanometer high pressure, high temperature vapor mixer temperature drops to 500 ℃, and pressure is 10
-5Pa reacted 10 hours, made CNT clad nano native graphite;
Coating and copper nanoparticle according to percentage by weight 10%: 90%, are put into nanometer high pressure, high temperature vapor mixer simultaneously, and the steam temperature scope is 100-600 ℃; With the high-temperature vapour is that carrier makes coating mix with copper nanoparticle; In nanometer high pressure, high temperature vapor mixer, stir simultaneously, nanometer high pressure, high temperature vapor mixer heating rate is 200 ℃ of intensifications in per 1 hour, and temperature rises to 1000 ℃; Temperature retention time is 20 hours, and mixing speed is 300 rev/mins; Nanometer high pressure, high temperature vapor mixer temperature drops to 400 ℃, and pressure is 10
-5Pa reacted 20 hours, coating is carried out secondary coat.
Material after secondary coated is put into the full-automatic Graphene trimmer of the third generation, and material and Graphene after the coating are integrated.
The negative material that adopts present embodiment to form is used for lithium ion battery, and capacitance is 550mAh/g, can improve charging performance and be up to 20C, and discharge performance is up to 100C, and after the cycle-index 3000 times, efficient still is 80%.
Embodiment two:
60 kilograms of nanometer carbonaceous mesophase spherules and 40 kilograms of CNTs are put into nanometer high pressure, high temperature vapor mixer simultaneously; The steam temperature scope is 100-600 ℃, is that carrier makes the nanometer carbonaceous mesophase spherules mix with CNT with the high-temperature vapour, in nanometer high pressure, high temperature vapor mixer, stirs simultaneously; Nanometer high pressure, high temperature vapor mixer heating rate is 100 ℃ of intensifications in per 1 hour; Temperature rises to 900 ℃, and temperature retention time is 10 hours, and mixing speed is 300 rev/mins; Nanometer high pressure, high temperature vapor mixer temperature drops to 400 ℃, and pressure is 10
-5Pa reacted 10 hours, made CNT clad nano carbonaceous mesophase spherules;
Coating and nano-sized magnesium hydroxide powder according to percentage by weight 20%: 80%, are put into nanometer high pressure, high temperature vapor mixer simultaneously, and the steam temperature scope is 100-600 ℃; With the high-temperature vapour is that carrier makes coating mix with the nano-sized magnesium hydroxide powder; In nanometer high pressure, high temperature vapor mixer, stir simultaneously, nanometer high pressure, high temperature vapor mixer heating rate is 200 ℃ of intensifications in per 1 hour, and temperature rises to 800 ℃; Temperature retention time is 10 hours, and mixing speed is 300 rev/mins; Nanometer high pressure, high temperature vapor mixer temperature drops to 800 ℃, and pressure is 10
-5Pa reacted 20 hours, coating is carried out secondary coat.
Material after secondary coated is put into the full-automatic Graphene trimmer of the third generation, and material and Graphene after the coating are integrated.
The negative material that adopts present embodiment to form is used for lithium ion battery, and capacitance is 560mAh/g, can improve charging performance and be up to 20C, and discharge performance is up to 100C, and after the cycle-index 3000 times, efficient still is 80%.
Embodiment three:
40 kilograms of carbon nano-fibers and 60 kilograms of Nano Silvers are put into nanometer high pressure, high temperature vapor mixer simultaneously; The steam temperature scope is 100-600 ℃, is that carrier makes carbon nano-fiber mix with Nano Silver with the high-temperature vapour, in nanometer high pressure, high temperature vapor mixer, stirs simultaneously; Nanometer high pressure, high temperature vapor mixer heating rate is 100 ℃ of intensifications in per 1 hour; Temperature rises to 1000 ℃, and temperature retention time is 10 hours, and mixing speed is 300 rev/mins; Nanometer high pressure, high temperature vapor mixer temperature drops to 500 ℃, and pressure is 10
-5Pa reacted 10 hours, made Nano Silver clad nano carbon fiber;
Coating and nanometer aluminium powder according to percentage by weight 30%: 70%, are put into nanometer high pressure, high temperature vapor mixer simultaneously, and the steam temperature scope is 100-600 ℃; With the high-temperature vapour is that carrier makes coating mix with nanometer aluminium powder; In nanometer high pressure, high temperature vapor mixer, stir simultaneously, nanometer high pressure, high temperature vapor mixer heating rate is 200 ℃ of intensifications in per 1 hour, and temperature rises to 800 ℃; Temperature retention time is 10 hours, and mixing speed is 300 rev/mins; Nanometer high pressure, high temperature vapor mixer temperature drops to 800 ℃, and pressure is 10
-5Pa reacted 20 hours, coating is carried out secondary coat.
Material after secondary coated is put into the full-automatic Graphene trimmer of the third generation, and material and Graphene after the coating are integrated.
The negative material that adopts present embodiment to form is used for lithium ion battery, and capacitance is 600mAh/g, can improve charging performance and be up to 20C, and discharge performance is up to 100C, and after the cycle-index 3000 times, efficient still is 80%.
Claims (7)
1. the inside alloy that contains three-dimensional conductive structure coats negative material; It is characterized in that: said negative material is kernel with the nano-carbon material; Form conductor with nuclear with nanometer high conductive material clad nano material with carbon element, this conductor with nuclear shell and kernel form first conductive layer, with nano metal or metal oxide conductor with nuclear are coated once more; The housing that coats once more forms second conductive layer; Promptly constitute the negative material micro particles through twice coating, second conductive layer and first conductive layer of this micro particles form three-dimensional conductive network jointly, do surface treatment and improve negative pole density with Graphene more at last.
2. the alloy that three-dimensional conductive structure is contained in a kind of inside as claimed in claim 1 coats negative material, and it is characterized in that: described nano-carbon material is one or more in electrographite, native graphite, modified graphite, graphitized carbon fibre, petroleum coke, carbonaceous mesophase spherules, resin carbon, organic polymer RESEARCH OF PYROCARBON, carbon black, CNT, Graphene, fullerene, nano-sized carbon microballoon, the carbon fiber.
3. the alloy that three-dimensional conductive structure is contained in a kind of inside as claimed in claim 1 coats negative material, it is characterized in that: described nanometer high conductive material is one or more of silver, copper, CNT.
4. the alloy that three-dimensional conductive structure is contained in a kind of inside as claimed in claim 1 coats negative material, and it is characterized in that: described nano metal or metallic compound are the metal or the metallic compound of nanometer metallic silver, copper, tin, aluminium, magnesium.
5. the alloy that three-dimensional conductive structure is contained in a kind of inside as claimed in claim 1 coats negative material, and it is characterized in that: described micro particles granularity is 2-100um.
6. the alloy that three-dimensional conductive structure is contained in a kind of inside as claimed in claim 1 coats negative material, and it is characterized in that: described Graphene thickness is 1-10nm, and the conductivity at room temperature rate is 800-1200S/cm.
7. the preparation method of the alloy coating negative material of three-dimensional conductive structure is contained in a kind of inside as claimed in claim 1, and its step condition is:
The formation of (1) first conductive layer: the nano-carbon material of percentage by weight 20%～60% and the nanometer high conductive material of percentage by weight 40～80% are put into nanometer high pressure, high temperature vapor mixer simultaneously; The steam temperature scope is 100-600 ℃; With the high-temperature vapour is that carrier makes nano-carbon material mix with the nanometer high conductive material; In nanometer high pressure, high temperature vapor mixer, stir simultaneously, nanometer high pressure, high temperature vapor mixer heating rate is 100 ℃ of intensifications in per 1 hour, and temperature rises to 500-1000 ℃; Temperature retention time is 2～10 hours, and mixing speed is 60～300 rev/mins; Nanometer high pressure, high temperature vapor mixer temperature drops to 300 ℃-500 ℃, and pressure is 10
-5-10
-3Pa reacted 1～10 hour, made nano-carbon material clad nano high conductive material, and nano-carbon material and nanometer high conductive material form first conductive layer;
The formation of (2) second conductive layers: with the coating in the step (1) and nano metal or metallic compound according to percentage by weight 10%～50%: 50～90%; Put into nanometer high pressure, high temperature vapor mixer simultaneously; The steam temperature scope is 100-600 ℃, is that carrier makes coating mix with nano metal or metallic compound with the high-temperature vapour, in nanometer high pressure, high temperature vapor mixer, stirs simultaneously; Nanometer high pressure, high temperature vapor mixer heating rate is 200 ℃ of intensifications in per 1 hour; Temperature rises to 400-1000 ℃, and temperature retention time is 5～20 hours, and mixing speed is 60～300 rev/mins; Temperature of reaction kettle drops to 400 ℃-800 ℃, and pressure is 10
-5-10
-3Pa reacted 2～20 hours, coating is carried out secondary coat, and nano metal or metallic compound and first conductive layer form three-dimensional conductive network jointly.
(3) Graphene surface treatment: the material after secondary coated is put into the full-automatic Graphene trimmer of the third generation, and material and Graphene after the coating are integrated.
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| CN201110270421A CN102324508A (en) | 2011-09-14 | 2011-09-14 | The alloy that three-dimensional conductive structure is contained in a kind of inside coats negative material and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102800852A (en) * | 2012-08-28 | 2012-11-28 | 湖南德天新能源科技有限公司 | Preparation method of negative electrode material of power lithium-ion battery |
| CN104332594A (en) * | 2014-10-10 | 2015-02-04 | 奇瑞汽车股份有限公司 | Silicon-based negative electrode material and preparation method and application thereof |
| CN107093710A (en) * | 2017-03-31 | 2017-08-25 | 宁夏博尔特科技有限公司 | Two-coat lithium ion battery negative material and preparation method thereof and lithium ion battery |
| CN109888243A (en) * | 2019-03-13 | 2019-06-14 | 蒙娜丽莎集团股份有限公司 | A kind of preparation method of multistage composite metal oxide functional ceramics |
| CN110423379A (en) * | 2019-08-12 | 2019-11-08 | 哈尔滨理工大学 | A kind of magnesium hydroxide/graphene platelet composite flame-retardant agent and preparation method thereof |
| CN114335552A (en) * | 2022-03-15 | 2022-04-12 | 浙江帕瓦新能源股份有限公司 | Positive electrode material, modification process thereof and solid-state battery |
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| CN101986442A (en) * | 2010-05-25 | 2011-03-16 | 耿世达 | Lithium ion battery cathode material containing three-dimensional conductive structure and preparation method thereof |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102800852A (en) * | 2012-08-28 | 2012-11-28 | 湖南德天新能源科技有限公司 | Preparation method of negative electrode material of power lithium-ion battery |
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| CN104332594A (en) * | 2014-10-10 | 2015-02-04 | 奇瑞汽车股份有限公司 | Silicon-based negative electrode material and preparation method and application thereof |
| CN107093710A (en) * | 2017-03-31 | 2017-08-25 | 宁夏博尔特科技有限公司 | Two-coat lithium ion battery negative material and preparation method thereof and lithium ion battery |
| CN107093710B (en) * | 2017-03-31 | 2019-10-08 | 宁夏博尔特科技有限公司 | Two-coat lithium ion battery negative material and preparation method thereof and lithium ion battery |
| CN109888243A (en) * | 2019-03-13 | 2019-06-14 | 蒙娜丽莎集团股份有限公司 | A kind of preparation method of multistage composite metal oxide functional ceramics |
| CN110423379A (en) * | 2019-08-12 | 2019-11-08 | 哈尔滨理工大学 | A kind of magnesium hydroxide/graphene platelet composite flame-retardant agent and preparation method thereof |
| CN110423379B (en) * | 2019-08-12 | 2021-05-07 | 哈尔滨理工大学 | Magnesium hydroxide/graphene sheet composite flame retardant and preparation method thereof |
| CN114335552A (en) * | 2022-03-15 | 2022-04-12 | 浙江帕瓦新能源股份有限公司 | Positive electrode material, modification process thereof and solid-state battery |
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Application publication date: 20120118 |