CN101986442A - Lithium ion battery cathode material containing three-dimensional conductive structure and preparation method thereof - Google Patents
Lithium ion battery cathode material containing three-dimensional conductive structure and preparation method thereof Download PDFInfo
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- CN101986442A CN101986442A CN2010101813862A CN201010181386A CN101986442A CN 101986442 A CN101986442 A CN 101986442A CN 2010101813862 A CN2010101813862 A CN 2010101813862A CN 201010181386 A CN201010181386 A CN 201010181386A CN 101986442 A CN101986442 A CN 101986442A
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Abstract
The invention relates to a lithium ion battery cathode material containing a three-dimensional conductive structure and a preparation method thereof. Nano silicon powder is adopted as a core and is coated by a nano carbon material to form a core-containing conductor, and the core-containing conductor is coated by nano metal or metal oxide again, so lithium ion battery cathode material silicon nanoparticles containing the three-dimensional conductive structure are formed through the two-time coating; and the invention also relates to a preparation method for the cathode material. The lithium ion battery cathode material prepared by the method contains the three-dimensional conductive structure, has the capacity of more than 1,500mAh/g and keeps over 80 percent of the capacity after 500-time circulation.
Description
Technical field
The present invention relates to a kind of inside and contain the lithium ion battery negative material of three-dimensional conductive structure, particularly relate to a kind of nano-carbon material and nano metal or metallic compound lithium ion battery negative material of twice clad nano silica flour respectively that adopts.
Background technology
Since Japanese Sony company in 1991 is with the lithium ion battery commercialization, lithium ion battery has obtained in fields such as mobile phone, micro-camera, palmtop PC, notebook computers rapidly using widely with its energy density height, operating voltage height, advantages such as load characteristic is good, charging rate is fast, safety non-pollution.
In lithium ion battery, the capacity of negative material is one of key factor that influences battery capacity.At present, the graphite of main employing graphite or modification is the negative material of lithium ion battery in the production.Yet the theoretical embedding lithium heap(ed) capacity of graphite only is 372mAh/g.For the needs of the lithium ion battery that satisfies high-energy-density, the negative material of seeking superelevation storage lithium ability is the research focus in lithium ion battery field always.
The comparatively successful carbon negative pole material of research has Delanium, carbonaceous mesophase spherules (MCMB), petroleum coke, carbon fiber, polymer pyrolysis etc. at present.Usually, the theoretical expression of the compound that lithium forms in material with carbon element is LiC6, is 372mAh/g by stoichiometric theoretical specific capacity.In recent years along with deepening continuously to the material with carbon element research work, have been found that by graphite and all kinds of material with carbon element are carried out surface modification and structural adjustment, or make the graphite part disordering, or in all kinds of material with carbon elements, form structures such as nano level hole, hole and passage, lithium therein embedding/taking off embedding not only can be undertaken by stoichiometry LiC6, but also chemical non-metering embedding/take off embedding can be arranged, its specific capacity increases greatly, theoretical value 372mAh/g by LiC6 brings up to 700～1000mAh/g, thereby the specific capacity of lithium ion battery is increased greatly.
Owing to exist specific capacity low, first charge-discharge efficiency is low as lithium ion battery negative material for carbon, forms the SEI film, and high-temperature electrolysis matter decomposes the uneasy congruent problem of bringing, and people have begun the research of the non-carbon negative pole material of other novel height ratio capacity.
Silicon has the theoretical embedding lithium capacity of 4200mAh/g, be the promising negative material of a class, but irreversible capacity is big first, and cycle performance is poor, is difficult to direct negative material as lithium ion battery.Nanometer can be improved the cycle performance of electrode under the prerequisite that guarantees embedding lithium capacity, but still is difficult to satisfy the requirement of lithium ion battery.
Summary of the invention
It is kernel that the present invention adopts nano silica fume, form conductor with nuclear with nano-carbon material clad nano silica flour, with nano metal or metal oxide conductor with nuclear is coated once more, promptly constitute the lithium ion battery negative material silicon micro particles that three-dimensional conductive structure is contained in a kind of inside through twice coating, and provided the preparation method of this negative material.
Wherein, described conductor with nuclear shell and kernel form first conductive layer, and the housing of Bao Fuing forms second conductive layer once more, and second conductive layer and first conductive layer form three-dimensional conductive network jointly.
Described nano-carbon material is one or more in native graphite, Delanium, CNT (carbon nano-tube), nano-sized carbon microballoon, the carbon fiber.
Described nano metal or metallic compound are one or more in nanometer metallic silver, copper, aluminium, magnesium oxide, aluminium oxide, magnesium hydroxide, the aluminium hydroxide.
Described silicon micro particles granularity is 2-100um.
Described nano silica fume granularity is 2-100nm.
The preparation method of the lithium ion battery negative material of three-dimensional conductive structure is contained in a kind of inside, and its step condition is:
(1) coats first: the nano silica fume of percentage by weight 20%～60% and the nano-carbon 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 silica fume mix with nano-carbon 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, 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 silica flour;
(2) coat once more: 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 ℃, with the high-temperature vapour is that carrier makes coating mix with nano metal or metallic compound, 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, temperature rises to 400-1000 ℃, 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.
The lithium ion battery negative material of the present invention's preparation, the inner three-dimensional conductive structure that forms, material is applied to lithium ion battery negative material, and its capacity is greater than 1500mAh/g, and 500 times circulation volume keeps more than 80%.
Description of drawings
Fig. 1 is the lithium ion battery negative material structural representation that three-dimensional conductive structure is contained in inside of the present invention.
In the accompanying drawing, 1 is the inner lithium ion battery negative material silicon micro particles that contains three-dimensional conductive structure, 2 for being coated on second conductive layer on conductor with nuclear surface, 3 for being coated on first conductive layer on nano silica fume surface, 4 is nano silica fume, and 5 is lithium ion battery negative material silicon micro particles interior three-dimensional conductive network.
Embodiment
Embodiment one:
30 kilograms of nano silica fumes and 70 kilograms of nano-carbon materials 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 silica fume mix with nano-carbon 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, 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 nano-carbon material clad nano silica flour;
With coating and copper nanoparticle according to percentage by weight 10%: 90%, 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 coating mix with copper nanoparticle, stir in nanometer high pressure high temperature vapor mixer 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.
The negative material that adopts present embodiment to form three-dimensional netted conductive structure is used for lithium ion battery, and capacitance is 1550mAh/g, circulates after 500 times, and capacity attenuation is 8%.
Embodiment two:
60 kilograms of nano silica fumes and 40 kilograms of nano-carbon materials 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 silica fume mix with nano-carbon 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, 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 nano-carbon material clad nano silica flour;
With coating and nano-sized magnesium hydroxide powder according to percentage by weight 20%: 80%, 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 coating mix with the nano-sized magnesium hydroxide powder, stir in nanometer high pressure high temperature vapor mixer 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.
The negative material that adopts present embodiment to form three-dimensional netted conductive structure is used for lithium ion battery, and capacitance is 1528mAh/g, circulates after 500 times, and capacity attenuation is 7%.
Embodiment three:
40 kilograms of nano silica fumes and 60 kilograms of nano-carbon materials 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 silica fume mix with nano-carbon 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, 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-carbon material clad nano silica flour;
With coating and nanometer aluminium powder according to percentage by weight 30%: 70%, 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 coating mix with nanometer aluminium powder, stir in nanometer high pressure high temperature vapor mixer 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.
The negative material that adopts present embodiment to form three-dimensional netted conductive structure is used for lithium ion battery, and capacitance is 1540mAh/g, circulates after 500 times, and capacity attenuation is 7.6%.
Claims (6)
1. the lithium ion battery negative material of three-dimensional conductive structure is contained in an inside, it is characterized in that: described negative material is kernel with the nano silica fume, form conductor with nuclear with nano-carbon material clad nano silica flour, 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 of Bao Fuing forms second conductive layer once more, promptly constitute negative material silicon micro particles through twice coating, second conductive layer and first conductive layer of this silicon micro particles form three-dimensional conductive network jointly.
2. the lithium ion battery negative material of three-dimensional conductive structure is contained in a kind of inside as claimed in claim 1, it is characterized in that: described nano-carbon material is one or more in native graphite, Delanium, CNT (carbon nano-tube), nano-sized carbon microballoon, the carbon fiber.
3. the lithium ion battery negative material of three-dimensional conductive structure is contained in a kind of inside as claimed in claim 1, it is characterized in that: described nano metal or metallic compound are one or more in nanometer metallic silver, copper, aluminium, magnesium oxide, aluminium oxide, magnesium hydroxide, the aluminium hydroxide.
4. the lithium ion battery negative material of three-dimensional conductive structure is contained in a kind of inside as claimed in claim 1, it is characterized in that: described silicon micro particles granularity is 2-100um.
5. the lithium ion battery negative material of three-dimensional conductive structure is contained in a kind of inside as claimed in claim 1, it is characterized in that: described nano silica fume granularity is 2-100nm.
6. the preparation method of the lithium ion battery negative material of three-dimensional conductive structure is contained in a kind of inside as claimed in claim 1, and its step condition is:
(1) coats first: the nano silica fume of percentage by weight 20%～60% and the nano-carbon 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 silica fume mix with nano-carbon 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, 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 silica flour;
(2) coat once more: 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 ℃, with the high-temperature vapour is that carrier makes coating mix with nano metal or metallic compound, 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, temperature rises to 400-1000 ℃, 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.
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Cited By (11)
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|---|---|---|---|---|
| CN102324508A (en) * | 2011-09-14 | 2012-01-18 | 耿世达 | The alloy that three-dimensional conductive structure is contained in a kind of inside coats negative material and preparation method thereof |
| CN102332571A (en) * | 2011-09-21 | 2012-01-25 | 广东达之邦新能源技术有限公司 | Silicon-carbon compound cathode material and manufacturing method thereof as well as lithium ion battery and cathode piece |
| CN104701487A (en) * | 2013-12-10 | 2015-06-10 | 通用汽车环球科技运作有限责任公司 | Nanocomposite coatings to obtain high performing silicon anodes |
| US9531004B2 (en) | 2013-12-23 | 2016-12-27 | GM Global Technology Operations LLC | Multifunctional hybrid coatings for electrodes made by atomic layer deposition techniques |
| CN108376781A (en) * | 2018-04-17 | 2018-08-07 | 天津巴莫科技股份有限公司 | A kind of lithium-ion-power cell silicon-carbon cathode material and preparation method thereof |
| US10164245B2 (en) | 2016-09-19 | 2018-12-25 | GM Global Technology Operations LLC | High performance silicon electrodes having improved interfacial adhesion between binder, silicon and conductive particles |
| US10396360B2 (en) | 2016-05-20 | 2019-08-27 | Gm Global Technology Operations Llc. | Polymerization process for forming polymeric ultrathin conformal coatings on electrode materials |
| CN110335996A (en) * | 2019-05-28 | 2019-10-15 | 上海德朗能动力电池有限公司 | A kind of high capacity lithium ion cells cathode and its application |
| CN111149241A (en) * | 2019-12-30 | 2020-05-12 | 上海杉杉科技有限公司 | Silicon-based lithium storage material and preparation method thereof |
| US10868307B2 (en) | 2018-07-12 | 2020-12-15 | GM Global Technology Operations LLC | High-performance electrodes employing semi-crystalline binders |
| US11228037B2 (en) | 2018-07-12 | 2022-01-18 | GM Global Technology Operations LLC | High-performance electrodes with a polymer network having electroactive materials chemically attached thereto |
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Cited By (15)
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| CN102324508A (en) * | 2011-09-14 | 2012-01-18 | 耿世达 | The alloy that three-dimensional conductive structure is contained in a kind of inside coats negative material and preparation method thereof |
| CN102332571A (en) * | 2011-09-21 | 2012-01-25 | 广东达之邦新能源技术有限公司 | Silicon-carbon compound cathode material and manufacturing method thereof as well as lithium ion battery and cathode piece |
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| CN104701487A (en) * | 2013-12-10 | 2015-06-10 | 通用汽车环球科技运作有限责任公司 | Nanocomposite coatings to obtain high performing silicon anodes |
| US9531004B2 (en) | 2013-12-23 | 2016-12-27 | GM Global Technology Operations LLC | Multifunctional hybrid coatings for electrodes made by atomic layer deposition techniques |
| US10396360B2 (en) | 2016-05-20 | 2019-08-27 | Gm Global Technology Operations Llc. | Polymerization process for forming polymeric ultrathin conformal coatings on electrode materials |
| US10991946B2 (en) | 2016-05-20 | 2021-04-27 | GM Global Technology Operations LLC | Polymerization process for forming polymeric ultrathin conformal coatings on electrode materials |
| US10164245B2 (en) | 2016-09-19 | 2018-12-25 | GM Global Technology Operations LLC | High performance silicon electrodes having improved interfacial adhesion between binder, silicon and conductive particles |
| CN108376781A (en) * | 2018-04-17 | 2018-08-07 | 天津巴莫科技股份有限公司 | A kind of lithium-ion-power cell silicon-carbon cathode material and preparation method thereof |
| US10868307B2 (en) | 2018-07-12 | 2020-12-15 | GM Global Technology Operations LLC | High-performance electrodes employing semi-crystalline binders |
| US11228037B2 (en) | 2018-07-12 | 2022-01-18 | GM Global Technology Operations LLC | High-performance electrodes with a polymer network having electroactive materials chemically attached thereto |
| CN110335996A (en) * | 2019-05-28 | 2019-10-15 | 上海德朗能动力电池有限公司 | A kind of high capacity lithium ion cells cathode and its application |
| CN111149241A (en) * | 2019-12-30 | 2020-05-12 | 上海杉杉科技有限公司 | Silicon-based lithium storage material and preparation method thereof |
| WO2021134195A1 (en) * | 2019-12-30 | 2021-07-08 | 上海杉杉科技有限公司 | Silicon-based lithium-storage material and preparation method therefor |
| CN111149241B (en) * | 2019-12-30 | 2023-11-28 | 上海杉杉科技有限公司 | Silicon-based lithium storage material and preparation method thereof |
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Application publication date: 20110316 |