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Preparation method of micro-nano dimensional graphene/lithium titanate composite negative electrode material

A negative electrode material, micro-nano-scale technology, applied in the field of preparation of graphene/lithium titanate composite negative electrode material, can solve the problems affecting the electrical conductivity of the material, long diffusion distance, low specific capacity, etc., to improve the reaction efficiency and diffusion distance Small, great performance

Active Publication Date: 2016-05-18
山东信开源科技创新发展有限责任公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, graphene as an electrode material needs to solve two problems: one is the relatively low specific capacity, because a lithium ion can only combine with six carbon atoms to form LiC between the structure of graphene and the relatively dense graphite layer. 6 Second, the special shape and size of graphene lead to a longer diffusion distance between lithium ions into graphene layers
[0009] In the above-mentioned comparative documents, comparative documents 1-3 give the graphene oxide / lithium titanate precursor obtained by compounding lithium source, titanium source and graphene oxide solution through liquid phase method, and then reducing the graphene oxide in the precursor Graphene, thereby obtaining the idea of ​​lithium titanate / graphene composite negative electrode material, but the molecules of titanium source and lithium source in the above preparation method cannot fully combine with graphene oxide, so the distance between molecules is relatively large, so that The size of the prepared lithium titanate / graphene material is large, which affects the electrical conductivity of the prepared material

Method used

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  • Preparation method of micro-nano dimensional graphene/lithium titanate composite negative electrode material
  • Preparation method of micro-nano dimensional graphene/lithium titanate composite negative electrode material
  • Preparation method of micro-nano dimensional graphene/lithium titanate composite negative electrode material

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0058] Such as figure 1 As shown, the preparation method of a micro-nano-scale graphene / lithium titanate composite negative electrode material in this embodiment is as follows:

[0059] 1. Selection of raw materials and proportioning

[0060] Deionized water, made by deionized water preparation machine, 30kg;

[0061] Diisopropoxy ethyl diacetoacetate titanium complex (purity) ≥ 98%, 6kg;

[0062] Monolayer graphene oxide, 15kg;

[0063] Isopropanol solution (purity) ≥ 99.9%, 3000L;

[0064] Glacial acetic acid (purity) ≥ 99.9%, 2kg;

[0065] Anhydrous lithium acetate (purity) ≥ 99%, 1kg;

[0066] Deionized water: titanium complex: graphene oxide: glacial acetic acid: lithium acetate mass ratio = 30:6:15:2:1

[0067] Second, select the main equipment:

[0068] Water bath steam heating enamel reaction pot (including condenser, high position and low tank, vacuum system);

[0069] Vacuum drying oven; Pulverizer; Reduction high temperature furnace; Ingredients pot;

[007...

Embodiment 2

[0095] The difference between this embodiment and embodiment 1 is:

[0096] 1. Raw material ratio

[0097] Deionized water, 36kg;

[0098] Diisopropoxy ethyl diacetoacetate titanium complex, 7.3kg;

[0099] Monolayer graphene oxide, 18kg;

[0100] Isopropanol solution, 3600L;

[0101] Glacial acetic acid, 2.4kg;

[0102] Anhydrous lithium acetate, 1.3kg;

[0103] Mass ratio of deionized water: titanium complex: graphene oxide: glacial acetic acid: lithium acetate = 36:7.3:18:2.4:1.3

[0104] 2. Preparation steps

[0105] Step (1) When preparing solution B, slowly add the titanium complex into the batching pot B, and stir for 20 minutes;

[0106] Step (2) When synthesizing the precursor of the graphene oxide / lithium titanate composite, control the temperature at 75°C for vacuum dehydration to obtain a colloidal product, place the colloidal product in a vacuum drying oven, and control the temperature at 85°C for vacuum dehydration. In addition to low boilers, block produ...

Embodiment 3

[0114] The difference between this embodiment and embodiment 1 is:

[0115] 1. Raw material ratio

[0116] Deionized water, 32kg;

[0117] Diisopropoxy ethyl diacetoacetate titanium complex, 6.5kg;

[0118] Monolayer graphene oxide, 16kg;

[0119] Isopropanol solution, 3200L;

[0120] Glacial acetic acid, 2.2kg;

[0121] Anhydrous lithium acetate, 1.1kg;

[0122] Mass ratio of deionized water: titanium complex: graphene oxide: glacial acetic acid: lithium acetate = 32:6.5:16:2.2:1.1

[0123] 2. Preparation steps

[0124] Step (1) When preparing solution B, slowly add the titanium complex into the batching pot B, and stir for 15 minutes;

[0125] Step (2) During the synthesis of the graphene oxide / lithium titanate composite precursor, control the temperature at 72°C for vacuum dehydration to obtain a colloidal product, place the colloidal product in a vacuum drying oven, and control the temperature at 82°C for vacuum dehydration. In addition to low boilers, block produc...

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Abstract

The invention provides a preparation method of a micro-nano dimensional graphene / lithium titanate composite negative electrode material. The preparation method includes the steps of (1) preparation of a graphene oxide / lithium acetate / titanium complex / glacial acetic acid / isopropyl alcohol mixed solution; (2) synthesis of a graphene oxide / lithium titanate compound precursor; and (3) thermal recovery treatment of the graphene oxide / lithium titanate compound precursor. The particle distribution of the graphene / lithium titanate composite negative electrode material is between 200nm and 5mum. Because the size of the prepared graphene is between nanometer and a few of microns, the size is small, the lithium ion of the material has a small diffusion distance, and the micro-nano dimensional graphene / lithium titanate composite negative electrode material has the good electrochemical property. The 1C capacity of the material is larger than 170mAh / g, 10C capacity is larger than 120mAh / g, the energy density can reach 132 watt-hour / kg or more, and the power density reaches 6800 watt / kg or more.

Description

technical field [0001] The invention relates to a preparation method of a graphene / lithium titanate composite negative electrode material, in particular to a preparation method of a micro-nano scale graphene / lithium titanate composite negative electrode material. Background technique [0002] Nano-sized lithium titanate can meet the requirements of hybrid supercapacitors for electrode materials: large capacity, low electrode potential, and long cycle life. The advantages of lithium titanate as the negative electrode material of hybrid supercapacitors include: ① The theoretical specific capacity of lithium titanate is high (175mAh / g), which is much higher than that of activated carbon (40mAh / g); The structure is almost unchanged, with "zero strain" characteristics, so the cycle performance is stable; ③High lithium intercalation potential (1.55Vvs.Li / Li + ), it is not easy to cause the precipitation of metallic lithium, and eliminates potential safety hazards; ④ in lithium ti...

Claims

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Application Information

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IPC IPC(8): H01G11/32H01G11/36H01G11/30H01G11/86B82Y30/00
CPCY02E60/13H01G11/32B82Y30/00H01G11/30H01G11/36H01G11/86
Inventor 王小峰罗丁袁再春
Owner 山东信开源科技创新发展有限责任公司
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