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Bimetal oxide and graphene composite material and preparation method thereof

A technology of double metal oxide and composite materials, which is applied in the field of preparation of graphene composite materials, can solve the problems that affect the properties, types and quantities of materials that are difficult to accurately control, and the molar ratio is difficult to accurately control, and achieve the effect of avoiding damage

Active Publication Date: 2018-09-28
HARBIN ENG UNIV
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  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Question 1: Existing technology in the synthesis of double metal oxides AB 2 o 4 In the process, the molar ratio of the two metals A and B is difficult to control accurately: the traditional method is to co-precipitate with two soluble metal salts to form a precursor by urea decomposition, and then obtain a double metal oxide by calcination
OH decomposed by urea - When co-precipitating with two metal cations, choose to be with OH - It is difficult to accurately control the type and quantity of the combined metal cations, so it is difficult to accurately control the type and molecular formula ratio of the precursors generated, so the product is often accompanied by more by-products
[0004] Problem 2: It is difficult to realize the compounding of bimetallic oxide and graphene through in-situ growth in the existing technology: the existing technology is mainly to obtain the bimetallic oxide under the condition of high-temperature aerobic calcination, because carbon materials such as graphene are in the It is flammable in the air, so the bimetallic oxide produced can only be composited with graphene after high-temperature calcination. The composite of the two can only be physically mixed with the bimetallic oxide and carbon material, which seriously affects the performance of the material.
[0005] Problem 3: It is difficult to realize the formation of double metal oxides with uniform particle size nanocube morphology on the surface of graphene by chemical growth

Method used

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  • Bimetal oxide and graphene composite material and preparation method thereof
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  • Bimetal oxide and graphene composite material and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0038] A kind of double metal oxide / graphene composite material preparation method, concrete steps are as follows:

[0039] Step 1, preparing a graphene oxide dispersion with a concentration of 3 mg / mL, adding metal chloride salt to it, controlling the concentration at 1 to 10 mmol / L, and recording it as solution 1; preparing a potassium metal cyanate solution with a concentration equal to that of metal chloride The salt is the same, and is recorded as solution 2;

[0040]Step 2: After stirring solution 1 and solution 2 evenly, add solution 2 dropwise to solution 1 at a volume ratio of 2:3 at a rate of 0.5-1 mL / min, and stir for 10 min;

[0041] Step 3, transfer the above mixed solution to a high temperature and high pressure reactor, and conduct a hydrothermal reaction at 120°C for 6 hours; continue to adjust the temperature to 180-220°C, and conduct a hydrothermal reaction for 18 hours. After natural cooling, the load AB is obtained 2 o 4 graphene hydrogel materials.

Embodiment 2

[0043] The steps of this embodiment are basically the same as those of Example 1, except that in step 1, the metal chloride salt is NiCl 2 , potassium metal cyanate is K 3 [Fe(CN) 6 ]; Step 3 continues to regulate the temperature to 180 ° C.

[0044] figure 1 It is the XRD pattern of the obtained material, and it can be seen from the corresponding peak position that the synthesized material is pure phase NiFe 2 o 4 / Graphene. Figure 2(a)-Figure 2(c) For this example NiFe 2 o 4 / Graphene: Figure 2(a) SEM, the magnification of the figure is 30000 times; Figure 2(b) TEM, it can be seen that the obtained NiFe 2 o 4 The nanocubes are loaded on the graphene surface; Figure 2(c) shows the particle size distribution diagram, which shows that the particle size is between 30 and 40nm, and the particle size distribution is relatively uniform.

[0045] Figure 3(a) for NiFe 2 o 4 / graphene material at scanning speeds of 5, 10, 20, 40mV s -1 The cyclic voltammetry curve below,...

Embodiment 3

[0047] The steps of this embodiment are basically the same as those of Embodiment 2, the difference is that in step 1, K 3 [Fe(CN) 6 ] for K 3 [Co(CN) 6 ]; In step 3, "control the temperature to 180°C" is replaced with "control the temperature to 200°C". The synthesized material is NiCo 2 o 4 / graphene material.

[0048] The prepared NiCo 2 o 4 / Graphene material electrochemical performance test shows that the current density is 1, 2, 3, 6A g -1 , the discharge specific capacity is 201, 187, 171, 155F g -1 ; when the current density increases to 6A g -1 , the discharge specific capacitance is still 1A g -1 When discharging 77% of the specific capacitance.

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Abstract

The invention provides a bimetal oxide and graphene composite material and a preparation method thereof. The method comprises the steps of 1: preparing a dispersion from a graphene oxide, and adding ametal chloride salt thereto to obtain a solution 1; preparing a solution 2 having the same concentration as the metal chloride salt from a metallic potassium cyanate salt; 2: stirring the solution 1and the solution 2 uniformly separately, and then dripping the solution 2 into the solution 1 at a ratio of 2:3 by volume; and 3: transferring the mixed solution to a high-temperature and high-pressure reaction vessel, and hydrothermally reacting at 120 DEG C for 6 h; continuing to control the temperature to 180 to 220 DEG C, hydrothermally reacting for 18 h, and performing natural cooling to obtain the bimetal oxide and graphene composite material. In-situ growth of the bimetal oxide on the surface of the carbon material can be realized without high-temperature calcination, and the molar ratio of the two metals in the bimetal oxide can be accurately controlled. The prepared bimetal oxide has regular nanocube morphology.

Description

technical field [0001] What the present invention relates to is a kind of graphene composite material, and the present invention also relates to a kind of preparation method of graphene composite material. Background technique [0002] Supercapacitors are a new type of energy storage device between traditional capacitors and rechargeable batteries, and their electrode materials are divided into two categories, one is based on the storage of energy through the rapid adsorption / desorption of electrolyte ions on the surface of the active electrode material carbon materials; the other category is pseudocapacitive materials that store energy through Faradaic reactions between electrolytes and active materials. Double metal oxide (AB 2 o 4 ) due to its excellent electrical conductivity, and has a variety of oxidation states can carry out a variety of redox reactions to obtain higher specific capacity. Therefore, the composite of carbon material and double metal oxide is an idea...

Claims

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Application Information

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IPC IPC(8): H01G11/26H01G11/30H01G11/32H01G11/46H01G11/86
CPCH01G11/26H01G11/30H01G11/32H01G11/46H01G11/86Y02E60/13
Inventor 曹殿学张旭程魁王贵领陈野朱凯
Owner HARBIN ENG UNIV
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