CN103482619B - A kind of Graphene-copper oxide three-dimensional foam composite material - Google Patents
A kind of Graphene-copper oxide three-dimensional foam composite material Download PDFInfo
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- CN103482619B CN103482619B CN201310409064.2A CN201310409064A CN103482619B CN 103482619 B CN103482619 B CN 103482619B CN 201310409064 A CN201310409064 A CN 201310409064A CN 103482619 B CN103482619 B CN 103482619B
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Abstract
The present invention discloses a kind of preparation method of Graphene-copper oxide three-dimensional foam composite material, comprises the following steps: step one, material oxidation Graphene and mantoquita is mixed than soluble in water by certain mass; Step 2, graphene oxide to be separated by centrifugal or suction filtration by the liquid mixed in step one, and with water or alcohol washes clean; Step 3, the product obtained in step 2 is re-dispersed in the aqueous solution, subsequently product is carried out lyophilize process; Step 4, by step 3 obtain product thermal treatment under air or oxygen obtain Graphene-copper oxide three-dimensional foam composite material, wherein said thermal treatment temp is at 150-800 degree Celsius, and heat treatment time was at 10 seconds-10 hours.
Description
Technical field
The present invention relates to nano material and manufacture field, particularly relate to a kind of preparation method of Graphene-copper oxide three-dimensional foam composite material.
Background technology
Cupric oxide is a kind of p-type semiconductor material, can be used for gas detection, solar energy converting, CO catalyzed oxidation and lithium ion battery electrode material etc.Copper oxide nano material specific surface area is high, has dimensional effect and quantum tunneling effect, and its every property can be more excellent than macroscopic material.But nano particle is easily reunited usually, constrain its practical application.Graphene is by a kind of carbon material with bi-dimensional cellular shape structure of monolayer carbon atomic arrangement, has excellent mechanical property, electric property.Meanwhile, Graphene has high specific surface area, can as the solid support material of nano material.By copper oxide nanometer particle and Graphene compound, can the reunion of inhibited oxidation copper nano particles, improve the excellent properties of copper oxide material.
The preparation method of current Graphene-cupric oxide matrix material is comparatively complicated, usually needs to add number of chemical reagent, or needs hydro-thermal reaction or backflow experiment.Nanoscale2 (2010) 988 discloses a kind of synthetic method based on water-aqueous isopropanol, and obtain graphene oxide-CuO particulate composite by backflow experiment, wherein cupric oxide size is about 50 nanometers.Materialsletters105 (2013) 242-245 discloses a kind of preparation method of CuO-Graphene, first graphene oxide high-temperature heat treatment is reduced to Graphene, then miscible in ethanolic soln with cupric nitrate, dried by solution subsequently and within 10 hours, obtain CuO-graphene composite material at 200 degrees Centigrade, wherein cupric oxide size is about 150 nanometers.
Summary of the invention
In order to reduce the preparation cost of Graphene-cupric oxide matrix material, simplify preparation technology, optimize the size of copper oxide nanometer particle, the invention provides a kind of preparation method of new Graphene-copper oxide three-dimensional foam composite material, only aerobic functionalized graphene and mantoquita two kinds of reagent.
The present invention is by the following technical solutions: a kind of preparation method of Graphene-copper oxide three-dimensional foam composite material, will carry out after soluble in water to material oxidation Graphene and mantoquita mixing being separated, cleaning; The product obtained is re-dispersed in the aqueous solution, and carries out lyophilize; Dried product exhibited heat treated certain hour under air or oxygen is obtained a kind of Graphene-copper oxide three-dimensional foam composite material.
Described mantoquita is any one in copper sulfate, cupric chloride, venus crystals or cupric nitrate.
Described thermal treatment temp is at 150-800 degree Celsius.
Heat treatment time was at 10 seconds-10 hours.
Described graphene oxide and the mass ratio of mantoquita are 1:10-10:1.
Described freezing dry process comprises and first graphene oxide is become solid-state with the mixing solutions of mantoquita by refrigeration compressor or liquid nitrogen freezing, makes water sublimed obtain graphene oxide-mantoquita foam subsequently under lower pressure.
Beneficial effect of the present invention: the present invention does not need other chemical reagent, method is simple, and environmental protection, reduces production cost simultaneously, and the nanoparticle size obtained is only 10 ran
Accompanying drawing explanation
Fig. 1 is the transmission electron microscope figure of the Graphene-copper oxide three-dimensional foam composite material that the embodiment of the present invention 1 obtains;
Fig. 2 is the scanning electron microscope diagram of the Graphene-copper oxide three-dimensional foam composite material that the embodiment of the present invention 1 obtains.
Embodiment:
Below in conjunction with embodiment and accompanying drawing the present invention done and further explain.According to following embodiment, can better understand the present invention.But concrete material proportion, processing condition and result thereof described by embodiment only for illustration of the present invention, and should can not limit the present invention described in detail in claims yet.
Embodiment 1
Material oxidation Graphene and cupric nitrate are respectively got 50mg to be dissolved in 100ml deionized water, by carrying out centrifugation after ultrasonic mixing and cleaning up;
The product obtained again ultrasonic disperse, in 50ml deionized water, is then obtained solution and obtains solid through liquid nitrogen freezing, transferred to subsequently in freeze drier and carry out lyophilize process;
The product obtained is heated in atmosphere 150 DEG C of insulations and obtains Graphene-copper oxide three-dimensional foam composite material in 10 hours.
Carry out transmission electron microscope sign to product, result as shown in Figure 1, finds that ferric oxide nanoparticle size is less than 10 nanometers.Carry out scanning electron microscope sign to product, as shown in Figure 2, visible matrix material is vesicular structure to result.
Embodiment 2
Getting graphene oxide 10mg and cupric chloride 20mg is dissolved in 20ml deionized water, by carrying out centrifugation after being uniformly mixed and cleaning up;
The product obtained is re-dispersed in 20ml deionized water, then solution is carried out the freezing and drying treatment of refrigeration compressor;
The product obtained is heated in oxygen 500 DEG C of insulations and obtains Graphene-copper oxide three-dimensional foam composite material in 10 minutes.
Acquired results is similar to Example 1.
Embodiment 3
Getting graphene oxide 100mg and venus crystals 10mg is dissolved in 100ml deionized water, by carrying out centrifugation after ultrasonic mixing and cleaning up;
The product obtained is re-dispersed in 100ml deionized water, then solution is carried out the freezing and drying treatment of refrigeration compressor;
The product obtained is heated in atmosphere 800 DEG C of insulations and obtains Graphene-copper oxide three-dimensional foam composite material in 10 seconds.
Acquired results is similar to Example 1.
Claims (4)
1. a preparation method for Graphene-copper oxide three-dimensional foam composite material, is characterized in that, will carry out after soluble in water to material oxidation Graphene and mantoquita mixing being separated, cleaning; The product obtained is re-dispersed in the aqueous solution, and carries out lyophilize; Dried product exhibited heat treated certain hour under air or oxygen is obtained a kind of Graphene-copper oxide three-dimensional foam composite material; Described thermal treatment temp is at 150-800 degree Celsius.
2. the preparation method of a kind of Graphene-copper oxide three-dimensional foam composite material according to claim 1, is characterized in that, described mantoquita is any one in copper sulfate, cupric chloride, venus crystals or cupric nitrate.
3. the preparation method of a kind of Graphene-copper oxide three-dimensional foam composite material according to claim 1, is characterized in that, heat treatment time was at 10 seconds-10 hours.
4. the preparation method of a kind of Graphene-copper oxide three-dimensional foam composite material according to claim 1, is characterized in that, described graphene oxide and the mass ratio of mantoquita are 1:10-10:1.
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| CN201310409064.2A CN103482619B (en) | 2013-09-09 | 2013-09-09 | A kind of Graphene-copper oxide three-dimensional foam composite material |
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| CN201310409064.2A CN103482619B (en) | 2013-09-09 | 2013-09-09 | A kind of Graphene-copper oxide three-dimensional foam composite material |
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| CN103482619A CN103482619A (en) | 2014-01-01 |
| CN103482619B true CN103482619B (en) | 2016-02-24 |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105036174A (en) * | 2015-07-10 | 2015-11-11 | 安鹏九 | Production method for submicron electronic-grade copper oxide powder |
| CN105923641B (en) * | 2016-04-26 | 2017-05-03 | 天津大学 | Preparation method of high-temperature and oxidation resisting heat conduction alumina/graphene foam composite material |
| CN108202146B (en) * | 2017-12-29 | 2019-11-22 | 华中科技大学 | A kind of three-dimensional porous graphene package nano zero-valence carbon/carbon-copper composite material and preparation method |
| CN108862248A (en) * | 2018-08-06 | 2018-11-23 | 南京工业大学 | A kind of quick macroblock quantization prepares graphene-metal oxide composite powder material method |
| CN113659193B (en) * | 2021-08-27 | 2023-09-01 | 西北工业大学 | All-solid-state sodium ion battery cell structure, preparation method and battery |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102185143A (en) * | 2011-04-02 | 2011-09-14 | 浙江大学 | Transition metal oxide/ graphene composite material and preparation method thereof |
| CN102765715A (en) * | 2012-07-12 | 2012-11-07 | 上海大学 | Graphene-loaded lamellar cupric oxide composite material and hydro-thermal synthesis method thereof |
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| CN102076447B (en) * | 2008-06-30 | 2014-12-17 | 同和电子科技有限公司 | Metal microparticle containing composition and process for production of the same |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102185143A (en) * | 2011-04-02 | 2011-09-14 | 浙江大学 | Transition metal oxide/ graphene composite material and preparation method thereof |
| CN102765715A (en) * | 2012-07-12 | 2012-11-07 | 上海大学 | Graphene-loaded lamellar cupric oxide composite material and hydro-thermal synthesis method thereof |
Non-Patent Citations (1)
| Title |
|---|
| Facile, mild and fast thermal-decomposition reduction of graphene oxide in air and its application in high-performance lithium batteries;Zhong-li Wang等;《Chem. Commun.》;20111124;第48卷;参见补充材料第2.2节实验部分，图S1-S9，图2 * |
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