CN103232058A - Method for preparing copper sulphide/graphene nano-composite material - Google Patents
Method for preparing copper sulphide/graphene nano-composite material Download PDFInfo
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- CN103232058A CN103232058A CN2013101827267A CN201310182726A CN103232058A CN 103232058 A CN103232058 A CN 103232058A CN 2013101827267 A CN2013101827267 A CN 2013101827267A CN 201310182726 A CN201310182726 A CN 201310182726A CN 103232058 A CN103232058 A CN 103232058A
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Abstract
The invention relates to a method for preparing a copper sulphide/graphene nano-composite material. The method comprises the following steps of: adding oxidized graphene to dimethyl sulfoxide, and performing ultrasonic processing to obtain a mixed solution having the concentration of 0.22 g/L; adding copper acetate to the mixed solution, stirring until the copper acetate is dissolved and then pouring the solution to a solvothermal reaction kettle for reacting for 6-8 hours under the solvothermal condition of 160-180 DEG C, then centrifuging and washing, and finally, performing vacuum drying. The method provided by the invention is capable of preparing the copper sulphide/graphene nano-composite material by taking common chemicals as the raw materials and using a simple solvothermal reaction experimental device; and the method is moderate in reaction condition and simple in operation process; the desired raw materials are cheap and easy to gain; and the method has no special requirement for equipment.
Description
Technical field
The invention belongs to the preparation field of graphene-based matrix material, particularly the preparation method of a kind of cupric sulfide/graphene nano matrix material.
Background technology
The material that Graphene is made up of the monolayer carbon atomic shell is present known the hardest the thinnest nano material, and Graphene has high specific surface area, can be used as the nanoparticle of substrate material stably dispersing on Graphene.And Graphene has excellent electron transport ability, makes it also have huge application potential in microelectronic field.Graphene is at nano electron device, photon sensor, and all many-sides such as the order-checking of gene electronics and supercomputer have broad prospect of application.
Nano material has the effect of a series of uniquenesses, when particle size enters Nano grade, size confinement meeting causes quantum size effect, small-size effect, surface effects and quantum tunneling effect, thereby make a lot of performance generation qualitative changes of material, present and be different from macroscopical block materials, also be different from the unusual appearance of single isolated atom.At light, electricity, aspects such as magnetic have using value widely.The solvent thermal reaction device is one of equipment of common preparation nano material, is expected to synthetic cupric sulfide/graphene nano matrix material.
Summary of the invention
Technical problem to be solved by this invention provides the preparation method of a kind of cupric sulfide/graphene nano matrix material, and this method is simple to operate, and desired raw material is cheap and easy to get.
The preparation method of a kind of cupric sulfide of the present invention/graphene nano matrix material comprises:
Graphene oxide is joined in the methyl-sulphoxide, ultrasonicly obtain the mixing solutions that concentration is 0.22g/L, in mixing solutions, add neutralized verdigris then, pour into after the stirring and dissolving in the solvent thermal reaction still, reaction is 6-8 hour under 160-180 ℃ of solvent thermal condition, centrifugal, washing then, last vacuum-drying gets final product.
The mass ratio of described graphene oxide and neutralized verdigris is 1:10.
The specification of described solvent thermal reaction still is 60mL.
The compactedness of described solvent thermal reaction still is 80%.
Described washing is for using deionized water and washing with alcohol 3-5 time respectively.
Temperature is controlled to be 50-60 ℃ in the described vacuum-drying, and the time is 6-8 hour.
The present invention is raw material with common pharmaceutical chemicals, can prepare cupric sulfide/graphene nano matrix material with simple solvent thermal reaction experimental installation; This preparation process has advantages such as required starting material are easy to get, price is cheaper, operating process is easy.
Beneficial effect:
(1) starting material required for the present invention be easy to get, cheap, operating process is easy;
(2) the present invention is raw material with common chemical substance, can prepare cupric sulfide/graphene nano matrix material with simple solvent thermal reaction experimental installation.
Description of drawings
Fig. 1 is the transmission electron microscope picture of cupric sulfide/graphene nano matrix material of preparing among the present invention;
Cupric sulfide/graphene nano matrix material high-resolution-ration transmission electric-lens the picture of Fig. 2 for preparing among the present invention;
Fig. 3 is the XRD figure sheet of cupric sulfide/graphene nano matrix material of preparing among the present invention.
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used for explanation the present invention and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Embodiment 1
The graphene oxide that adds 0.01g in the 45mL dimethyl sulfoxide solution forms mixing solutions ultrasonic half an hour, adds the neutralized verdigris of 0.1g in the mixing solutions, stirs and makes it dissolving, and solution is added in the 60mL reactor, reacts 6h under 180 ℃ of conditions.With solution centrifugal, filter after reaction is finished, with throw out in vacuum drying oven dry 60 ℃, 6h namely gets product.
Embodiment 2
The graphene oxide that adds 0.01g in the 45mL dimethyl sulfoxide solution forms mixing solutions ultrasonic half an hour, adds the neutralized verdigris of 0.1g in the mixing solutions, stirs and makes it dissolving, and solution is added in the 60mL reactor, reacts 7h under 170 ℃ of conditions.With solution centrifugal, filter after reaction is finished, with throw out in vacuum drying oven dry 60 ℃, 6h namely gets product.
Embodiment 3
The graphene oxide that adds 0.01g in the 45mL dimethyl sulfoxide solution forms mixing solutions ultrasonic half an hour, adds the neutralized verdigris of 0.1g in the mixing solutions, stirs and makes it dissolving, and solution is added in the 60mL reactor, reacts 8h under 160 ℃ of conditions.With solution centrifugal, filter after reaction is finished, with throw out in vacuum drying oven dry 55 ℃, 7h namely gets product.
Embodiment 4
The graphene oxide that adds 0.01g in the 45mL dimethyl sulfoxide solution forms mixing solutions ultrasonic half an hour, adds the neutralized verdigris of 0.1g in the mixing solutions, stirs and makes it dissolving, and solution is added in the 60mL reactor, reacts 6h under 160 ℃ of conditions.With solution centrifugal, filter after reaction is finished, with throw out in vacuum drying oven dry 50 ℃, 8h namely gets product.
Claims (6)
1. the preparation method of cupric sulfide/graphene nano matrix material comprises:
Graphene oxide is joined in the methyl-sulphoxide, ultrasonicly obtain the mixing solutions that concentration is 0.22g/L, in mixing solutions, add neutralized verdigris then, pour into after the stirring and dissolving in the solvent thermal reaction still, reaction is 6-8 hour under 160-180 ℃ of solvent thermal condition, centrifugal, washing then, last vacuum-drying gets final product.
2. the preparation method of a kind of cupric sulfide according to claim 1/graphene nano matrix material, it is characterized in that: the mass ratio of described graphene oxide and neutralized verdigris is 1:10.
3. the preparation method of a kind of cupric sulfide according to claim 1/graphene nano matrix material, it is characterized in that: the specification of described solvent thermal reaction still is 60mL.
4. the preparation method of a kind of cupric sulfide according to claim 1/graphene nano matrix material, it is characterized in that: the compactedness of described solvent thermal reaction still is 80%.
5. the preparation method of a kind of cupric sulfide according to claim 1/graphene nano matrix material, it is characterized in that: described washing is for using deionized water and washing with alcohol 3-5 time respectively.
6. the preparation method of a kind of cupric sulfide according to claim 1/graphene nano matrix material, it is characterized in that: temperature is controlled to be 50-60 ℃ in the described vacuum-drying, and the time is 6-8 hour.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104237349A (en) * | 2014-10-09 | 2014-12-24 | 无锡百灵传感技术有限公司 | Nano graphene and ferrous sulfide based electrochemical sensor |
| CN104465127A (en) * | 2014-11-22 | 2015-03-25 | 湖南科技大学 | Method for rapid preparation of grapheme/silver sulfide quantum dot nanocomposite and product |
| CN105958037A (en) * | 2016-07-08 | 2016-09-21 | 华东师范大学 | Copper sulphide/graphene composite material for negative electrode of sodium-ion battery and preparation method |
| CN106972161A (en) * | 2017-04-05 | 2017-07-21 | 深圳市佩成科技有限责任公司 | A kind of preparation method of nitrogen-doped graphene/copper sulfide/hollow sulphur composite |
| CN108597906A (en) * | 2018-06-13 | 2018-09-28 | 常熟理工学院 | A kind of preparation method of fiber/graphene/copper sulfide flexible electrode material |
| WO2018184157A1 (en) * | 2017-04-05 | 2018-10-11 | 深圳市佩成科技有限责任公司 | Preparation method of composite material having nitrogen-doped graphene/copper sulfide/hollow sulfur particles |
| CN109573997A (en) * | 2018-11-07 | 2019-04-05 | 江苏城乡建设职业学院 | A kind of preparation method of graphene oxide-loaded vulcanization carbon/carbon-copper composite material |
| CN109607592A (en) * | 2018-12-13 | 2019-04-12 | 温州大学 | Transient metal sulfide/C-base composte material preparation method and applications of N doping |
| CN110085448A (en) * | 2019-05-17 | 2019-08-02 | 西北工业大学 | Copper sulfide with high-energy density/redox graphene composite material and preparation method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101274749A (en) * | 2008-03-25 | 2008-10-01 | 大连理工大学 | Universal synthesis method for porous hollow metallic oxide |
| CN102040239A (en) * | 2011-01-18 | 2011-05-04 | 中科院广州化学有限公司 | Preparation method of submicron CuS (copper sulphide) classification ball |
| CN102760877A (en) * | 2012-07-23 | 2012-10-31 | 浙江大学 | Transition metal sulfide/graphene composite material, and preparation method and application thereof |
-
2013
- 2013-05-16 CN CN2013101827267A patent/CN103232058A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101274749A (en) * | 2008-03-25 | 2008-10-01 | 大连理工大学 | Universal synthesis method for porous hollow metallic oxide |
| CN102040239A (en) * | 2011-01-18 | 2011-05-04 | 中科院广州化学有限公司 | Preparation method of submicron CuS (copper sulphide) classification ball |
| CN102760877A (en) * | 2012-07-23 | 2012-10-31 | 浙江大学 | Transition metal sulfide/graphene composite material, and preparation method and application thereof |
Non-Patent Citations (2)
| Title |
|---|
| JUN LIU ET AL.: "Solvothermal synthesis of copper sulfide semiconductor micro/nanostructures", 《MATERIALS RESEARCH BULLETIN》, vol. 45, 16 December 2009 (2009-12-16), pages 309 - 313, XP026904914, DOI: doi:10.1016/j.materresbull.2009.12.013 * |
| YONGFENG LI ET AL.: "Graphene–ZnS quantum dot nanocomposites produced by solvothermal route", 《MATERIALS LETTERS》, vol. 65, 15 May 2011 (2011-05-15), pages 2518 - 2521 * |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104237349A (en) * | 2014-10-09 | 2014-12-24 | 无锡百灵传感技术有限公司 | Nano graphene and ferrous sulfide based electrochemical sensor |
| CN104465127A (en) * | 2014-11-22 | 2015-03-25 | 湖南科技大学 | Method for rapid preparation of grapheme/silver sulfide quantum dot nanocomposite and product |
| CN105958037A (en) * | 2016-07-08 | 2016-09-21 | 华东师范大学 | Copper sulphide/graphene composite material for negative electrode of sodium-ion battery and preparation method |
| CN105958037B (en) * | 2016-07-08 | 2019-05-17 | 华东师范大学 | Sodium-ion battery cathode copper sulfide/graphene composite material and preparation method |
| CN106972161A (en) * | 2017-04-05 | 2017-07-21 | 深圳市佩成科技有限责任公司 | A kind of preparation method of nitrogen-doped graphene/copper sulfide/hollow sulphur composite |
| WO2018184157A1 (en) * | 2017-04-05 | 2018-10-11 | 深圳市佩成科技有限责任公司 | Preparation method of composite material having nitrogen-doped graphene/copper sulfide/hollow sulfur particles |
| CN108597906A (en) * | 2018-06-13 | 2018-09-28 | 常熟理工学院 | A kind of preparation method of fiber/graphene/copper sulfide flexible electrode material |
| CN108597906B (en) * | 2018-06-13 | 2020-02-14 | 常熟理工学院 | Preparation method of fiber/graphene/copper sulfide flexible electrode material |
| CN109573997A (en) * | 2018-11-07 | 2019-04-05 | 江苏城乡建设职业学院 | A kind of preparation method of graphene oxide-loaded vulcanization carbon/carbon-copper composite material |
| CN109573997B (en) * | 2018-11-07 | 2022-04-19 | 江苏城乡建设职业学院 | Preparation method of graphene oxide loaded copper sulfide composite material |
| CN109607592A (en) * | 2018-12-13 | 2019-04-12 | 温州大学 | Transient metal sulfide/C-base composte material preparation method and applications of N doping |
| CN110085448A (en) * | 2019-05-17 | 2019-08-02 | 西北工业大学 | Copper sulfide with high-energy density/redox graphene composite material and preparation method |
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Application publication date: 20130807 |