CN103170647A - Method for forming copper nanometer sheet through self-assembly - Google Patents
Method for forming copper nanometer sheet through self-assembly Download PDFInfo
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- CN103170647A CN103170647A CN2013101158003A CN201310115800A CN103170647A CN 103170647 A CN103170647 A CN 103170647A CN 2013101158003 A CN2013101158003 A CN 2013101158003A CN 201310115800 A CN201310115800 A CN 201310115800A CN 103170647 A CN103170647 A CN 103170647A
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Abstract
The invention discloses a method for forming a copper nanometer sheet through self-assembly. According to the method, copper sulfate serves as a copper source, glucose serves as reducing agents, the glucose is effectively prevented from being carbonized under a high-temperature condition through adding of polyvinylpyrrolidone, and the copper nanometer sheet is successfully prepared through using of a hydrothermal method. According to the method, equipment is simple, technological parameters are controllable, repeatability is high, raw materials needed by preparation are abundant, cost is low, and no waste is generated. The copper nanometer sheet is widely applied to aspects of solid lubricant, catalytic agents, conducting materials and the like.
Description
Technical field
The invention belongs to the nano material preparing technical field, relate in particular to a kind of method that adopts hydro-thermal method to prepare the copper nanometer sheet.
Background technology
Copper nanoparticle is little due to size, specific area large, the Active sites number is many, resistance is little, have the characteristics such as quantum size effect and macro quanta tunnel effect, and some new features different from conventional material are arranged, and uses very extensive.Nanometer Copper is used as kollag, and being scattered in by rights becomes a kind of stable suspension in lubricating oil, combines with the surface of solids to form smooth protective layer, clogs simultaneously little cut, thereby reduces friction and wear.Copper nanoparticle has high activity and selectivity in the hydrogenation and dehydrogenation reaction of high molecular polymer, be a kind of good catalyst.Because copper nanoparticle has low resistance characteristic, can be used for making electrocondution slurry simultaneously, be widely used in the encapsulation in microelectronics industry.Connect etc., the miniaturization of microelectronic component is played an important role.
Along with the development of nanoscale science and technology, two-dimensional nanostructure material (nanometer sheet) in nano science, becomes study hotspot in the development of nanosecond science and technology and nano-device due to its special optics, magnetics, optical property and catalytic performance.Copper belongs to high symmetric face-centred cubic crystal structure, and the preparation of its two-dimensional nanostructure (nanometer sheet) is very difficult.At present, though the open source literature record of many copper nano material preparations is arranged, few about the preparation of two-dimentional copper nanometer sheet, technique and method that especially extensive self assembly forms the copper nanometer sheet have no open report.
Summary of the invention
The object of the invention is to overcome the defective of prior art, a kind of method that provides self assembly to form the copper nanometer sheet, the method cost is low, simple to operate, can form on a large scale two-dimentional copper nanometer sheet.
The objective of the invention is to be achieved through the following technical solutions: a kind of self assembly forms the method for copper nanometer sheet, and the method comprises the following steps:
(1) with the 25:0.5-1:0.2-1 mixing in mass ratio of water, glucose, polyvinylpyrrolidone, stir more than 3 hours, obtain clarifying mixed liquid;
(2) under the condition that stirs, drip copper sulfate solution in the mixed liquid of clarification in the step 1, in copper sulphate and step 1, the mol ratio of glucose is 1:2.5-5, after at room temperature stirring 30-60min, with light blue color contamination liquid, transfer in hydrothermal reaction kettle and react 2.5-4h under 160-200 ℃;
(3) product is centrifugal, obtain the copper nanometer sheet after using deionized water and absolute ethanol washing, vacuum drying successively.
The invention has the beneficial effects as follows: this method equipment is simple, and technological parameter is controlled, and is repeatable high.The preparation needed raw material is abundant, and cost is low, without generation of waste materials.The copper nanometer sheet of preparation has a wide range of applications at aspects such as kollag, catalyst, conductive materials.
Description of drawings
Fig. 1 is the SEM picture of the present invention's two dimension copper nanometer sheet;
Fig. 2 is the XRD picture of the present invention's two dimension copper nanometer sheet;
Fig. 3 is the EDS picture of the present invention's two dimension copper nanometer sheet;
Fig. 4 is the TEM picture of the present invention's two dimension copper nanometer sheet;
Fig. 5 is the SEM picture of the present invention's two dimension copper nanometer sheet self assembling process.
The specific embodiment
Below in conjunction with specific embodiment, further illustrate 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 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 limited range equally.
Self assembly of the present invention forms the method for copper nanometer sheet, comprises the following steps:
1, Jiang Shui, glucose, polyvinylpyrrolidone 25:0.5-1:0.2-1 mixing was in mass ratio stirred more than 3 hours, obtained clarifying mixed liquid.
In this step, glucose and polyvinylpyrrolidone need fully mix, when polyvinylpyrrolidone can make glucose play a role as reducing agent, can prevent again its under the pyroreaction condition by charing, form other impurity.
2, under the condition that stirs, drip copper sulfate solution in the mixed liquid of clarification in the step 1, in copper sulphate and step 1), the mol ratio of glucose is 1:2.5-5.After at room temperature stirring 30-60min, transfer in hydrothermal reaction kettle and react 2.5-4h under 160-200 ℃.
3, product is centrifugal, obtain the copper nanometer sheet after using deionized water and absolute ethanol washing, vacuum drying successively.
(1) 0.4g glucose, 0.15g polyvinylpyrrolidone are put into the clean beaker of a 50mL, add wherein the deionized water of 12.5mL, stir at ambient temperature 4h, obtain clarifying mixed liquid.
(2) in the situation that stir, the copper-bath that adds 0.8mmoL in the step (1), after fully stirring 1h, be transferred in hydrothermal reaction kettle and react 4h under 160 ℃, product is centrifugal, use successively deionized water, absolute ethanol washing three times, with products therefrom drying for standby in vacuum drying chamber.
The prepared copper nanometer sheet of the present invention pattern is seen scanned picture 1, and as can be seen from the figure, resulting self assembly copper nanometer sheet form homogeneous, regular is all the individual layer laminated structure.
Fig. 2 is the XRD picture of copper nanometer sheet of the present invention, and Fig. 3 is the EDS picture of copper nanometer sheet of the present invention, can find out from these two figure, and prepared copper nanometer sheet purity is fabulous, without the existence such as oxide of other copper.Fig. 4 is the electron diffraction diagram of choosing of copper nanometer sheet of the present invention, is the electron diffraction diagram in the lamella district of copper nanometer sheet in figure, and the large-scale lamella district that can find out that we see is corresponding to (111) face of copper.Fig. 5 is the SEM picture of copper nanometer sheet of the present invention self assembling process under different time, can clearly find out from figure, when reaction 55min, play initial action and have to copper nano particles, along with the increase in reaction time, copper nano particles begins to bond together, and begins to connect into tablet.When the reaction time was 1h35min, copper nano particles substantially all was connected to form nanometer sheet, but the nanometer sheet that forms surface utmost point out-of-flatness.Until after reaction 3h, copper nanometer sheet surface smoothing, the no concave-convex phenomenon exists, pattern homogeneous, regular.
Embodiment 2
(1) 0.5g glucose, 1g polyvinylpyrrolidone are put into the clean beaker of a 50mL, add wherein the deionized water of 25mL, stir at ambient temperature 5h, obtain clarifying mixed liquid.
(2) in the situation that stir, the copper-bath that adds 0.63mmoL in the step (1), after fully stirring 1h, be transferred in hydrothermal reaction kettle and react 3h under 180 ℃, product is centrifugal, use successively deionized water, absolute ethanol washing three times, with products therefrom drying for standby in vacuum drying chamber.
The resulting copper nanometer sheet of this embodiment pattern homogeneous, favorable dispersibility, the copper Nanosurface is smooth, regular, has good individual layer laminated structure.
Claims (1)
1. the method for a self assembly formation copper nanometer sheet, is characterized in that, the method comprises the following steps:
(1) with the 25:0.5-1:0.2-1 mixing in mass ratio of water, glucose, polyvinylpyrrolidone, stir more than 3 hours, obtain clarifying mixed liquid;
(2) under the condition that stirs, drip copper sulfate solution in the mixed liquid of clarification in the step 1, in copper sulphate and step 1, the mol ratio of glucose is 1:2.5-5, after at room temperature stirring 30-60min, transfers in hydrothermal reaction kettle and react 2.5-4h under 160-200 ℃;
(3) product is centrifugal, obtain the copper nanometer sheet after using deionized water and absolute ethanol washing, vacuum drying successively.
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| CN201310115800.3A CN103170647B (en) | 2013-04-03 | 2013-04-03 | Method for forming copper nanometer sheet through self-assembly |
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| CN201310115800.3A CN103170647B (en) | 2013-04-03 | 2013-04-03 | Method for forming copper nanometer sheet through self-assembly |
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| CN103170647A true CN103170647A (en) | 2013-06-26 |
| CN103170647B CN103170647B (en) | 2015-01-28 |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105127536A (en) * | 2015-09-09 | 2015-12-09 | 哈尔滨工业大学（威海） | Method for brazing titanium alloy through nano-copper solder |
| CN106363165A (en) * | 2016-09-05 | 2017-02-01 | 国核电力规划设计研究院 | Flaky copper particles, preparation method thereof, catalyst and electrode |
| CN106531966A (en) * | 2016-12-12 | 2017-03-22 | 北京科技大学 | Preparation method for nanometer Cu@CuO material and application of nanometer Cu@CuO material to lithium ion battery |
| CN106699550A (en) * | 2016-12-12 | 2017-05-24 | 北京科技大学 | Preparation method of nano Cu-CuBTC type metal organic framework material |
| CN108127125A (en) * | 2016-12-01 | 2018-06-08 | 中国科学院大连化学物理研究所 | A kind of preparation method of the copper nanometer sheet of high stability |
| CN108620601A (en) * | 2018-05-14 | 2018-10-09 | 哈尔滨理工大学 | A method of it is nanocrystalline to prepare sheet Cu under room temperature |
| CN110548880A (en) * | 2019-09-11 | 2019-12-10 | 南京牧科纳米科技有限公司 | Method and equipment for preparing metal nanosheets |
| CN110586953A (en) * | 2018-06-12 | 2019-12-20 | 本田技研工业株式会社 | High yield preparation of two-dimensional copper nanosheets |
| CN111659898A (en) * | 2019-03-08 | 2020-09-15 | 深圳先进技术研究院 | Preparation method of micro-nano copper sheet |
| CN112974831A (en) * | 2021-03-05 | 2021-06-18 | 西北有色金属研究院 | Cu-Cu with nano array structure3Preparation method of P material |
| CN113000855A (en) * | 2021-03-23 | 2021-06-22 | 中国科学技术大学先进技术研究院 | Preparation method of micro-nano copper powder |
| CN113996799A (en) * | 2021-10-08 | 2022-02-01 | 郑州工程技术学院 | Preparation method of copper nano material |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02294415A (en) * | 1989-05-10 | 1990-12-05 | Seidou Kagaku Kogyo Kk | Production of fine copper powder |
| CN1958197A (en) * | 2006-11-16 | 2007-05-09 | 中国科学院长春应用化学研究所 | Method for preparing Nano silver piece |
| CN1978096A (en) * | 2005-12-10 | 2007-06-13 | 中国科学院合肥物质科学研究院 | Gold-nano-piece having absorbing property to near-infrared ray and preparing method |
| CN102407343A (en) * | 2011-11-11 | 2012-04-11 | 华东师范大学 | Method for synthesizing copper nanoparticles |
| CN102728849A (en) * | 2012-05-08 | 2012-10-17 | 清华大学 | Self-supporting noble metal nanosheet with equal thickness of monatomic layer and preparation method of nanosheet |
-
2013
- 2013-04-03 CN CN201310115800.3A patent/CN103170647B/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02294415A (en) * | 1989-05-10 | 1990-12-05 | Seidou Kagaku Kogyo Kk | Production of fine copper powder |
| JP2728727B2 (en) * | 1989-05-10 | 1998-03-18 | 正同化学工業株式会社 | Method for producing fine copper powder |
| CN1978096A (en) * | 2005-12-10 | 2007-06-13 | 中国科学院合肥物质科学研究院 | Gold-nano-piece having absorbing property to near-infrared ray and preparing method |
| CN1958197A (en) * | 2006-11-16 | 2007-05-09 | 中国科学院长春应用化学研究所 | Method for preparing Nano silver piece |
| CN102407343A (en) * | 2011-11-11 | 2012-04-11 | 华东师范大学 | Method for synthesizing copper nanoparticles |
| CN102728849A (en) * | 2012-05-08 | 2012-10-17 | 清华大学 | Self-supporting noble metal nanosheet with equal thickness of monatomic layer and preparation method of nanosheet |
Cited By (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105127536A (en) * | 2015-09-09 | 2015-12-09 | 哈尔滨工业大学（威海） | Method for brazing titanium alloy through nano-copper solder |
| CN106363165A (en) * | 2016-09-05 | 2017-02-01 | 国核电力规划设计研究院 | Flaky copper particles, preparation method thereof, catalyst and electrode |
| CN108127125A (en) * | 2016-12-01 | 2018-06-08 | 中国科学院大连化学物理研究所 | A kind of preparation method of the copper nanometer sheet of high stability |
| CN108127125B (en) * | 2016-12-01 | 2020-01-14 | 中国科学院大连化学物理研究所 | Preparation method of high-stability copper nanosheet |
| CN106699550B (en) * | 2016-12-12 | 2020-05-12 | 北京科技大学 | Preparation method of nano Cu-CuBTC type metal organic framework material |
| CN106531966A (en) * | 2016-12-12 | 2017-03-22 | 北京科技大学 | Preparation method for nanometer Cu@CuO material and application of nanometer Cu@CuO material to lithium ion battery |
| CN106699550A (en) * | 2016-12-12 | 2017-05-24 | 北京科技大学 | Preparation method of nano Cu-CuBTC type metal organic framework material |
| CN106531966B (en) * | 2016-12-12 | 2019-06-11 | 北京科技大学 | Nanometer and its is applied Cu@CuO material preparation method in lithium ion battery |
| CN108620601A (en) * | 2018-05-14 | 2018-10-09 | 哈尔滨理工大学 | A method of it is nanocrystalline to prepare sheet Cu under room temperature |
| CN108620601B (en) * | 2018-05-14 | 2021-06-22 | 哈尔滨理工大学 | Method for preparing flaky Cu nanocrystalline at room temperature |
| CN110586953A (en) * | 2018-06-12 | 2019-12-20 | 本田技研工业株式会社 | High yield preparation of two-dimensional copper nanosheets |
| CN111659898A (en) * | 2019-03-08 | 2020-09-15 | 深圳先进技术研究院 | Preparation method of micro-nano copper sheet |
| CN110548880A (en) * | 2019-09-11 | 2019-12-10 | 南京牧科纳米科技有限公司 | Method and equipment for preparing metal nanosheets |
| CN112974831A (en) * | 2021-03-05 | 2021-06-18 | 西北有色金属研究院 | Cu-Cu with nano array structure3Preparation method of P material |
| CN112974831B (en) * | 2021-03-05 | 2022-04-19 | 西北有色金属研究院 | Cu-Cu with nano array structure3Preparation method of P material |
| CN113000855A (en) * | 2021-03-23 | 2021-06-22 | 中国科学技术大学先进技术研究院 | Preparation method of micro-nano copper powder |
| CN113000855B (en) * | 2021-03-23 | 2024-04-19 | 中国科学技术大学先进技术研究院 | Preparation method of micro-nano copper powder |
| CN113996799A (en) * | 2021-10-08 | 2022-02-01 | 郑州工程技术学院 | Preparation method of copper nano material |
| CN113996799B (en) * | 2021-10-08 | 2024-02-02 | 郑州工程技术学院 | Preparation method of copper nanomaterial |
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