CN104707997A - Preparation technology for copper/graphite core-shell structure - Google Patents
Preparation technology for copper/graphite core-shell structure Download PDFInfo
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- CN104707997A CN104707997A CN201310694221.9A CN201310694221A CN104707997A CN 104707997 A CN104707997 A CN 104707997A CN 201310694221 A CN201310694221 A CN 201310694221A CN 104707997 A CN104707997 A CN 104707997A
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Abstract
The invention discloses a preparation technology for a copper/graphite core-shell structure. According to the technical scheme, RF-PECVD equipment is adopted, a copper film prepared through DPS-III type ultrahigh vacuum facing-target magnetron sputtering is used as a copper source, and a copper/graphite core-shell structure (GS/CC) material is successfully prepared. The preparation technology has the advantages that the copper/graphite core-shell structure material is prepared through direct-current magnetron sputtering and radio frequency plasma enhanced chemical vapor deposition methods. The field emission performance of the material can be effectively improved as Cu particles are introduced, the field emission performance of grapheme can be effectively improved by modulating the morphology of the grapheme, and therefore the material has potential application in a field emission device. By using complementary advantages of graphite and copper, the copper/graphite core-shell structure (GS/CC) material is prepared, while cost is reduced, the field emission performance of the core-shell structure material is promoted substantially, and the material has potential application in the fields of the information technology, biomedical science, sensors and the like.
Description
Technical field
The invention discloses the preparation technology of a kind of copper/graphite nuclei shell structure.
Background technology
Nucleocapsid structure refer to kernel wrap up by other materials (i.e. shell).In general kernel has certain functional character, and shell has certain protection even strengthens the effect of core performance or can introduce new performance, and core-shell composite material can be the nanometer of zero to three-dimensional or the structural material of micron-scale.Nucleocapsid structure shows the physics more excellent than single component and chemical property usually, and the performance enhanced is mainly owing to the effect of shell, these advantages make nucleocapsid structure present potential using value in optics, magnetics, biology, catalysis, Conversion of Energy and storage etc.Although the application of nucleocapsid structure a lot, prepares novel nucleocapsid structure and the range of application widening nucleocapsid structure is still very important.The method preparing carbon element nucleocapsid structure is a lot, comprising: the methods such as carbon-arc discharge technology that is traditional and improvement, pyrolytic metallorganic, the high temperature anneal carbon-based material or metal precursor, blast or catalytic decomposition methane.But the nucleocapsid structure prepared by these methods is some noble metals (silver, platinum, gold) and magnetic metal (iron, cobalt, nickel) that graphite linings closely wraps up, and greatly limits its application.
In order to overcome the problems referred to above, the present invention designs the preparation technology of a kind of copper/graphite nuclei shell structure, and copper is that a kind of metal of cheapness but has fabulous electricity, light and heat character, can be widely used in the fields such as catalysis, electronics and photoelectronics.Therefore, by Optimization Technology, preparing with copper is the carbon element core-shell material of kernel, has bright prospects.
Summary of the invention
Object of the present invention is exactly the defect existed for prior art, invents the preparation technology of a kind of copper/graphite nuclei shell structure.Its technical scheme is the preparation technology of a kind of copper/graphite nuclei shell structure, it is characterized in that: adopt RF-PECVD equipment, the Copper thin film utilizing DPS-III type ultrahigh vacuum facing-target magnetron sputtering system to prepare is copper source, has successfully prepared copper/graphite nuclei shell structure (GS/CC) material.
The preparation of Copper thin film: adopt DPS-III type ultrahigh vacuum facing-target magnetron sputtering system plated film to arrange to prepare the Copper thin film that thickness is 120nm.The substrate used is single crystalline Si 100, the high purity copper target (purity is 99.95%) of target to be diameter be 6cm.By Si100 substrate respectively with putting on the sample stage of filming equipment after acetone, alcohol and deionized water ultrasonic cleaning 15min, when the background pressure of vacuum chamber is lower than 5 × 10
4after Pa, start at Si(100) upper depositing copper film, in deposition process, Ar throughput is 60sccm, and sputtering pressure is 0.5Pa, and sputtering current is 0.1A.
The preparation of copper/graphite Core-shell structure material: the Copper thin film prepared by facing-target magnetron sputtering system puts into the reative cell that radio frequency plasma strengthens chemical vapor depsotition equipment (RF-PECVD).After the pressure of reative cell is lower than 10Pa, pass into Ar gas (flow is 20sccm), and the gas pressure intensity keeping reative cell is 220Pa, start to heat up, after 40min, Copper thin film is warmed up to 800 DEG C and constant temperature 10min, now Copper thin film will be transformed into copper particle.Use RF-PECVD system to prepare GS/CC, Ar throughput is increased to 50sccm, passes into carbon-source gas-methane simultaneously, flow is 20sccm, when the gas pressure intensity of reative cell is stabilized in 800Pa, opens radio-frequency power supply, and radio-frequency power is adjusted to 200W, start deposition preparation GS/CC.Sedimentation time 15min.After deposition terminates, close methane, make reative cell Temperature fall under an ar atmosphere.
Feature of the present invention is: carbon nanomaterial is considered to extraordinary field emmision material, this is because carbon nanomaterial has the excellent character such as high specific area, good mechanical strength and high electron conductivity.Promote electron emission because CNT pointed end can form the electric field of local, thus make the research in field emission performance of CNT and composite thereof widely.But the Joule heat that higher emission current produces can cause the distortion on CNT top, and then the launch stability of CNT is caused to be deteriorated.The graphene nanometer sheet (GNS) of vertical growth is the field emmision material of new generation with development prospect, it grows along two-dimensional directional, there is the specific area larger than CNT, improve area of dissipation, thus avoid the destruction of Joule heat to field emmision material.Generally, the local electric field on reinforcing material surface can improve the electron tunneling probability on surface, but, the distribution density of graphene nanometer sheet also can hinder the enhancing of local electric field, the larger Electric field shielding effect of density is stronger, visible, for graphene nanometer sheet, the field emission performance that reduction Electric field shielding effect (namely strengthening local electric field) improves material is very important.But copper has good electric conductivity, good thermal conductivity, good thermodynamic stability and lower resistance temperature system, can make up this shortcoming.The method that the present invention strengthens chemical vapour deposition (CVD) by magnetically controlled DC sputtering and radio frequency plasma has prepared copper/graphite Core-shell structure material.The introducing of Cu particle can improve the field emission performance of material effectively, by modulating the pattern of Graphene, effectively can improve the field emission performance of Graphene, making it in feds, have potential application.The present invention utilizes graphite and copper feature to have complementary advantages, prepare copper/graphite nuclei shell structure (GS/CC) material, significantly promote the field emission performance of Core-shell structure material while reducing costs, in information technology, biomedicine and sensor field, there is potential application.
Detailed description of the invention
A preparation technology for copper/graphite nuclei shell structure, is characterized in that: adopt RF-PECVD equipment, the Copper thin film utilizing DPS-III type ultrahigh vacuum facing-target magnetron sputtering system to prepare is copper source, has successfully prepared copper/graphite nuclei shell structure (GS/CC) material.
The preparation of Copper thin film: adopt DPS-III type ultrahigh vacuum facing-target magnetron sputtering system plated film to arrange to prepare the Copper thin film that thickness is 120nm.The substrate used is single crystalline Si 100, the high purity copper target (purity is 99.95%) of target to be diameter be 6cm.By Si(100) substrate respectively with putting on the sample stage of filming equipment after acetone, alcohol and deionized water ultrasonic cleaning 15min, when the background pressure of vacuum chamber is lower than 5 × 10
4after Pa, start depositing copper film on Si100, in deposition process, Ar throughput is 60sccm, and sputtering pressure is 0.5Pa, and sputtering current is 0.1A.
The preparation of copper/graphite Core-shell structure material: the Copper thin film prepared by facing-target magnetron sputtering system puts into the reative cell that radio frequency plasma strengthens chemical vapor depsotition equipment (RF-PECVD).After the pressure of reative cell is lower than 10Pa, pass into Ar gas (flow is 20sccm), and the gas pressure intensity keeping reative cell is 220Pa, start to heat up, after 40min, Copper thin film is warmed up to 800 DEG C and constant temperature 10min, now Copper thin film will be transformed into copper particle.When using RF-PECVD system to prepare GS/CC, Ar throughput is increased to 50sccm, passes into carbon-source gas-methane simultaneously, flow is 20sccm, when the gas pressure intensity of reative cell is stabilized in 800Pa, opens radio-frequency power supply, and radio-frequency power is adjusted to 200W, start deposition preparation GS/CC.Sedimentation time 15min.After deposition terminates, close methane, make reative cell Temperature fall under an ar atmosphere.
Claims (4)
1. a preparation technology for copper/graphite nuclei shell structure, is characterized in that: adopt RF-PECVD equipment, the Copper thin film utilizing DPS-III type ultrahigh vacuum facing-target magnetron sputtering system to prepare is copper source, has successfully prepared copper/graphite nuclei shell structure (GS/CC) material.
2. the preparation technology of a kind of copper/graphite nuclei shell structure according to claim 1, it is characterized in that: the preparation of Copper thin film: adopt DPS-III type ultrahigh vacuum facing-target magnetron sputtering system plated film to arrange to prepare the Copper thin film that thickness is 120nm, the substrate used is single crystalline Si 100, the high purity copper target (purity is 99.95%) of target to be diameter be 6cm.By Si(100) substrate respectively with putting on the sample stage of filming equipment after acetone, alcohol and deionized water ultrasonic cleaning 15min, when the background pressure of vacuum chamber is lower than 5 × 10
4after Pa, start at Si(100) upper depositing copper film, in deposition process, Ar throughput is 60sccm, and sputtering pressure is 0.5Pa, and sputtering current is 0.1A.。
3. the preparation technology of a kind of copper/graphite nuclei shell structure according to claim 1, it is characterized in that: the preparation of copper/graphite Core-shell structure material: the Copper thin film prepared by facing-target magnetron sputtering system puts into the reative cell that radio frequency plasma strengthens chemical vapor depsotition equipment (RF-PECVD), after the pressure of reative cell is lower than 10Pa, pass into Ar gas (flow is 20sccm), and keep the gas pressure intensity of reative cell to be 220Pa, start to heat up, after 40min, Copper thin film is warmed up to 800 DEG C and constant temperature 10min, now Copper thin film will be transformed into copper particle.
4. the preparation technology of a kind of copper/graphite nuclei shell structure according to claim 1, it is characterized in that: when using RF-PECVD system to prepare GS/CC, Ar throughput is increased to 50sccm, pass into carbon-source gas-methane simultaneously, flow is 20sccm, when the gas pressure intensity of reative cell is stabilized in 800Pa, opens radio-frequency power supply, and radio-frequency power is adjusted to 200W, start deposition preparation GS/CC.Sedimentation time 15min.After deposition terminates, close methane, make reative cell Temperature fall under an ar atmosphere.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106521455A (en) * | 2016-09-21 | 2017-03-22 | 见嘉环境科技（苏州）有限公司 | Preparation method for copper nanoparticles wrapped with single-layer graphene and grown on porous carbon material |
| CN107697906A (en) * | 2017-08-21 | 2018-02-16 | 上海理工大学 | A kind of preparation method of copper/graphene composite material |
| CN107875456A (en) * | 2016-09-29 | 2018-04-06 | 北京大学 | Copper-based biomaterial of graphene coated and preparation method and application |
| CN108788134A (en) * | 2018-06-05 | 2018-11-13 | 上海利物盛企业集团有限公司 | A kind of preparation method of graphene-nanometer pltine core-shell structural conductive material |
| CN108929745A (en) * | 2018-08-17 | 2018-12-04 | 深圳南科新材科技有限公司 | A kind of anti-wear additive, preparation method, purposes and the lubricating oil containing it |
| CN109107500A (en) * | 2018-10-15 | 2019-01-01 | 盐城师范学院 | A kind of preparation method of copper/graphene core-shell structure |
| CN113838725A (en) * | 2021-09-03 | 2021-12-24 | 深圳先进技术研究院 | Graphene field emission cathode and preparation method thereof |
| CN115401363A (en) * | 2022-08-19 | 2022-11-29 | 重庆平创半导体研究院有限责任公司 | Device and method for preparing flaky core-shell structure and low-temperature sintering soldering paste |
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2013
- 2013-12-17 CN CN201310694221.9A patent/CN104707997A/en active Pending
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106521455A (en) * | 2016-09-21 | 2017-03-22 | 见嘉环境科技（苏州）有限公司 | Preparation method for copper nanoparticles wrapped with single-layer graphene and grown on porous carbon material |
| CN107875456A (en) * | 2016-09-29 | 2018-04-06 | 北京大学 | Copper-based biomaterial of graphene coated and preparation method and application |
| CN107697906A (en) * | 2017-08-21 | 2018-02-16 | 上海理工大学 | A kind of preparation method of copper/graphene composite material |
| CN108788134A (en) * | 2018-06-05 | 2018-11-13 | 上海利物盛企业集团有限公司 | A kind of preparation method of graphene-nanometer pltine core-shell structural conductive material |
| CN108929745A (en) * | 2018-08-17 | 2018-12-04 | 深圳南科新材科技有限公司 | A kind of anti-wear additive, preparation method, purposes and the lubricating oil containing it |
| CN109107500A (en) * | 2018-10-15 | 2019-01-01 | 盐城师范学院 | A kind of preparation method of copper/graphene core-shell structure |
| CN109107500B (en) * | 2018-10-15 | 2021-06-04 | 盐城师范学院 | Preparation method of copper/graphene core-shell structure |
| CN113838725A (en) * | 2021-09-03 | 2021-12-24 | 深圳先进技术研究院 | Graphene field emission cathode and preparation method thereof |
| CN115401363A (en) * | 2022-08-19 | 2022-11-29 | 重庆平创半导体研究院有限责任公司 | Device and method for preparing flaky core-shell structure and low-temperature sintering soldering paste |
| CN115401363B (en) * | 2022-08-19 | 2023-11-03 | 重庆平创半导体研究院有限责任公司 | Device and method for preparing flaky core-shell structure and low-temperature sintering soldering paste |
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Application publication date: 20150617 |