CN106191802A - The preparation method that selective growth vertical graphite is dilute - Google Patents
The preparation method that selective growth vertical graphite is dilute Download PDFInfo
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- CN106191802A CN106191802A CN201610540870.7A CN201610540870A CN106191802A CN 106191802 A CN106191802 A CN 106191802A CN 201610540870 A CN201610540870 A CN 201610540870A CN 106191802 A CN106191802 A CN 106191802A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/04—Coating on selected surface areas, e.g. using masks
- C23C16/042—Coating on selected surface areas, e.g. using masks using masks
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/02—Pretreatment of the material to be coated
- C23C16/0209—Pretreatment of the material to be coated by heating
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/26—Deposition of carbon only
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/50—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges
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Abstract
The invention discloses the preparation method that a kind of selective growth vertical graphite is dilute.The preparation method that selective growth vertical graphite is dilute, comprises the following steps: the substrate providing any one or more in metal mask plate and iron content, cobalt or nickel to combine, and is placed on substrate by metal mask plate;Substrate with metal mask plate is inserted physics vapour deposition system deposition shielding layer;Take off metal mask plate, form the substrate being coated with graphical shielding layer;Then exist > 800 DEG C anneal containing in the environment of hydrogen;Then insert plasma-assisted chemical vapour deposition system to grow, and be passed through the gas of hydrogen, argon and carbon elements.The preparation method processing step that selective growth vertical graphite of the present invention is dilute is few, simple to operation, escapable cost.
Description
Technical field
The present invention relates to technical field prepared by Graphene, particularly relate to the system that a kind of selective growth vertical graphite is dilute
Preparation Method.
Background technology
Graphene (Graphene) is by a kind of carbonaceous of monolayer carbon atom tightly packed one-tenth bi-dimensional cellular shape lattice structure
New material.The scientist Geim A of Univ Manchester UK in 2004 is peeled off by micromechanics stripping method and observes monolayer carbon
The existence of atomic plane structure, i.e. Graphene, broken two-dimension single layer atomic crystal structure can not individualism thermodynamics pass
Overall view is read, and causes the whole world research boom to grapheme material.Two dimensional crystal structure due to its uniqueness so that it is at electricity
Learn, the aspect such as calorifics and mechanics shows the physical property of some novelties, it is expected to High-performance micro-nano electronic device, field emmision material,
The field such as composite, gas sensor and energy storage obtains extensively application, be after fullerene and CNT another
Landmark new carbon.
And wherein vertical graphite alkene material has the sharp edges of atomic layer level thickness, cause it and there is excellent electronic field emission
Characteristic, therefore it has vast application prospect in nanometer field electron transmitting device.In emission electronic device designs, focus on electricity
The distribution of field can determine that the effect that field emission electron bundle focuses on, burnt therefore the size of cathodic field emissive material and figure are necessary for and gather
Burnt Electric Field Characteristics is optimized, and can be only achieved optimum efficiency.But, vertical graphite alkene material is different from other thin-film material, its
Lamellar vertical structure is difficult to lithography process and etching, it is achieved patterned difficulty greatly improves.
Summary of the invention
The technical problem to be solved in the present invention be to provide a kind of can the dilute system of patterned selective growth vertical graphite
Preparation Method.
For solving the problems referred to above, the present invention provides the preparation method that a kind of selective growth vertical graphite is dilute, including following
Step:
A. the substrate that any one or more in metal mask plate and iron content, cobalt or nickel combines is provided, by metal mask
Plate is placed on substrate;
B. the substrate with metal mask plate is inserted physics vapour deposition system deposition shielding layer;
C. take off metal mask plate, form the substrate being coated with graphical shielding layer;
The most then exist > 800 DEG C anneal containing in the environment of hydrogen;
The most then insert plasma-assisted chemical vapour deposition system to grow, and be passed through hydrogen, argon and carbon containing unit
The gas of element.
Further, described shielding layer thickness at least 10 nanometer.
Further, described shielding layer can be metal, metal-oxide or non-metal nitride.
Further, annealing time at least 10 minutes.
Further, growth time at least 5 minutes.
Further, it is passed through hydrogen, argon and carbon containing unit in growth course plasma enhanced chemical vapor deposition system
Element gas.
Further, after having grown, lower the temperature.
Further, argon or nitrogen is utilized to lower the temperature.
Further, described physics vapour deposition system is deposition system or sputter system.
The preparation method that selective growth vertical graphite of the present invention is dilute, utilizes mask plate to be patterned shielding layer, so
After on the substrate with graphical shielding layer, carry out Graphene vertically grow, the most optionally carry out the life of Graphene
Long.Only need to carry out once graphical, technique is simple, it is easy to operation.
Accompanying drawing explanation
Fig. 1 is the schematic diagram that metal mask plate is positioned on the substrate containing metal.
Fig. 2 is the substrat structure schematic diagram that Fig. 1 deposits shielding layer.
Fig. 3 is the structural representation after Fig. 2 takes off metal mask plate.
Fig. 4 is that carbon atom is dissolved in metal substrate schematic diagram
Fig. 5 is that on patterned substrate, vertically growth has the schematic diagram of Graphene.
Fig. 6 is vertical growth Graphene scanning electron microscope (SEM) photograph.
Detailed description of the invention
The invention will be further described below in conjunction with the accompanying drawings.
The most as shown in Figures 1 to 6, the preparation method better embodiment that selective growth vertical graphite of the present invention is dilute includes
Following steps,
First, it is provided that metal mask plate 2 and the substrate 1 comprising nickel, such as dilval or thin film.Metal mask plate 2 is put
In the surface of substrate 1, described metal mask plate 2 is placed on the position of Graphene 5 growth.In other embodiments, substrate 1 is also
Can be made up of ferrum, cobalt or nickel, it is also possible to be to make containing a kind of alloy or thin film, it is also possible to be only to kill two of which
Alloy or thin film make.
Then by the substrate 1 with metal mask plate 2, put into physics vapour deposition system and carry out depositing shielding layer 3;Described
Physics vapour deposition system is deposition system or sputter system;Described shielding layer 3 can be metal (such as Cu, W, Ti, Ta etc.), metal
Oxide (such as titanium oxide, tantalum oxide, hafnium oxide, lanthana etc.), nonmetal oxide (such as silicon oxide etc.) or nonmetal nitridation
Thing (such as silicon nitride etc.);Thickness at least 10 nanometer of described shielding layer 3, it is ensured that shielding layer 3 can effectively block carbon atom.
After shielding layer 3 reaches preset thickness, take off metal mask plate 2, thus form the lining being coated with graphical shielding layer 3
The end 1.
Then the substrate 1 after graphical is existed > 800 DEG C anneal containing in the environment of hydrogen, argon or nitrogen;Annealing
At least 10 minutes time, it is ensured that enough annealing times.
After having annealed, patterned substrate 1 is inserted plasma-assisted chemical vapour deposition system and grows;Growth
At least 5 minutes time, it is ensured that vertical Graphene 5 can be grown;Plasma enhanced chemical vapor deposition is given in growth course
System is passed through the gas of hydrogen, argon and carbon elements, and the gas of described carbon elements is methane, ethane or acetylene etc..Due to
Carbon atom is far below the solid solubility containing nickel substrate 1, so carbon is at shielding layer 3 in the solid solubility of shielding layer 3
Beneath concentration is relatively low.The dilute structure of vertical graphite, according to patterned shielding layer 3, is selected on the substrate 1 that partial denudation goes out
Selecting property grows.
After having grown, utilize argon or nitrogen, it is possible to be that the mixed gas of two kinds of gases is lowered the temperature.To Graphene 5
Cooling can prevent Graphene oxidized.Use gas that Graphene 5 is lowered the temperature, it is possible to decrease cost.
By the position one layer of shielding layer 3 of deposition without growing Graphene 5, only shielding layer 3 need to be carried out once graphical,
Can the most optionally grow Graphene 5.Technique is simple, easy to operate, moreover it is possible to reduce cost.
These are only embodiments of the present invention, not thereby limit the scope of the claims of the present invention, every utilize the present invention
The equivalent structure that description and accompanying drawing content are made, is directly or indirectly used in other relevant technical fields, the most in like manner at this
Within the scope of patent protection of invention.
Claims (9)
1. the preparation method that a selective growth vertical graphite is dilute, it is characterised in that: comprise the following steps:
A. the substrate providing any one or more in metal mask plate and iron content, cobalt or nickel to combine, puts metal mask plate
On substrate;
B. the substrate with metal mask plate is inserted physics vapour deposition system deposition shielding layer;
C. take off metal mask plate, form the substrate being coated with graphical shielding layer;
The most then exist > 800 DEG C anneal containing in the environment of hydrogen;
The most then insert plasma-assisted chemical vapour deposition system to grow, and be passed through hydrogen, argon and carbon elements
Gas.
2. the preparation method that selective growth vertical graphite as claimed in claim 1 is dilute, it is characterised in that cover thickness described in:
Degree at least 10 nanometers.
3. the preparation method that selective growth vertical graphite as claimed in claim 1 is dilute, it is characterised in that: described shielding layer can
For metal, metal-oxide, nonmetal oxide or non-metal nitride.
4. the preparation method that selective growth vertical graphite as claimed in claim 1 is dilute, it is characterised in that: annealing time is at least
10 minutes.
5. the preparation method that selective growth vertical graphite as claimed in claim 1 is dilute, it is characterised in that: growth time is at least
5 minutes.
6. the preparation method that selective growth vertical graphite as claimed in claim 1 is dilute, it is characterised in that: described carbon elements
Gas is methane, ethane or acetylene.
7. the preparation method that selective growth vertical graphite as claimed in claim 1 is dilute, it is characterised in that: after having grown,
Lower the temperature.
8. the preparation method that selective growth vertical graphite as claimed in claim 7 is dilute, it is characterised in that: utilize argon and/
Or nitrogen lowers the temperature.
9. the preparation method that selective growth vertical graphite as claimed in claim 1 is dilute, it is characterised in that: described physical vapor
Depositing system is deposition system or sputter system.
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Cited By (4)
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CN111293013A (en) * | 2020-03-27 | 2020-06-16 | 中山大学 | Field emission cold cathode structure and manufacturing method thereof |
CN113213460A (en) * | 2021-05-08 | 2021-08-06 | 北京工业大学 | Method for graphically growing vertically-oriented graphene |
CN113990723A (en) * | 2021-09-26 | 2022-01-28 | 杭州电子科技大学 | Preparation method of arrayed vertical graphene field emission cold cathode |
CN114772584A (en) * | 2022-03-23 | 2022-07-22 | 重庆大学 | Patterned vertical graphene and preparation method thereof |
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US20130143000A1 (en) * | 2011-12-05 | 2013-06-06 | Egypt Nanotechnology Center (Egnc) | Forming Patterned Graphene Layers |
CN103151245A (en) * | 2013-03-28 | 2013-06-12 | 中国科学院上海微系统与信息技术研究所 | Thin film patterning method |
CN103280404A (en) * | 2013-05-17 | 2013-09-04 | 中国科学院上海微系统与信息技术研究所 | Patterned preparation method of field emission electrode on basis of vertical graphene |
CN104217930A (en) * | 2013-06-05 | 2014-12-17 | 中芯国际集成电路制造(上海)有限公司 | Method for forming graphene patterns |
CN105110324A (en) * | 2015-08-18 | 2015-12-02 | 中国科学院上海微系统与信息技术研究所 | Method for preparing wrinkle-free graphene |
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Patent Citations (5)
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US20130143000A1 (en) * | 2011-12-05 | 2013-06-06 | Egypt Nanotechnology Center (Egnc) | Forming Patterned Graphene Layers |
CN103151245A (en) * | 2013-03-28 | 2013-06-12 | 中国科学院上海微系统与信息技术研究所 | Thin film patterning method |
CN103280404A (en) * | 2013-05-17 | 2013-09-04 | 中国科学院上海微系统与信息技术研究所 | Patterned preparation method of field emission electrode on basis of vertical graphene |
CN104217930A (en) * | 2013-06-05 | 2014-12-17 | 中芯国际集成电路制造(上海)有限公司 | Method for forming graphene patterns |
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
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CN111293013A (en) * | 2020-03-27 | 2020-06-16 | 中山大学 | Field emission cold cathode structure and manufacturing method thereof |
CN113213460A (en) * | 2021-05-08 | 2021-08-06 | 北京工业大学 | Method for graphically growing vertically-oriented graphene |
CN113990723A (en) * | 2021-09-26 | 2022-01-28 | 杭州电子科技大学 | Preparation method of arrayed vertical graphene field emission cold cathode |
CN113990723B (en) * | 2021-09-26 | 2023-10-03 | 杭州电子科技大学 | Preparation method of arrayed vertical graphene field emission cold cathode |
CN114772584A (en) * | 2022-03-23 | 2022-07-22 | 重庆大学 | Patterned vertical graphene and preparation method thereof |
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Address after: 401329 Fengsheng Road, Jiulongpo District, Chongqing Applicant after: Chongqing Qiyue Yongyang Microelectronic Technology Development Co., Ltd. Address before: 401332 No. 1 Building, 5th Floor, No. 98 Xiyuan Second Road, Shapingba District, Chongqing Applicant before: Chongqing Qiyue Yongyang Microelectronic Technology Development Co., Ltd. |
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Application publication date: 20161207 |