CN203593622U - Device for preparing graphene on silicon carbide substrate - Google Patents
Device for preparing graphene on silicon carbide substrate Download PDFInfo
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- CN203593622U CN203593622U CN201320664729.XU CN201320664729U CN203593622U CN 203593622 U CN203593622 U CN 203593622U CN 201320664729 U CN201320664729 U CN 201320664729U CN 203593622 U CN203593622 U CN 203593622U
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Abstract
The utility model belongs to the technical field of new materials, and particularly relates to a device for preparing graphene on a silicon carbide substrate through high-temperature annealing. The device comprises a quartz heating cavity and a graphite barrel which can be placed in the quartz heating cavity; during use, the graphite barrel can be placed in the cavity, and can be heated in a conventional radio-frequency heating manner to produce graphene; the quartz heating cavity comprises a cavity with an upper opening and a top cap; a hollow sandwich and a thermal insulation layer are arranged in the cavity; a thermal insulation layer groove is formed in the middle of the thermal insulation layer; the graphite barrel comprises a barrel body with an opening in the upper end; a groove is formed in the upper surface of the bottom of the barrel body; positioning blocks are arranged on the side wall of the upper part of the graphite barrel; a heat reflecting screen is placed on the positioning blocks. According to the device with the structure, the heating is uniform, the efficiency is high, and the heat loss is less; as the device is used for preparing the graphene on the silicon carbide substrate through high-temperature annealing, the purity of the graphene is improved, the preparing cost is reduced, and the preparing efficiency is improved.
Description
Technical field
The utility model belongs to novel material processing technique field, is specifically related to a kind of device of preparing Graphene, particularly a kind of device that utilizes high temperature annealing to prepare Graphene in silicon carbide substrates.
Background technology
Graphene is a kind of carbonaceous novel material by the tightly packed one-tenth of carbon atom, there is individual layer bi-dimensional cellular shape (only including hexagonal primitive unit cell) crystalline network, only has the thickness (～0.35nm) of an atom, its structural stability is very high, and connection between each carbon atom is quite pliable and tough, in the time being subject to external force and attacking, will distorted deformation, make carbon atom needn't rearrange to adapt to external force, thereby guaranteed the stability of self structure.
As simple substance, Graphene has the performance of many excellences, the characteristic of its maximum be exactly the movement velocity of its electronics be one of three percentages of the light velocity, be that in current known materials, electronic conduction speed is the fastest, be the twice of indium antimonide material (the at present known material with high mobility).Although Graphene only has the thickness of an atom, intensity is very high, and maximum intensity reaches 130GPa, is more than 100 times of steel.Graphene also has a series of special propertys such as half-integer quantum hall effect under room temperature, tunnel effect, permanent electric conductivity.
At present successful development goes out the multiple method of preparing Graphene, as: adhesive tape micromechanics stripping method, chemical reagent intercalation peel off under expansion graphite method, transiting metal surface high temperature, infiltrate carbon atom then fast cooling segregation go out chemical vapour deposition (CVD) method, the graphite oxide reduction method etc. of Graphene.Graphene prepared by first two method all needs to be transferred in insulating substrate, the third method utilize in the metallic surface of copper or nickel chemical Vapor deposition process can prepare large-area graphene film and quality pretty good, but the controllability of the graphene film thickness that this method obtains is poor.Although graphite oxide reduction method can obtain larger area graphene film, because the Graphene in preparation process has been introduced a large amount of defects, and monolithic Graphene size is less, causes the graphene film that obtains discontinuous, and its electroconductibility also has much room for improvement.
In order to overcome the deficiency of above-mentioned preparation technology's existence, need to research and develop a kind of preparation method and equipment of new Graphene.
Summary of the invention
For the weak point of existing Graphene preparation technology and equipment existence, contriver of the present utility model provides a kind of device that utilizes high temperature annealing to prepare Graphene in silicon carbide substrates, this device comprises quartz heating chamber and can be placed on the graphite bucket in heating chamber, when use, graphite bucket can be placed in cavity, utilize conventional RF heating to add hot preparation Graphene to it, wherein there is upper shed cavity and the top cover of hollow sandwich in quartz heating chamber in comprising, in cavity, be provided with thermal insulation layer, thermal insulation layer middle part is thermal insulation layer groove; The graphite bucket adopting comprises the staving of upper end open, and staving upper base surface is provided with groove, in graphite bucket upper portion side wall, is provided with preset pieces, is placed with heat reflection screen on preset pieces; Adopt the device of this structure, when use, only silicon carbide substrates need be inserted in graphite chime, again graphite bucket is inserted in the thermal insulation layer groove of quartz heating chamber, just can utilize conventional radio frequency heating apparatus to heat the silicon carbide substrates in cavity, homogeneous heating and efficiency are high, and heat loss is few, utilize high temperature annealing in silicon carbide substrates, to prepare Graphene by it, improve the purity of Graphene, saved production cost, improved production efficiency.
Concrete technical scheme of the present utility model is:
Utilize high temperature annealing in silicon carbide substrates, to prepare a device for Graphene, this device comprises quartz heating chamber and can be placed on the graphite bucket in heating chamber;
Wherein said quartz heating chamber, in comprising, there are upper shed cavity and the top cover of hollow sandwich, on top cover, be provided with thermometric window and inlet mouth, cavity bottom is provided with thermometric window and air outlet, cavity one side roof part is provided with the cooling water outlet with hollow sandwich UNICOM, cavity opposite side bottom is provided with the entrance of cooling water with hollow sandwich UNICOM, in cavity, be provided with thermal insulation layer, thermal insulation layer middle part is thermal insulation layer groove, and the thermometric window of cavity bottom setting runs through thermal insulation layer and is connected with thermal insulation layer groove;
Described graphite bucket comprises the staving of upper end open, and staving upper base surface is provided with groove, in graphite bucket upper portion side wall, is provided with at least two preset piecess, is placed with heat reflection screen on preset pieces.
Adopt the quartz heating chamber of this structure, when use, graphite bucket directly can be placed on by the opening of cavity upper end in the thermal insulation layer groove at thermal insulation layer middle part, afterwards top cover is covered and make to become airtight space in cavity, be convenient to vacuumize or pass in later stage preparation process rare gas element; Just can in the hollow sandwich in cavity, add water coolant by entrance of cooling water afterwards, the temperature of quartz cavity itself while reducing heating, in order to avoid cavity impaired and overheated after be difficult to pick and place; Can pass into rare gas element by the inlet mouth on top cover, or seal this inlet mouth and directly utilize the air outlet of cavity bottom setting to vacuumizing in cavity, to reach the requirement of reaction; When use, this cavity is placed directly in radio frequency heating coil and goes to heat the graphite bucket in cavity, in heat-processed, can be by the thermometric window on top cover by the temperature in Instrument measuring cavity, the thermometric window that also can arrange by cavity bottom is directly measured the namely real time temperature of graphite bucket of temperature of thermal insulation layer groove, thereby better grasp the temperature distribution in whole cavity, adjust in real time the intensity of radio frequency heating, better control the temperature of reaction;
And adopt the graphite bucket of this structure, the groove of staving upper base surface setting can be fixed on silicon carbide substrates portion's upper surface and guarantee can not produce in whole production process displacement, can utilize afterwards external heat source to heat, utilize the thermal conductivity of graphite to heat silicon carbide substrates; In graphite bucket upper portion side wall, be provided with at least two preset piecess, on preset pieces, can place heat reflection screen, like this in heat-processed, the heat reflection screen arranging can return the reflect heat of stroll staving bottom, guarantee that heat does not does not scatter and disappear, and the temperature field that utilizes heat reflection screen to obtain is more even, particularly can keeps SiC substrate surface temperature field evenly, improve the temperature in crystal vessel, be convenient to the preparation of Graphene;
In order to reach better effect, staving upper base surface is provided with tantalum carbide coating, utilizes this coating can prevent that SiC substrate lower surface from high temperature reacting with graphite;
The heat reflection screen adopting, its material is the refractory metal materials such as rhenium, tungsten, tantalum, generally be prepared into thin plate according to the shape of graphite bucket with size, and guarantee that the surface of thin plate is minute surface, can play like this effect of good reflecting heat and homogenize temperature field.
In sum, adopt the device of this structure, can utilize conventional radio frequency heating apparatus to heat the silicon carbide substrates in cavity, homogeneous heating and efficiency are high, heat loss is few, utilizes high temperature annealing in silicon carbide substrates, to prepare Graphene by it, has improved the purity of Graphene, save production cost, improved production efficiency.
Accompanying drawing explanation
Fig. 1 is the structural representation in quartz heating described in the utility model chamber;
Fig. 2 is the vertical view in quartz heating described in the utility model chamber;
Fig. 3 is the sectional view of A-A in Fig. 2;
Fig. 4 is the structural representation of graphite bucket described in the utility model;
Fig. 5 is the vertical view of graphite bucket described in the utility model;
Fig. 6 is the sectional view of A-A in Fig. 5;
Fig. 7 is the structure sectional view of the device of preparing Graphene described in the utility model;
In figure, 1 is cavity, and 2 is inlet mouth, and 3 is thermometric window, and 4 is cooling water outlet, and 5 is air outlet, 6 is entrance of cooling water, and 7 is thermal insulation layer, and 8 is thermal insulation layer groove, and 9 is top cover, and 10 is staving, 11 is groove, and 12 is preset pieces, and 13 is heat reflection screen, and 14 is radio frequency heating coil.
Embodiment
Utilize high temperature annealing in silicon carbide substrates, to prepare a device for Graphene, this device comprises quartz heating chamber and can be placed on the graphite bucket in heating chamber;
Wherein said quartz heating chamber, in comprising, there are upper shed cavity 1 and the top cover 9 of hollow sandwich, on top cover 9, be provided with thermometric window 3 and inlet mouth 2, cavity bottom is provided with thermometric window 3 and air outlet 5, cavity 1 one side roof parts are provided with the cooling water outlet 4 with hollow sandwich UNICOM, cavity 1 opposite side bottom is provided with the entrance of cooling water 6 with hollow sandwich UNICOM, in cavity 1, be provided with thermal insulation layer 7, thermal insulation layer 7 middle parts are thermal insulation layer groove 8, and the thermometric window 3 of cavity bottom setting runs through thermal insulation layer 7 and is connected with thermal insulation layer groove 8.
Described graphite bucket, this graphite bucket comprises the staving 10 of upper end open, staving 10 upper base surface are provided with groove 11, in graphite bucket upper portion side wall, are provided with at least two preset piecess 12, are placed with heat reflection screen 13 on preset pieces 12;
Staving upper base surface is provided with tantalum carbide coating;
The heat reflection screen adopting, its material is the refractory metal materials such as rhenium, tungsten, tantalum, is generally prepared into thin plate according to the shape of graphite bucket and size, and guarantees that the surface of thin plate is minute surface.
When use, silicon carbide substrates is fixed in the groove of staving upper base surface, guarantees can not produce displacement in whole production process, heat reflection screen is placed on preset pieces; Afterwards graphite bucket is directly placed in the thermal insulation layer groove at thermal insulation layer middle part by the opening of cavity upper end, then top cover is covered and makes to become airtight space in cavity, be convenient to vacuumize or pass in later stage preparation process rare gas element; Just can in the hollow sandwich in cavity, add water coolant by entrance of cooling water afterwards, the temperature of quartz cavity itself while reducing heating, in order to avoid cavity impaired and overheated after be difficult to pick and place; Can pass into rare gas element by the inlet mouth on top cover, or seal this inlet mouth and directly utilize the air outlet of cavity bottom setting to vacuumizing in cavity, to reach the requirement of reaction; When use, this cavity is placed directly in radio frequency heating coil 14 and goes to heat the graphite bucket in cavity.
Claims (5)
1. in silicon carbide substrates, prepare a device for Graphene, comprise quartz heating chamber and can be placed on the graphite bucket in heating chamber, it is characterized in that:
Described quartz heating chamber, in comprising, there are upper shed cavity (1) and the top cover (9) of hollow sandwich, on top cover (9), be provided with thermometric window (3) and inlet mouth (2), cavity bottom is provided with thermometric window (3) and air outlet (5), cavity (1) one side roof part is provided with the cooling water outlet (4) with hollow sandwich UNICOM, cavity (1) opposite side bottom is provided with the entrance of cooling water (6) with hollow sandwich UNICOM, is provided with thermal insulation layer (7) in cavity (1);
Described graphite bucket, comprises the staving (10) of upper end open, and staving (10) upper base surface is provided with groove (11), is provided with at least two preset piecess (12) in graphite bucket upper portion side wall, is placed with heat reflection screen (13) on preset pieces (12).
2. device according to claim 1, is characterized in that: thermal insulation layer (7) middle part in described quartz heating chamber is thermal insulation layer groove (8).
3. device according to claim 2, is characterized in that: the thermometric window (3) that the cavity bottom in described quartz heating chamber arranges runs through thermal insulation layer (7) and is connected with thermal insulation layer groove (8).
4. device according to claim 1, is characterized in that: the staving upper base surface of described graphite bucket is provided with tantalum carbide coating.
5. device according to claim 1, is characterized in that: heat reflection screen (13) surface of described graphite bucket is minute surface.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201320664729.XU CN203593622U (en) | 2013-10-25 | 2013-10-25 | Device for preparing graphene on silicon carbide substrate |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201320664729.XU CN203593622U (en) | 2013-10-25 | 2013-10-25 | Device for preparing graphene on silicon carbide substrate |
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| CN203593622U true CN203593622U (en) | 2014-05-14 |
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| CN201320664729.XU Withdrawn - After Issue CN203593622U (en) | 2013-10-25 | 2013-10-25 | Device for preparing graphene on silicon carbide substrate |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103523774A (en) * | 2013-10-25 | 2014-01-22 | 山东天岳晶体材料有限公司 | Preparation method of graphene |
| CN105984865A (en) * | 2015-02-11 | 2016-10-05 | 中国科学院物理研究所 | Crucible for graphene growth through silicon carbide platelet pyrolysis |
| CN108517512A (en) * | 2018-03-09 | 2018-09-11 | 昆山国显光电有限公司 | A kind of chemical vapor depsotition equipment and its reaction chamber |
| IT201900000235A1 (en) * | 2019-01-09 | 2020-07-09 | Lpe Spa | Reaction chamber for a deposition reactor with cavity and bottom sealing element and reactor |
| CN114197039A (en) * | 2021-12-09 | 2022-03-18 | 山东大学 | Method for epitaxially growing uniform graphene more than six inches on 4H-SiC substrate |
-
2013
- 2013-10-25 CN CN201320664729.XU patent/CN203593622U/en not_active Withdrawn - After Issue
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103523774A (en) * | 2013-10-25 | 2014-01-22 | 山东天岳晶体材料有限公司 | Preparation method of graphene |
| CN103523774B (en) * | 2013-10-25 | 2016-02-10 | 山东天岳晶体材料有限公司 | A kind of preparation method of Graphene |
| CN105984865A (en) * | 2015-02-11 | 2016-10-05 | 中国科学院物理研究所 | Crucible for graphene growth through silicon carbide platelet pyrolysis |
| CN108517512A (en) * | 2018-03-09 | 2018-09-11 | 昆山国显光电有限公司 | A kind of chemical vapor depsotition equipment and its reaction chamber |
| IT201900000235A1 (en) * | 2019-01-09 | 2020-07-09 | Lpe Spa | Reaction chamber for a deposition reactor with cavity and bottom sealing element and reactor |
| WO2020144567A1 (en) * | 2019-01-09 | 2020-07-16 | Lpe S.P.A. | Reaction chamber for a deposition reactor with interspace and lower closing element and reactor |
| CN114197039A (en) * | 2021-12-09 | 2022-03-18 | 山东大学 | Method for epitaxially growing uniform graphene more than six inches on 4H-SiC substrate |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of utility model: Device for preparing graphene on silicon carbide substrate Effective date of registration: 20150618 Granted publication date: 20140514 Pledgee: China Co truction Bank Corp Ji'nan hi tech sub branch Pledgor: Shandong Tianyue Crystal Material Co., Ltd. Registration number: 2015990000494 |
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| PLDC | Enforcement, change and cancellation of contracts on pledge of patent right or utility model | ||
| AV01 | Patent right actively abandoned |
Granted publication date: 20140514 Effective date of abandoning: 20160210 |
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| C25 | Abandonment of patent right or utility model to avoid double patenting | ||
| PC01 | Cancellation of the registration of the contract for pledge of patent right |
Date of cancellation: 20160726 Granted publication date: 20140514 Pledgee: China Co truction Bank Corp Ji'nan hi tech sub branch Pledgor: Shandong Tianyue Crystal Material Co., Ltd. Registration number: 2015990000494 |
|
| PLDC | Enforcement, change and cancellation of contracts on pledge of patent right or utility model |