CN204324891U - A kind of alternating expression prepares the fixture of Graphene on a large scale - Google Patents
A kind of alternating expression prepares the fixture of Graphene on a large scale Download PDFInfo
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- CN204324891U CN204324891U CN201420786852.3U CN201420786852U CN204324891U CN 204324891 U CN204324891 U CN 204324891U CN 201420786852 U CN201420786852 U CN 201420786852U CN 204324891 U CN204324891 U CN 204324891U
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Abstract
The utility model relates to the fixture that a kind of alternating expression prepares Graphene on a large scale, comprise two bracing frames vertically arranged, two support frames as described above are fixedly connected with by the support bar that two be arranged in parallel, the two ends of two described support bars are fixedly connected with the upper vertical of two bracing frames respectively, two described support bars are in same level and leave gap between two described support bars, and the top of two described support bars is placed with at least two support sticks.The beneficial effects of the utility model are: the utility model breaches existing silica tube size to the quantitative limitation of single growth number; metal catalyst and quartzy tube wall are isolated by support; avoid adhesion between metal catalyst and quartzy tube wall under high temperature; and then make metal catalyst generation fold; the use of support and buffer layer, had both improve the growth quality of Graphene, too increased the quantity of single growth Graphene; easy and simple to handle, be applicable to large-scale production.
Description
Technical field
The utility model relates to technical field of graphene preparation, particularly relates to the fixture that a kind of alternating expression prepares Graphene on a large scale.
Background technology
Graphene is the cellular monolayer carbon material that carbon atom becomes key to form according to sp2 hydridization, its special crystalline structure has given the physical properties of the many excellences of Graphene, as room-temperature quantum Lovell effect, high carrier rate of migration, high heat conductance, long-range ballistic transport character etc. suddenly.The physical properties of these excellences makes Graphene become one of electronic material of most potentiality.
At present, the method preparing Graphene mainly comprises mechanically peel method, SiC crystal epitaxial growth method, graphite oxide reduction method and the chemical Vapor deposition process on transition metal.Mechanically peel method is mainly used in laboratory and prepares high-quality graphene sample, but the Graphene size prepared is less, the number of plies is difficult to control, and yields poorly.SiC crystal epitaxial growth method can prepare large size multi-layer graphene, because SiC single crystal is expensive, thus causes its preparation cost higher.Graphite oxide reduction method can prepare a large amount of multi-layer graphene, but the different numbers of plies being separated Graphene are more difficult, and the Graphene size prepared is little, of poor quality.Prepare the chemical Vapor deposition process of method mainly on the metallic film such as copper, nickel of large-area high-quality Graphene at present.
In the CVD preparation process of existing Graphene, metal catalyst substrate is generally directly placed in silica tube inside, can place 1 to several pieces according to the size of heating installation, and the quantity of single growth Graphene is subject to the restriction of silica tube size.And metal catalyst very easily deformation occurs under high temperature, produce fold, thus reduce the growth quality of graphene product.
Utility model content
Technical problem to be solved in the utility model is to provide one can prepare Graphene on a large scale, and the alternating expression of metal catalyst layer generation deformation can be avoided to prepare the fixture of Graphene on a large scale.
The technical scheme that the utility model solves the problems of the technologies described above is as follows: a kind of alternating expression prepares the fixture of Graphene on a large scale, comprise two bracing frames vertically arranged, two support frames as described above are fixedly connected with by the support bar that two be arranged in parallel, the two ends of two described support bars are fixedly connected with the upper vertical of two bracing frames respectively, two described support bars are in same level and leave gap between two described support bars, and the top of two described support bars is placed with at least two support sticks.
On the basis of technique scheme, the utility model can also do following improvement.
Further, the material of support frame as described above, described support bar and described support stick is the ordinary rigid material of high temperature resistant mechanically resistant material or surperficial spin coating high-temperature-resistant layer.
Further, the vertical section of support frame as described above is square trapezoidal or semicircle.
Further, the cylindrical rod of described support stick to be diameter be 1-10mm.
Adopt above-mentioned fixture to prepare the method for Graphene, comprise the following steps:
Step one, cleans and pre-treatment fixture and buffer layer;
Step 2, at least two holes are beaten respectively in the same level position on metal catalyst layer top and buffer layer top, hole is identical with the number of described support stick, multiple metal catalyst layer and multiple buffer layers alternating are stacked and makes the hole in metal catalyst layer and the hole site one_to_one corresponding on buffer layer, by two described support sticks respectively one to one through hole, then there is the support stick of metal catalyst layer and buffer layer to be positioned on two described support bars string, make metal catalyst layer and described buffer layer between two described support bars;
Step 3, is positioned over the fixture being mounted with metal catalyst layer and buffer layer in graphene growth device, adopts chemical vapor deposition graphene film;
Step 4, after graphene growth completes, takes out fixture from graphene growth device, is extracted out by support stick, and separately metal catalyst layer and buffer layer, must grow the metal catalyst layer having Graphene.
Further, the method that in described step one, clean adopts is ultrasonic cleaning successively in acetone, ethanol, and scavenging period is 15-30min.
Further, in described step one, pretreated processing mode is dry up with the nitrogen that purity is 99.999%.
Further, the material of described metal catalyst layer is copper, nickel, iron, the alloy of one or more combinations in cobalt.
The beneficial effects of the utility model are: the utility model breaches existing silica tube size to the quantitative limitation of single growth number, metal catalyst and quartzy tube wall are isolated by support, avoid adhesion between metal catalyst and quartzy tube wall under high temperature, and then make metal catalyst generation fold, reduce the growth quality of Graphene; Buffer layer is isolated between metal catalyst layer, avoids adhesion between metal catalyst layer under high temperature, also improves the growth quality of Graphene.The use of support and buffer layer, had both improve the growth quality of Graphene, too increased the quantity of single growth Graphene, easy and simple to handle, was applicable to large-scale production.
Accompanying drawing explanation
Fig. 1 is the structural representation of the utility model fixture;
Fig. 2 is the schematic diagram of the utility model holder metal catalytic basic unit and buffer layer;
Fig. 3 is the schema that fixture of the present utility model prepares Graphene;
In accompanying drawing, the list of parts representated by each label is as follows:
1, bracing frame, 2, support bar, 3, support stick, 4, metal catalyst layer, 5, buffer layer.
Embodiment
Be described principle of the present utility model and feature below in conjunction with accompanying drawing, example, only for explaining the utility model, is not intended to limit scope of the present utility model.
Embodiment one
As shown in Figure 1, the fixture of the present embodiment comprises two bracing frames 1 vertically arranged, two support frames as described above 1 are fixedly connected with by two support bars be arranged in parallel 2, the two ends of two described support bars 2 are fixed with the top of two bracing frames 1 respectively, two described support bars 2 are in same level and leave gap between two described support bars 2, and two described support bars 2 are placed with two support sticks 3.The material of support frame as described above 1, described support bar 2 and described support stick 3 is the ordinary rigid material of high temperature resistant mechanically resistant material or surperficial spin coating high-temperature-resistant layer.The vertical section of support frame as described above 1 is square trapezoidal or semicircle, described support stick 3 for diameter be the cylindrical rod of 1-10mm.
As shown in Figure 3, clean and pre-treatment fixture and buffer layer: the ultrasonic cleaning successively in acetone, ethanol by fixture and buffer layer, scavenging period is respectively 20min, then dries up with the nitrogen that purity is 99.999%;
Two holes are made a call to respectively at the same position on Copper Foil top and buffer layer top, multi-disc Copper Foil and multi-disc buffer layers alternating are stacked and makes the hole on Copper Foil and the hole site on buffer layer corresponding, two described support sticks are each passed through two holes, then the quartz pushrod of Copper Foil and buffer layer there is is to be positioned on two described support bars 2 string, make Copper Foil and described buffer layer between two described support bars 2, as shown in Figure 2;
The fixture being mounted with Copper Foil and buffer layer is put into silica tube, system is vacuumized, be evacuated to 0.1Pa, pass into hydrogen, system is warming up to 900 degree, annealing 30min, passes into methane and hydrogen (if fixture or buffer layer carbon containing in silica tube, in the growing graphene stage, can as carbon source, then not need to pass into carbon-source gas), methane is in metallic surface cracking nucleation, and generate graphene-structured, growth time 20min;
After growth, close methane, continue logical hydrogen, lower the temperature, be down to after room temperature taken out from graphene growth device by fixture until silica tube, extracted out by support stick, separately Copper Foil and buffer layer, must grow the Copper Foil having Graphene.
Embodiment two
As shown in Figure 1, the fixture of the present embodiment comprises two bracing frames 1 vertically arranged, two support frames as described above 1 are fixedly connected with by two support bars be arranged in parallel 2, the two ends of two described support bars 2 are fixed with the top of two bracing frames 1 respectively, two described support bars 2 are in same level and leave gap between two described support bars 2, and two described support bars 2 are placed with two support sticks 3.The material of support frame as described above 1, described support bar 2 and described support stick 3 is the ordinary rigid material of high temperature resistant mechanically resistant material or surperficial spin coating high-temperature-resistant layer.The vertical section of support frame as described above 1 is square trapezoidal or semicircle, described support stick 3 for diameter be the cylindrical rod of 1-10mm.
Clean and pre-treatment fixture and tetrafluoroethylene high temperature cloth: the ultrasonic cleaning successively in acetone, ethanol by fixture and buffer layer, scavenging period is respectively 20min, then dries up with the nitrogen that purity is 99.999%;
Two holes are made a call to respectively at the same position on the top of nickel foil top and tetrafluoroethylene high temperature cloth, multiple nickel foil and multiple buffer layers alternating are stacked and makes the hole on nickel foil and the hole site on buffer layer corresponding, two described quartz pushrods are each passed through two holes, then the quartz pushrod of nickel foil and buffer layer there is is to be positioned on two described support bars 2 string, make nickel foil and described buffer layer between two described support bars 2, as shown in Figure 2;
The fixture being mounted with nickel foil and buffer layer is put into silica tube, system is vacuumized, be evacuated to 0.1Pa, pass into hydrogen, system is warming up to 900 degree, annealing 30min, methane and hydrogen is passed into (if fixture or buffer layer carbon containing in silica tube, in the growing graphene stage, can as carbon source, then not need to pass into carbon-source gas), methane is in metallic surface cracking nucleation, and generate graphene-structured, growth time 20min
After growth, close methane, continue logical hydrogen, lower the temperature, be down to after room temperature taken out from graphene growth device by fixture until silica tube, extracted out by quartz pushrod, separately nickel foil and buffer layer, must grow the nickel foil having Graphene.
The beneficial effects of the utility model are: the utility model breaches existing silica tube size to the quantitative limitation of single growth number, metal catalyst and quartzy tube wall are isolated by support, avoid adhesion between metal catalyst and quartzy tube wall under high temperature, and then make metal catalyst generation fold, reduce the growth quality of Graphene; Buffer layer 5 is isolated between metal catalyst layer 4, avoids adhesion between metal catalyst layer 4 under high temperature, also improves the growth quality of Graphene.The use of fixture and buffer layer 5, had both improve the growth quality of Graphene, too increased the quantity of single growth Graphene, easy and simple to handle, was applicable to large-scale production.
The foregoing is only preferred embodiment of the present utility model, not in order to limit the utility model, all within spirit of the present utility model and principle, any amendment done, equivalent replacement, improvement etc., all should be included within protection domain of the present utility model.
Claims (4)
1. an alternating expression prepares the fixture of Graphene on a large scale, it is characterized in that, comprise two bracing frames (1) vertically arranged, two support frames as described above (1) are fixedly connected with by two support bars be arranged in parallel (2), the two ends of two described support bars (2) are fixedly connected with the upper vertical of two bracing frames (1) respectively, two described support bars (2) are in same level and leave gap between two described support bars (2), and the top of two described support bars (2) is placed with at least two support sticks (3).
2. a kind of alternating expression according to claim 1 prepares the fixture of Graphene on a large scale, it is characterized in that, the material of support frame as described above (1), described support bar (2) and described support stick (3) is the ordinary rigid material of high temperature resistant mechanically resistant material or surperficial spin coating high-temperature-resistant layer.
3. a kind of alternating expression according to claim 1 and 2 prepares the fixture of Graphene on a large scale, it is characterized in that, the vertical section of support frame as described above (1) is square trapezoidal or semicircle.
4. a kind of alternating expression according to claim 1 and 2 prepares the fixture of Graphene on a large scale, it is characterized in that, described support stick (3) for diameter be the cylindrical rod of 1-10mm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201420786852.3U CN204324891U (en) | 2014-12-12 | 2014-12-12 | A kind of alternating expression prepares the fixture of Graphene on a large scale |
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| CN201420786852.3U CN204324891U (en) | 2014-12-12 | 2014-12-12 | A kind of alternating expression prepares the fixture of Graphene on a large scale |
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| CN204324891U true CN204324891U (en) | 2015-05-13 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104495813A (en) * | 2014-12-12 | 2015-04-08 | 重庆墨希科技有限公司 | Fixture and preparation method for staggered-type large-scale preparation of graphene |
-
2014
- 2014-12-12 CN CN201420786852.3U patent/CN204324891U/en not_active Withdrawn - After Issue
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104495813A (en) * | 2014-12-12 | 2015-04-08 | 重庆墨希科技有限公司 | Fixture and preparation method for staggered-type large-scale preparation of graphene |
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| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| AV01 | Patent right actively abandoned |
Granted publication date: 20150513 Effective date of abandoning: 20160608 |
|
| AV01 | Patent right actively abandoned |
Granted publication date: 20150513 Effective date of abandoning: 20160608 |
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| C25 | Abandonment of patent right or utility model to avoid double patenting |