CN104477897B - Fixture and the preparation method of graphene film are prepared in a kind of mass-producing - Google Patents
Fixture and the preparation method of graphene film are prepared in a kind of mass-producing Download PDFInfo
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- CN104477897B CN104477897B CN201410767015.0A CN201410767015A CN104477897B CN 104477897 B CN104477897 B CN 104477897B CN 201410767015 A CN201410767015 A CN 201410767015A CN 104477897 B CN104477897 B CN 104477897B
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Abstract
The present invention relates to fixture and preparation method that graphene film is prepared in a kind of mass-producing, fixture of the present invention comprises grid and Under The Grille frame, the some perpendicular straight arranged top grating that upper grills comprises the semicircle fixed frame of grills and is fixed on the inner headed face of the semicircle fixed frame of grills, top grating gap is equipped with between adjacent top grating, some perpendicular straight arranged lower grid plate under Under The Grille frame comprises the semicircle fixed frame of Under The Grille frame and is fixed on the inner headed face of the semicircle fixed frame of Under The Grille frame, lower grid plate gap is equipped with between adjacent lower grid plate, top grating is inserted in lower grid plate gap, lower grid plate is inserted in top grating gap, the semicircle fixed frame of upper grills abuts with the semicircle fixed frame of Under The Grille frame.The present invention makes full use of the growing space of graphene film, improves the growth population of single graphene film, realizes mass-producing preparation, reduces the production cost of graphene film greatly.
Description
Technical field
The present invention relates to graphene growth preparing technical field, particularly relate to fixture and preparation method that graphene film is prepared in a kind of mass-producing.
Background technology
Graphene is the two-dimentional novel material of single carbon atom thickness, in mechanics, calorifics, optics, electricity etc., all have very excellent character, as the physical strength of superelevation, good thermal conductivity, wide spectrum high-clarity and superpower electroconductibility etc.The physical properties of Graphene uniqueness determines its wide application prospect, has caused the research boom of international academic community and industry member.Be applied to flexible transparent electrode, then the transmittance of device is stronger, electroconductibility is better, power consumption is lower, is expected to replace the leading ito transparent electrode of existing market, is widely used in the optoelectronic device such as Flexible Displays and touch-screen.Graphene is for the manufacture of photon sensor and photodetector, and the comparable similar detector of sensitivity improves several order of magnitude.Graphene also can be used as the basic material of nanoelectronic integrated device of future generation, makes device travelling speed up to 500GHz, and the existing device of observable index significantly reduces.In addition, Graphene still can play an important role in other sides such as medical treatment.
Through extensive research in recent years, chemical Vapor deposition process (CVD) prepares one of the most promising method of graphene film.CVD in vacuum vessel, the carbon sources such as methane is heated to specified temp make it decompose, on the transition metal paper tinsels such as Ni, Cu, then form the technology of graphene film.But fast, mass-producing prepares big area, the method for high-quality graphene never makes a breakthrough, significantly limit efficiency and output prepared by Graphene, hinder its further industrialized development.Because CVD prepares high-quality Graphene and usually needs to carry out at graphene growth substrate fusing point (about 1000 degree), metallic growth substrate can bond at these elevated temperatures each other, which limits the amount that single prepares Graphene.Although the graphene film that diagonal lines reaches 15 inches once can be prepared by Korea S Cheng Jun shop university, but it adopts diameter to be the tube furnace of 8 inches, and graphene growth substrate is paved with the acquisition of overall boiler tube inwall, all the other growing spaces are not used appropriately, not only the quantity of single growth batch preparation is few, but also causes the wasting of resources.In the recent period, Sony adopts the way of heated by electrodes growth substrates to achieve volume to volume growing graphene, but owing to being local heating and temperature is lower, the Graphene prepared is of poor quality, can not meet application demand.
Summary of the invention
Technical problem to be solved by this invention is to provide fixture and the preparation method that graphene film is prepared in a kind of mass-producing, improves the growth population of single graphene film, realizes mass-producing preparation, reduces the production cost of graphene film greatly.
The technical scheme that the present invention solves the problems of the technologies described above is as follows: the fixture of graphene film is prepared in a kind of mass-producing, comprise grid and Under The Grille frame, some top gratings of arranging straight down that described upper grills comprises the semicircle fixed frame of grills and is fixed on the inner headed face of the semicircle fixed frame of described upper grills, top grating gap is equipped with between adjacent described top grating, some lower grid plates of arranging straight up under described Under The Grille frame comprises the semicircle fixed frame of Under The Grille frame and is fixed on the inner headed face of the semicircle fixed frame of described Under The Grille frame, lower grid plate gap is equipped with between adjacent described lower grid plate, described top grating is inserted in described lower grid plate gap, described lower grid plate is inserted in described top grating gap, the semicircle fixed frame of described upper grills abuts with the semicircle fixed frame of described Under The Grille frame, described top grating is provided with gap away between one side of the semicircle fixed frame of described upper grills and the semicircle fixed frame of described Under The Grille frame, described lower grid plate is provided with gap away between one side of the semicircle fixed frame of described Under The Grille frame and the semicircle fixed frame of described upper grills.
On the basis of technique scheme, the present invention can also do following improvement.
Further, the two ends of the semicircle fixed frame of described upper grills are equipped with the upper grills horizontal fixed plate be fixedly connected with described top grating.
Further, the two ends of the semicircle fixed frame of described Under The Grille frame are equipped with the Under The Grille frame horizontal fixed plate be fixedly connected with described lower grid plate.
Further, the bottom surface of described upper grills horizontal fixed plate is provided with projection, and the end face of described Under The Grille frame horizontal fixed plate is provided with the groove matched with described projection.
Further, the clearance distance in described top grating gap 2mm to 15cm wider than the thickness of described lower grid plate.
Further, the thickness of described top grating and described lower grid plate is 2mm to 10cm.
The method of graphene film is prepared in a kind of mass-producing, the preparation of the method by using above-mentioned fixture to realize graphene film, comprise the following steps: step one, separate upper grills and the Under The Grille frame of fixture, graphene growth substrate is laid between upper grills and Under The Grille frame, upper grills and Under The Grille frame are slowly closed up, in the gap that graphene growth substrate is filled between top grating and lower grid plate, cuts off the peripheral unnecessary graphene growth substrate of fixture;
Step 2, puts into graphene growth device by the fixture being filled with graphene growth substrate, adopts chemical vapor deposition graphene film.
Further, the material of described upper grills and described Under The Grille frame is one or more combinations in quartz, pottery, carbon fiber.
Further, the foil of described graphene growth substrate to be material be in copper, nickel, iron, cobalt, platinum, ruthenium one or more alloys of composition arbitrarily.
The invention has the beneficial effects as follows: the present invention makes full use of the growing space of graphene film; put graphene growth substrate as much as possible into limited growing space; thus improve the growth population of single graphene film; realize mass-producing preparation, reduce the production cost of graphene film greatly.Prepare in Graphene process at CVD single, be placed in process cavity limited in CVD growing system by back-shaped superimposing technique by as much as possible for graphene growth substrate, and achieve graphene growth substrate after vacuum, hot conditions, between graphene growth substrate with graphene growth substrate together with mutually non-adhesive or graphene substrate surface finish deform.Single is prepared in Graphene process, while mass-producing increases graphene growth substrate quantity, also assures that the planarization on growth substrates surface, for the preparation of high-quality graphene is laid a good foundation.
Accompanying drawing explanation
Fig. 1 is the side-view that the fixture of graphene film is prepared in a kind of mass-producing of the present invention;
Fig. 2 is the side-view that the upper grills of the fixture of graphene film is prepared in a kind of mass-producing of the present invention;
Fig. 3 is the stereographic map that the upper grills of the fixture of graphene film is prepared in a kind of mass-producing of the present invention;
Fig. 4 is the end enlarged view that the upper grills of the fixture of graphene film is prepared in a kind of mass-producing of the present invention;
Fig. 5 is the side-view that the Under The Grille frame of the fixture of graphene film is prepared in a kind of mass-producing of the present invention;
Fig. 6 is the stereographic map that the Under The Grille frame of the fixture of graphene film is prepared in a kind of mass-producing of the present invention;
Fig. 7 is the end enlarged view that the Under The Grille frame of the fixture of graphene film is prepared in a kind of mass-producing of the present invention;
Fig. 8 be a kind of mass-producing of the present invention prepare graphene film fixture on grills and Under The Grille frame separately, the schematic diagram before fixing Graphene growth substrates;
Fig. 9 be a kind of mass-producing of the present invention prepare graphene film fixture on grills and Under The Grille frame fix the schematic diagram of Graphene growth substrates;
In accompanying drawing, the list of parts representated by each label is as follows:
1, upper grills, the semicircle fixed frame of 1-1, upper grills, 1-2, top grating, 1-3, top grating gap, 1-4, upper grills horizontal fixed plate, 1-5, projection, 2, Under The Grille frame, the semicircle fixed frame of 2-1, Under The Grille frame, 2-2, lower grid plate, 2-3, lower grid plate gap, 2-4, Under The Grille frame horizontal fixed plate, 2-5, groove, 3, graphene growth substrate.
Embodiment
Be described principle of the present invention and feature below in conjunction with accompanying drawing, example, only for explaining the present invention, is not intended to limit scope of the present invention.
Fixture of the present invention comprises grid 1 and Under The Grille frame 2, the some perpendicular straight arranged top grating 1-2 that described upper grills 1 comprises the semicircle fixed frame 1-1 of grills and is fixed on the inner headed face of the semicircle fixed frame 1-1 of described upper grills, top grating gap 1-3 is equipped with between adjacent described top grating 1-2, some perpendicular straight arranged lower grid plate 2-2 under described Under The Grille frame 2 comprises the semicircle fixed frame 2-1 of Under The Grille frame and is fixed on the inner headed face of the semicircle fixed frame 2-1 of described Under The Grille frame, lower grid plate gap 2-3 is equipped with between adjacent described lower grid plate 2-2, described top grating 1-2 is inserted in described lower grid plate gap 2-3, described lower grid plate 2-2 is inserted in described top grating gap 1-3, the semicircle fixed frame 1-1 of described upper grills abuts with the semicircle fixed frame 2-1 of described Under The Grille frame, described top grating 1-2 is provided with gap away between one side of the semicircle fixed frame 1-1 of described upper grills and the semicircle fixed frame 2-1 of described Under The Grille frame, described lower grid plate 2-2 is provided with gap away between one side of the semicircle fixed frame 2-1 of described Under The Grille frame and the semicircle fixed frame 1-1 of described upper grills.
The two ends of the semicircle fixed frame 1-1 of described upper grills are equipped with the upper grills horizontal fixed plate 1-4 be fixedly connected with described top grating 1-2.The two ends of the semicircle fixed frame 2-1 of described Under The Grille frame are equipped with the Under The Grille frame horizontal fixed plate 2-4 be fixedly connected with described lower grid plate 2-2.The bottom surface of described upper grills horizontal fixed plate 1-4 is provided with protruding 1-5, and the end face of described Under The Grille frame horizontal fixed plate 2-4 is provided with the groove 2-5 matched with described protruding 1-5.The clearance distance 2mm to 15cm wider than the thickness of described lower grid plate 2-2 of described top grating gap 1-3.The clearance distance 2mm to 15cm wider than the thickness of described top grating 1-2 of described lower grid plate gap 2-3.The thickness of described top grating 1-2 and described lower grid plate 2-2 is 2mm to 10cm.Described top grating 1-2 can be solid material, also can be hollow structure.The hollow quartz plate that preferably 5mm is thick in the present invention.The thickness of slab of described top grating 1-2 and described lower grid plate 2-2 can be the combination of identical or different thickness turbogrid plates.
A method for graphene film is prepared in mass-producing, and the method, by the preparation using above-mentioned fixture to realize graphene film, comprises the following steps:
Step one, separate upper grills 1 and the Under The Grille frame 2 of fixture, graphene growth substrate 3 is laid between upper grills 1 and Under The Grille frame 2, as shown in Figure 8, upper grills 1 and Under The Grille frame 2 are slowly closed up, in the gap that graphene growth substrate 3 is filled between top grating 1-2 and lower grid plate 2-2, cut off the peripheral unnecessary graphene growth substrate 3 of fixture, as shown in Figure 9;
Step 2, puts into graphene growth device by the fixture being filled with graphene growth substrate 3, adopts chemical vapor deposition graphene film.
The material of described upper grills 1 and described Under The Grille frame 2 be quartz, pottery, carbon fiber, can the non-metallic material of resistance to about 1000 degree high temperature, resistance to about 1000 degree high temperature outer metallic surface plating pottery in one or more combinations.Described graphene growth substrate 3 for material be the foil of one or more any alloys of composition in copper, nickel, iron, cobalt, platinum, ruthenium.The thickness of graphene growth substrate 3 gets 10-200 micron, in the present invention preferably the Copper Foil of 45 micron thickness as graphene growth substrate 3.
In the present invention, the semicircle retaining plate that the semicircle fixed frame of lower turbogrid plates is preferably isometric with turbogrid plates, the semicircle retaining plate of upper turbogrid plates is made up of two pieces of short slabs, is distributed in turbogrid plates two ends respectively.
The invention has the beneficial effects as follows: the present invention makes full use of the growing space of graphene film; put graphene growth substrate 3 as much as possible into limited growing space; thus improve the growth population of single graphene film; realize mass-producing preparation, reduce the production cost of graphene film greatly.Prepare in Graphene process at CVD single, be placed in process cavity limited in CVD growing system by back-shaped superimposing technique by as much as possible for graphene growth substrate 3, and achieve graphene growth substrate 3 after vacuum, hot conditions, between graphene growth substrate 3 with graphene growth substrate 3 together with mutually non-adhesive or graphene substrate surface finish do not deform.Single is prepared in Graphene process, while mass-producing increases graphene growth substrate 3 quantity, also assures that the planarization on growth substrates surface, for the preparation of high-quality graphene is laid a good foundation.
Upper grid horizontal fixed plate and lower grid horizontal fixed plate play the effect of fixing top grating 1-2 and lower grid plate 2-2 on the one hand, and can serve as the operation " handle " of grid and lower grid, facilitate the operation to upper grid and lower grid; On the other hand, the protruding 1-5 part of the groove 2-5 of lower grid horizontal fixed plate and upper grid horizontal fixed plate upper and lower grid dock combine time riveted, play the effect of fixing upper and lower grid slippage, prevent landing or displacement in grid transmission or technological process.The horizontal fixed plate abnormity of upper and lower turbogrid plates can riveted part be not limited to be lower grid retaining plate groove 2-5 mutually, and the protruding 1-5 of upper grid retaining plate can be the permutation and combination of the two, also can be that other can the polymorphic structure of riveted mutually.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. the fixture of graphene film is prepared in a mass-producing, it is characterized in that, comprise grid (1) and Under The Grille frame (2), some top gratings (1-2) of arranging straight down that described upper grills (1) comprises the semicircle fixed frame (1-1) of grills and is fixed on the inner headed face of the semicircle fixed frame (1-1) of described upper grills, top grating gap (1-3) is equipped with between adjacent described top grating (1-2), some lower grid plates (2-2) of arranging straight up under described Under The Grille frame (2) comprises the semicircle fixed frame (2-1) of Under The Grille frame and is fixed on the inner headed face of the semicircle fixed frame (2-1) of described Under The Grille frame, lower grid plate gap (2-3) is equipped with between adjacent described lower grid plate (2-2), described top grating (1-2) is inserted in described lower grid plate gap (2-3), described lower grid plate (2-2) is inserted in described top grating gap (1-3), the semicircle fixed frame (1-1) of described upper grills abuts with the semicircle fixed frame (2-1) of described Under The Grille frame, described top grating (1-2) away from the semicircle fixed frame (1-1) of described upper grills while and be provided with gap between the semicircle fixed frame (2-1) of described Under The Grille frame, described lower grid plate (2-2) away from the semicircle fixed frame (2-1) of described Under The Grille frame while and be provided with gap between the semicircle fixed frame (1-1) of described upper grills.
2. the fixture of graphene film is prepared in a kind of mass-producing according to claim 1; it is characterized in that, the two ends of the semicircle fixed frame (1-1) of described upper grills are equipped with the upper grills horizontal fixed plate (1-4) be fixedly connected with described top grating (1-2).
3. the fixture of graphene film is prepared in a kind of mass-producing according to claim 2; it is characterized in that, the two ends of the semicircle fixed frame (2-1) of described Under The Grille frame are equipped with the Under The Grille frame horizontal fixed plate (2-4) be fixedly connected with described lower grid plate (2-2).
4. the fixture of graphene film is prepared in a kind of mass-producing according to claim 3; it is characterized in that; the bottom surface of described upper grills horizontal fixed plate (1-4) is provided with projection (1-5), and the end face of described Under The Grille frame horizontal fixed plate (2-4) is provided with the groove (2-5) matched with described projection (1-5).
5. the fixture of graphene film is prepared in a kind of mass-producing according to any one of Claims 1-4, it is characterized in that, the clearance distance 2mm to 15cm wider than the thickness of described lower grid plate (2-2) of described top grating gap (1-3).
6. the fixture of graphene film is prepared in a kind of mass-producing according to any one of Claims 1-4, it is characterized in that, the clearance distance 2mm to 15cm wider than the thickness of described top grating (1-2) of described lower grid plate gap (2-3).
7. the fixture of graphene film is prepared in a kind of mass-producing according to any one of Claims 1-4, it is characterized in that, the thickness of described top grating (1-2) and described lower grid plate (2-2) is 2mm to 10cm.
8. a method for graphene film is prepared in mass-producing, it is characterized in that, the method, by the preparation using the fixture as described in any one of claim 1-7 to realize graphene film, comprises the following steps:
Step one, separate upper grills (1) and the Under The Grille frame (2) of fixture, graphene growth substrate (3) is laid between upper grills (1) and Under The Grille frame (2), upper grills (1) and Under The Grille frame (2) are slowly closed up, in the gap that graphene growth substrate (3) is filled between top grating (1-2) and lower grid plate (2-2), cut off the peripheral unnecessary graphene growth substrate of fixture;
Step 2, puts into graphene growth device by the fixture being filled with graphene growth substrate (3), adopts chemical vapor deposition graphene film.
9. the method for graphene film is prepared in a kind of mass-producing according to claim 8, it is characterized in that, the material of described upper grills (1) and described Under The Grille frame (2) is one or more combinations in quartz, pottery, carbon fiber.
10. the method for graphene film is prepared in a kind of mass-producing according to claim 8; it is characterized in that, described graphene growth substrate (3) for material be the foil of one or more any alloys of composition in copper, nickel, iron, cobalt, platinum, ruthenium.
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