CN105274491A - Preparation method for graphene-boron nitride heterogeneous phase composite thin film material - Google Patents
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- CN105274491A CN105274491A CN201510769561.2A CN201510769561A CN105274491A CN 105274491 A CN105274491 A CN 105274491A CN 201510769561 A CN201510769561 A CN 201510769561A CN 105274491 A CN105274491 A CN 105274491A
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Abstract
The invention relates to a preparation method for a graphene-boron nitride heterogeneous phase composite thin film material. Both graphene and boron nitride atomic layer thin films can be grown through a chemical vapor deposition method at present, and graphene and boron nitride of a graphene boron nitride heterogeneous phase composite thin film are transferred to the substrate surface to achieve the preparation of a composite thin film after a fractional step method is used. The interface of the graphene and the boron nitride is always polluted through the method, and the electrical properties of the composite thin film are influenced. A boron nitride and graphene composite material in the same atomic layer face is always obtained by growing the boron nitride on the surface of the graphene. According to the preparation method for the graphene-boron nitride heterogeneous phase composite thin film material, a stepwise synthesis method is adopted; the boron nitride is firstly synthesized, and then the graphene is grown on an interface layer of the boron nitride and a metal catalyzer to obtain the graphene boron nitride heterogeneous phase composite thin film material. The graphene and the boron nitride interface prepared through the method is clean and free of pollution, and the electrical properties of the composite thin film material are facilitated to be improved.
Description
Technical field
The invention belongs to field of material technology, be specifically related to the preparation method of a kind of Graphene-boron nitride compound tow-dimensions atom layer film.
Background technology
Graphene is obtained by mechanically peel legal system first from 2004, the whole world has started the upsurge of research Graphene and other two dimensions (2D) material, successfully prepare multiple 2D material, as hexagonal boron nitride (h-BN), moly-sulfide, cobalt acid lithium, silene, germanium alkene and arsenic alkene and antimony alkene etc.The 2D material that Graphene is led has the property not available for many macroscopic body materials.Graphene is thin, the hardest material in known world, and almost completely transparent, individual layer only absorbs the light of 2.3%; Thermal conductivity is higher than carbon nanotube and diamond, and normal temperature electronic mobility exceedes carbon nanotube or silicon wafer, resistivity than copper and Yin Geng low, be in the world electroconductibility best material.Hexagonal boron nitride h-BN is also the plane hexagonal honeycomb structure of similar Graphene, has the high heat conductance of the Graphene that matches in excellence or beauty; The chemical stability higher than Graphene, in atmosphere, 1000 DEG C are not oxidized, and Graphene 600 DEG C is oxidized; H-BN is isolator, specific inductivity 3-4, voltage breakdown 0.7V/nm, close with silicon oxide, be the extraordinary base material of Graphene, compared with silicon oxide substrate, h-BN atom planar Cheng Jian, vertical direction is without any outstanding key, and surface finish reaches atom level, the scattering of interface to electronics can be reduced, Graphene electronic mobility can be made to improve an order of magnitude.The two-dimentional composite film material of hexagonal boron nitride and Graphene will have broad application prospects in following nanometer Two-dimensional electron device preparation.
The most frequently used preparation method also most with application prospect of Graphene is chemical Vapor deposition process (CVD).The method Graphene is created on metallic catalyst surfaces, adopts polymkeric substance as support, dissolves removal metal catalyst and is finally transferred to target substrate.In h-BN two-dimensional film synthetic method, most study is CVD, expects to obtain high quality, large size, the controlled h-BN atomic layer level thin film of the atom number of plies by CVD.About the seventies in last century, successfully synthesize h-BN [10-11] by CVD, the stuctures and properties of boron nitride body material is mainly paid close attention in research at that time.The people such as nineteen ninety-five Nagashima are with borazine under ultrahigh vacuum(HHV), hot conditions, and the h-BN monoatomic layer in metallic surface epitaxy, finds that the electronic structure of h-BN is irrelevant with growth substrate (nickel, palladium and platinum).The people such as Preobrajenski in 2005 grown monoatomic layer h-BN in copper and mickel substrate, and find that h-BN is chemisorbed on copper nickel substrate surface, the chemical bond between h-BN with nickel is stronger, more weak with the chemical bond between copper.2010, by Graphene preparation inspire, the people such as Ajayan prepare large size polyatom layer h-BN film by CVD on metal copper foil surface first, and successfully by h-BN film transfer to other substrate surface.
In sum, can in the Graphene of metal catalyst substrate surface synthesis single kind or boron nitride by chemical Vapor deposition process.Although graphenic surface growing boron nitride also studies have reported that, growth method is continued growth boron nitride on the graphenic surface of metallic catalyst surfaces growth, or at the mixture of metallic catalyst surfaces simultaneously growing boron nitride and Graphene while growing graphene, but boron nitride and metallic film catalyzer two-layer between the method for interface growing graphene also do not have been reported.Present method is by the method for High temperature diffusion crystallization at metallic film catalyst surface and two-dimentional boron nitride atomic shell interface growing graphene, the heterogeneous phase composite film material of synthesizing graphite alkene/boron nitride.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, propose the preparation method of the heterogeneous phase composite film material of a kind of Graphene-boron nitride.
The inventive method adopts chemical Vapor deposition process (CVD) with transition metal copper or nickel catalyzator for substrate, cool fast after soak, the boron nitride pellicle of 1 ~ 5 carbon atomic layer thickness is prepared at metal catalyst film surface, then the boron nitride on one of them surface in metal catalytic film upper and lower surface is removed, carbon source is applied afterwards on the metallic surface of removing boron nitride, then under protection of reducing atmosphere, be elevated to high temperature and cool after keeping certain temperature, obtain the heterogeneous phase laminated film of Graphene-boron nitride in the growth of metal catalyst film surface.
The concrete steps of the preparation method of the heterogeneous phase composite film material of a kind of Graphene-boron nitride of the present invention are:
Step (1), be that the hydrochloric acid of O.5 ~ 1.5mol/L embathes 5 ~ 10 seconds by tinsel concentration, dry up with nitrogen after washed with de-ionized water, put into the silica tube of electric furnace;
The metal of described tinsel is copper, nickel or cupronickel.
Continue the gas mixture passing into argon gas and hydrogen in step (2), silica tube, the throughput ratio of argon gas and hydrogen is 1 ~ 3:2, is incubated 5 ~ 30 minutes after furnace temperature being risen to 900 ~ 1000 DEG C.
Step (3), simultaneously in silica tube, pass into boron ammonia alkane steam, close after 20 ~ 30 minutes and pass into boron ammonia alkane steam.Boron ammonia alkane steam is produced by heating in water bath boron ammonia alkane, bath temperature 40 ~ 100 DEG C.
Step (4), electric furnace stop heating, and silica tube is cooled to normal temperature, and rate of cooling is 20 ~ 30 DEG C/min, then close and pass into hydrogen and argon gas, take out tinsel.
Step (5), by tinsel take out, tinsel has two surfaces, is respectively upper surface and lower surface.By the aqueous solution soaking metallic upper surface 10 ~ 60 seconds of iron(ic) chloride, then use washed with de-ionized water.
Step (6), the tinsel upper surface that step (5) is obtained, coating carbon source 0.1 ~ 0.5g;
Described carbon source is paraffin or carbon dust.
Step (7), the upper surface that step (6) obtains there is the tinsel of carbon source, put into the gas mixture that silica tube continues to pass into argon gas and hydrogen, the throughput ratio of argon gas and hydrogen is 5 ~ 15:10, is incubated 5 ~ 30 minutes after furnace temperature being risen to 900 ~ 1000 DEG C.
Step (8). electric furnace stops heating, and silica tube is cooled to normal temperature, and rate of cooling is 20 ~ 30 DEG C/min, then closes and passes into hydrogen and argon gas, take out tinsel.
Step (9). tinsel is taken out, at tinsel lower surface surface spin coating PMMA solution, PMMA solution forms PMMA film in atmosphere for dry 5 ~ 30 minutes and is attached on tinsel surface, then immerse in ferric chloride Solution to dissolve and remove tinsel, to the PMMA film transfer on ferric chloride Solution surface be swum in silicon substrate surface afterwards, then silicon base is immersed in acetone, through 30 ~ 180 minutes, obtain the Graphene-boron nitride two dimension composite film material being transferred to silicon chip surface.
Beneficial effect of the present invention: the inventive method is by crystallization when carbon high-temperature digestion in a metal and cooling, growing graphene between boron nitride and metal base, form Graphene-boron nitride two dimension composite film material, the matrix material of preparation is owing to being direct growth acquisition, in growth and transfer process, Graphene and boron nitride interface are not all subject to any pollution, and the two-dimentional composite film material of preparation has good electric property.
Embodiment
Embodiment 1:
Step (1). be that hydrochloric acid O.5mol/L embathes 10 seconds by copper sheet (3cmx2cmx0.05cm) by concentration, dry up with nitrogen after washed with de-ionized water, put into the silica tube of electric furnace;
Step (2). continue the gas mixture passing into argon gas and hydrogen in silica tube, the throughput ratio of argon gas and hydrogen is 1:2, is incubated 30 minutes after furnace temperature being risen to 900 DEG C;
Step (3). in silica tube, pass into boron ammonia alkane steam simultaneously, close after 20 minutes and pass into boron ammonia alkane steam.The boron ammonia alkane steam passed into is obtained by heating in water bath, bath temperature 40 DEG C.
Step (4). electric furnace stops heating, and silica tube is cooled to normal temperature, and rate of cooling is 20 DEG C/min, then closes and passes into hydrogen and argon gas, take out copper sheet.
Step (5). taken out by copper sheet, copper sheet has two surfaces, is respectively upper surface A and lower surface B.With the aqueous solution soaking copper sheet upper surface A10 second of iron(ic) chloride, then use washed with de-ionized water.
Step (6). the copper sheet upper surface A that step (5) is obtained, coated with paraffin 0.1g.
The upper surface that step (6) obtains is had the copper sheet of carbon source by step (7), puts into the gas mixture that silica tube continues to pass into argon gas and hydrogen, and the throughput ratio of argon gas and hydrogen is 1:2, is incubated 5 minutes after furnace temperature being risen to 900 DEG C.
Step (8). electric furnace stops heating, and silica tube is cooled to normal temperature, and rate of cooling is 20 DEG C/min, then closes and passes into hydrogen and argon gas, take out copper sheet.
Step (9). copper sheet is taken out, at copper sheet lower surface B surface spin coating PMMA solution, PMMA solution forms PMMA film in atmosphere for dry 5 minutes and is attached on copper sheet surface, then immerse in ferric chloride Solution and remove copper sheet, to the PMMA film transfer on ferric chloride Solution surface be swum in silicon substrate surface afterwards, then silicon base is immersed in acetone, through 30 minutes, obtain the Graphene/boron nitride two dimension composite film material being transferred to silicon chip surface.
Embodiment 2:
Step (1). be that hydrochloric acid O.6mol/L embathes 9 seconds by cupronickel sheet concentration, dry up with nitrogen after washed with de-ionized water, put into the silica tube of electric furnace;
Step (2). continue the gas mixture passing into argon gas and hydrogen in silica tube, the throughput ratio of argon gas and hydrogen is 15:10, is incubated 20 minutes after furnace temperature being risen to 1000 DEG C.
Step (3). in silica tube, pass into boron ammonia alkane steam simultaneously, close after 30 minutes and pass into boron ammonia alkane steam; The boron ammonia alkane steam passed into is obtained by heating in water bath, bath temperature 100 DEG C.
Step (4). electric furnace stops heating, and silica tube is cooled to normal temperature, and rate of cooling is 30 DEG C/min, then closes and passes into hydrogen and argon gas, take out cupronickel sheet.
Step (5). taken out by cupronickel sheet, cupronickel sheet has two surfaces, is respectively upper surface A and lower surface B.By the aqueous solution soaking cupronickel sheet surface A 60 seconds of iron(ic) chloride, then use washed with de-ionized water.
Step (6). the cupronickel sheet upper surface A that step (5) is obtained, coating carbon dust 0.5g.
The upper surface that step (6) obtains is had the cupronickel sheet of carbon source by step (7), put into the gas mixture that silica tube continues to pass into argon gas and hydrogen, the throughput ratio of argon gas and hydrogen is 3:2, is incubated 30 minutes after furnace temperature being risen to 1000 DEG C.
Step (8). electric furnace stops heating, and silica tube is cooled to normal temperature, and rate of cooling is 30 DEG C/min, then closes and passes into hydrogen and argon gas, take out cupronickel sheet.
Step (9). cupronickel sheet is taken out, at cupronickel sheet lower surface B surface spin coating PMMA solution, PMMA solution forms PMMA film in atmosphere for dry 30 minutes and is attached on cupronickel sheet surface, then immerse in ferric chloride Solution and remove cupronickel sheet, to the PMMA film transfer on ferric chloride Solution surface be swum in silicon substrate surface afterwards, then silicon base is immersed in acetone, through 180 minutes, obtain the Graphene/boron nitride two dimension composite film material being transferred to silicon chip surface.
Embodiment 3:
Step (1). be that the hydrochloric acid of 1.5mol/L embathes 5 seconds by nickel sheet concentration, dry up with nitrogen after washed with de-ionized water, put into the silica tube of electric furnace;
Step (2). continue the gas mixture passing into argon gas and hydrogen in silica tube, the throughput ratio of argon gas and hydrogen is 3:2, is incubated 5 minutes after furnace temperature being risen to 950 DEG C.
Step (3). in silica tube, pass into boron ammonia alkane steam simultaneously, close after 25 minutes and pass into boron ammonia alkane steam.The boron ammonia alkane steam passed into is obtained by heating in water bath, bath temperature 60 DEG C.
Step (4). electric furnace stops heating, and silica tube is cooled to normal temperature, and rate of cooling is 25 DEG C/min, then closes and passes into hydrogen and argon gas, take out nickel sheet.
Step (5). nickel sheet taken out, nickel sheet has two surfaces, is respectively upper surface A and lower surface B.With the aqueous solution soaking nickel sheet upper surface A50 second of iron(ic) chloride, then use washed with de-ionized water.
Step (6). the nickel sheet upper surface A that step (5) is obtained, coated with paraffin 0.35g.
The upper surface that step (6) obtains is had the nickel sheet of carbon source by step (7), puts into the gas mixture that silica tube continues to pass into argon gas and hydrogen, and the throughput ratio of argon gas and hydrogen is 1:1, is incubated 26 minutes after furnace temperature being risen to 980 DEG C.
Step (8). electric furnace stops heating, and silica tube is cooled to normal temperature, and rate of cooling is 22 DEG C/min, then closes and passes into hydrogen and argon gas, take out nickel sheet.
Step (9). nickel sheet is taken out, at nickel sheet lower surface (B) surperficial spin coating PMMA solution, PMMA solution forms PMMA film in atmosphere for dry 16 minutes and is attached on nickel sheet surface, then immerse in ferric chloride Solution and remove nickel sheet, to the PMMA film transfer on ferric chloride Solution surface be swum in silicon substrate surface afterwards, then silicon base is immersed in acetone, through 90 minutes, obtain the Graphene/boron nitride two dimension composite film material being transferred to silicon chip surface.
Claims (4)
1. a preparation method for the heterogeneous phase composite film material of Graphene-boron nitride, it is characterized in that, the method concrete steps are:
Step (1), be that the hydrochloric acid of O.5 ~ 1.5mol/L embathes 5 ~ 10 seconds by tinsel concentration, dry up with nitrogen after washed with de-ionized water, put into the silica tube of electric furnace;
Continue the gas mixture passing into argon gas and hydrogen in step (2), silica tube, the throughput ratio of argon gas and hydrogen is 1 ~ 3:2, is incubated 5 ~ 30 minutes after furnace temperature being risen to 900 ~ 1000 DEG C.
Step (3), simultaneously in silica tube, pass into boron ammonia alkane steam, close after 20 ~ 30 minutes and pass into boron ammonia alkane steam.
Step (4), electric furnace stop heating, and silica tube is cooled to normal temperature, and rate of cooling is 20 ~ 30 DEG C/min, then close and pass into hydrogen and argon gas, take out tinsel.
Step (5), by tinsel take out, tinsel has two surfaces, is respectively upper surface and lower surface.By the aqueous solution soaking metallic upper surface 10 ~ 60 seconds of iron(ic) chloride, then use washed with de-ionized water.
Step (6), the tinsel upper surface that step (5) is obtained, coating carbon source 0.1 ~ 0.5g;
Step (7), the upper surface that step (6) obtains there is the tinsel of carbon source, put into the gas mixture that silica tube continues to pass into argon gas and hydrogen, the throughput ratio of argon gas and hydrogen is 5 ~ 15:10, is incubated 5 ~ 30 minutes after furnace temperature being risen to 900 ~ 1000 DEG C.
Step (8). electric furnace stops heating, and silica tube is cooled to normal temperature, and rate of cooling is 20 ~ 30 DEG C/min, then closes and passes into hydrogen and argon gas, take out tinsel.
Step (9). tinsel is taken out, at tinsel lower surface surface spin coating PMMA solution, PMMA solution forms PMMA film in atmosphere for dry 5 ~ 30 minutes and is attached on tinsel surface, then immerse in ferric chloride Solution to dissolve and remove tinsel, to the PMMA film transfer on ferric chloride Solution surface be swum in silicon substrate surface afterwards, then silicon base is immersed in acetone, through 30 ~ 180 minutes, obtain the Graphene-boron nitride two dimension composite film material being transferred to silicon chip surface.
2. the preparation method of the heterogeneous phase composite film material of a kind of Graphene-boron nitride as claimed in claim 1, is characterized in that: the metal of described tinsel is copper, nickel or cupronickel.
3. the preparation method of the heterogeneous phase composite film material of a kind of Graphene-boron nitride as claimed in claim 1, is characterized in that: described carbon source is paraffin or carbon dust.
4. the preparation method of the heterogeneous phase composite film material of a kind of Graphene-boron nitride as claimed in claim 1, is characterized in that: boron ammonia alkane steam is produced by heating in water bath boron ammonia alkane, bath temperature 40 ~ 100 DEG C.
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Cited By (8)
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| CN105908152A (en) * | 2016-04-29 | 2016-08-31 | 杭州电子科技大学 | Transfer method of hexagonal boron nitride film |
| CN106145103A (en) * | 2016-08-10 | 2016-11-23 | 中国人民大学 | A kind of preparation method of two-dimensional layer hetero-junctions based on Graphene |
| CN108841048A (en) * | 2018-06-08 | 2018-11-20 | 江苏嘉仁禾科技有限公司 | A kind of dedicated low smell in floor is without phenol calcium zinc stabilizer and preparation method thereof |
| CN110451498A (en) * | 2019-09-09 | 2019-11-15 | 吉林大学 | A kind of graphene-boron nitride nanosheet composite construction and preparation method thereof |
| CN110510604A (en) * | 2019-09-09 | 2019-11-29 | 吉林大学 | A kind of graphene/boron nitride stratiform heterojunction structure and preparation method thereof |
| CN112159970A (en) * | 2020-10-12 | 2021-01-01 | 哈尔滨工业大学 | Preparation method of wafer-level high-quality boron nitride/graphene heterojunction film |
| CN112186152A (en) * | 2020-09-21 | 2021-01-05 | 天元军融(辽宁)化工研究所新材料孵化器股份有限公司 | Method for absorbing terahertz waves to supplement electric quantity for battery and battery |
| CN114203326A (en) * | 2021-12-13 | 2022-03-18 | 中国核动力研究设计院 | Graphene-packaged ultrathin nickel-63 radiation source film and preparation method and application thereof |
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| CN105908152A (en) * | 2016-04-29 | 2016-08-31 | 杭州电子科技大学 | Transfer method of hexagonal boron nitride film |
| CN105908152B (en) * | 2016-04-29 | 2018-09-25 | 杭州电子科技大学 | A kind of transfer method of hexagonal boron nitride film |
| CN106145103A (en) * | 2016-08-10 | 2016-11-23 | 中国人民大学 | A kind of preparation method of two-dimensional layer hetero-junctions based on Graphene |
| CN106145103B (en) * | 2016-08-10 | 2018-06-26 | 中国人民大学 | A kind of preparation method of the two-dimensional layer hetero-junctions based on graphene |
| CN108841048A (en) * | 2018-06-08 | 2018-11-20 | 江苏嘉仁禾科技有限公司 | A kind of dedicated low smell in floor is without phenol calcium zinc stabilizer and preparation method thereof |
| CN110451498A (en) * | 2019-09-09 | 2019-11-15 | 吉林大学 | A kind of graphene-boron nitride nanosheet composite construction and preparation method thereof |
| CN110510604A (en) * | 2019-09-09 | 2019-11-29 | 吉林大学 | A kind of graphene/boron nitride stratiform heterojunction structure and preparation method thereof |
| CN110510604B (en) * | 2019-09-09 | 2022-11-18 | 吉林大学 | Graphene/boron nitride layered heterostructure and preparation method thereof |
| CN112186152A (en) * | 2020-09-21 | 2021-01-05 | 天元军融(辽宁)化工研究所新材料孵化器股份有限公司 | Method for absorbing terahertz waves to supplement electric quantity for battery and battery |
| CN112159970A (en) * | 2020-10-12 | 2021-01-01 | 哈尔滨工业大学 | Preparation method of wafer-level high-quality boron nitride/graphene heterojunction film |
| CN112159970B (en) * | 2020-10-12 | 2023-10-27 | 哈尔滨工业大学 | Preparation method of wafer-level high-quality boron nitride/graphene heterojunction film |
| CN114203326A (en) * | 2021-12-13 | 2022-03-18 | 中国核动力研究设计院 | Graphene-packaged ultrathin nickel-63 radiation source film and preparation method and application thereof |
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