CN107964680A - A kind of method for preparing individual layer hexagonal boron nitride large single crystal - Google Patents
A kind of method for preparing individual layer hexagonal boron nitride large single crystal Download PDFInfo
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- CN107964680A CN107964680A CN201610916379.XA CN201610916379A CN107964680A CN 107964680 A CN107964680 A CN 107964680A CN 201610916379 A CN201610916379 A CN 201610916379A CN 107964680 A CN107964680 A CN 107964680A
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
- C30B25/02—Epitaxial-layer growth
- C30B25/18—Epitaxial-layer growth characterised by the substrate
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/40—AIIIBV compounds wherein A is B, Al, Ga, In or Tl and B is N, P, As, Sb or Bi
- C30B29/403—AIII-nitrides
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- C—CHEMISTRY; METALLURGY
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- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
- C30B29/64—Flat crystals, e.g. plates, strips or discs
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Abstract
The invention discloses a kind of method for preparing large single crystal hexagonal boron nitride.This method includes：Using the compound containing boron element and nitrogen as raw material, chemical vapor deposition is carried out on substrate, and deposition finishes to obtain the individual layer hexagonal boron nitride monocrystalline；Also contain foamed material in the system of the chemical vapor deposition.By this method can simply, efficiently, the large single crystal hexagonal boron nitride that high quality is prepared in metal substrate surface of environmental protection, and large single crystal hexagonal boron nitride is obtained on platinized platinum surface by the method first.
Description
Technical field
The invention belongs to Material Field, is related to a kind of method for preparing individual layer hexagonal boron nitride large single crystal.
Background technology
Hexagonal boron nitride (h-BN), have atomic structure similar to graphene New Two Dimensional material, its lattice coefficient with
Graphene is close (lattice mismatch rate is only 1.8%), is a kind of ultra-thin insulating materials (energy gap is about 5.9eV).It is gathered around
Have an atomically flat surface and less surface dangling bonds, thus its as graphene or molybdenum disulfide etc., other two dimensions are partly led
During the substrate of body material, mutually more conventional SiO2/ Si substrates can significantly improve graphene or other two-dimensional semiconductor materials
Carrier mobility.In addition, h-BN is also excellent with higher thermal conductivity, mechanical strength, chemistry and heat endurance and light transmittance etc.
Heterogeneity, therefore it also has wide application in the thermal control of micro-nano device, protective coating and dark purple external transmitter etc.
Prospect.Therefore, prepare high quality, monocrystalline h-BN in uniform thickness be the investigation of materials, using so commercialized foundation stone.Mesh
The preceding technology for preparing large single crystal h-BN, is to carry out electrification to copper foil before growth using method mainly using copper foil as substrate
Optical polishing, or extend annealing time (6h) during growth, to suppress the nucleation density of h-BN, so as to obtain big monocrystalline h-BN.This
A little methods, although the monocrystalline size of h-BN can be improved effectively, but have that cost is higher, efficiency is low and processing procedure has
The shortcomings of pollution waste water (polishing fluid) produces.In addition, apart from copper, platinized platinum is also h- due to the advantages of its is reusable
Common substrate prepared by BN two-dimensional materials.It is stronger yet with the catalytic activity of platinized platinum, h-BN in platinized platinum surface nucleation density very
Height, it is only poor in nano-scale, crystal quality to obtain monocrystalline size.There has been no be reported on platinized platinum substrate to prepare greatly at present
Monocrystalline h-BN, this compares copper foil with platinized platinum has high chemical stability, is not easy to be processed by shot blasting related, therefore uses routine techniques
It is difficult to the h-BN of large single crystal is prepared on platinized platinum.
The content of the invention
The object of the present invention is to provide a kind of method for preparing individual layer hexagonal boron nitride large single crystal.
The method provided by the invention for preparing individual layer hexagonal boron nitride monocrystalline, includes the following steps：
Using the compound containing boron element and nitrogen as raw material, chemical vapor deposition is carried out on substrate, and deposition finishes
To the individual layer hexagonal boron nitride monocrystalline；
Also contain foamed material in the system of the chemical vapor deposition.
In the above method, the position relationship of the foamed material and the substrate is the various position relationships that can be realized,
It is not particularly limited；The position relationship concretely vertical pile, be placed in parallel or front and rear placement.The position relationship is
During front and rear placement, the foamed material can be placed in air-flow upstream end, or the substrate is placed in air-flow upstream end；
Chemical vapor deposition is carried out using the above method, individual layer hexagonal boron nitride monocrystalline can be deposited closer to the foam material
On the substrate surface of material.
The method may also include the steps of：Before the chemical vapor deposition step, by the substrate and foam
Material is placed in the container of half opening.
In this case, individual layer hexagonal boron nitride monocrystalline can be deposited on the upper and lower surface of the substrate；The foamed material
Position relationship with the substrate is the various position relationships that can be realized, is not particularly limited；The position relationship is specific
It can be vertical pile, be placed in parallel or front and rear placement.Specifically, when the position relationship is placed for before and after, can be by the foam
Material is placed in air-flow upstream end, or the substrate is placed in air-flow upstream end.
The material for forming the substrate is transition metal, is specially that platinum, copper, nickel, iron, corronil etc. have catalytic performance
Transition metal or alloy；
The foamed material has molten for nickel foam, foam copper or foamed iron etc. containing high-specific surface area and to boron or nitrogen
The material of Xie Du；
The aperture of the foamed material is 0.1mm-1mm；
PPI (namely per inch hole count) is 50-120；
Porosity is 70%-98%.
The raw material be selected from it is following any one：
1) ammonia borine；
2) borazine；
3) diborane and ammonia；
4) halogenation boron and ammonia.
The halogenation boron is boron chloride, boron fluoride or boron bromide.
In the chemical vapor deposition step, carrier gas is hydrogen；
The flow velocity of carrier gas is 10sccm-30sccm, is specially 10sccm；
The flow velocity of gaseous feed is 2-100sccm, is specially 5sccm；
When raw materials used for borazine, diborane, ammonia or during halogenation boron, since it is in chemical gaseous phase of the present invention
It is gaseous state in itself under depositing temperature, therefore its gaseous flow rate can be easily carried out；
For it is raw materials used be ammonia borine when, in order to obtain the gaseous flow rate of the raw material, first raw material can be heated by room temperature
To 75 DEG C so that ammonia borine brings it into reaction zone by carrier gas again after decomposing can proceed by chemical vapor deposition.
System pressure is 14Pa-44Pa, is specially 14Pa or 16Pa；
Depositing temperature is 1030 DEG C -1100 DEG C, is specially 1050 DEG C；
Sedimentation time is 30min-75min, is specially 30min.
It is 10min by the time of chemical vapor deposition greenhouse cooling to room temperature.
The method further includes following steps：Before the chemical vapour deposition reaction, first system is annealed.
In the annealing steps, annealing temperature is 1030 DEG C -1100 DEG C, is specially 1050 DEG C；
Annealing time is 10min-75min, is specially 30min；
The time that annealing temperature is risen to by room temperature is 20-60min, is specially 30min.
The annealing steps can arrange the Pt surface topographies of substrate, can increase the crystallite dimension of substrate relatively,
It is more advantageous to the growth of h-BN.
The length of the individual layer hexagonal boron nitride monocrystalline longest edge is 15-100 μm.
The method provided by the invention for preparing individual layer hexagonal boron nitride monocrystalline, without changing other conditions, without to substrate
It is processed by shot blasting, is simply simply placed around one piece of foamed material such as nickel foam in growth substrates, can effectively reduce
Nucleation densities of the h-BN in growth substrates, so as to improve the monocrystalline size of h-BN, has the advantages that low cost, low stain；It is logical
Cross this method can simply, efficiently, environmental protection prepare the large single crystal hexagonal boron nitride of high quality in metal substrate surface, and adopt
Realize the large single crystal h-BN that hundred micron levels are prepared on platinized platinum first with this method.
Brief description of the drawings
Growth substrates and the foamed material that Fig. 1 is the present invention place pictorial diagram, and a) figure is copper sheet and nickel foam stacked configuration,
B) figure is substrate and foam material structure figure in half opening quartz ampoule.
Fig. 2 is the SEM image of the h-BN obtained in the embodiment of the present invention 1 at 1050 DEG C in copper foil surface, it is a) still
Foam nickel group, b) have copper foil surface of the nickel foam group towards nickel foam, c) large single crystal that the time obtains is appropriately extended under the conditions of this；Mark
Ruler length is respectively 5 μm, 5 μm, 10 μm.
Fig. 3 be the embodiment of the present invention 2 at 1050 DEG C Pt pieces surface obtain h-BN SEM image, a) non-foam
Nickel group, b) there is nickel foam group；Length of the scale is 10 μm.
The image being transferred on copper mesh for the h-BN samples that Fig. 4 prepares for the embodiment of the present invention 2, a) SEM image, b)
TEM image, c) selective electron diffraction (SAED) figure, d) TEM image, e) selective electron diffraction (SAED) figure.
Fig. 5 is the N1s spectrums in the x-ray photoelectron spectroscopy (XPS) of h-BN samples prepared by the present invention.
Fig. 6 is the B1s spectrums in the x-ray photoelectron spectroscopy (XPS) of h-BN samples prepared by the present invention.
Embodiment
With reference to specific embodiment, the present invention is further elaborated, but the present invention is not limited to following embodiments.Institute
It is conventional method unless otherwise instructed to state method.The raw material can be obtained from open commercial sources unless otherwise instructed.
Embodiment 1,
Experimental procedure
1st, the copper foil and nickel foam of suitable dimension are cut；Wherein, the aperture of nickel foam is 0.1mm；
PPI is 120；Porosity is 98%；
2nd, copper foil and nickel foam are cleaned with ammonium persulfate, deionized water and alcohol successively；
Cleaned copper foil is directly stacked in above nickel foam (such as Fig. 1 a)；In addition one group of copper for being free of nickel foam is prepared
Paper tinsel is as a control group；
3rd, the ammonia borine of 5mg is held by the use of quartz boat as growth raw material, is put together with the two groups of substrates prepared in step 2
Enter two regions into tube furnace, wherein, ammonia borine is placed in source region, and two groups of substrates are placed in reaction zone；
4th, tubular type furnace system is closed, opens mechanical pump, after system vacuum is evacuated to 0.2Pa, the hydrogen for being passed through 10sccm is (whole
A preparation process is passed through the hydrogen of this flow all the time), system pressure rises to 14Pa at this time, and at the same time by the temperature of reaction zone by room
Temperature rises to 1050 DEG C, and be kept at this temperature to two groups of substrate annealing 30min so that the crystal grain of metal substrate in 30min
Size increases, and is conducive to the growth of h-BN；
5th, after the completion of annealing, the temperature of reaction zone is continually maintained in 1050 DEG C, while source region temperature is heated to by room temperature
75 DEG C, ammonia borine is resolved into gaseous borazine, bringing it into reaction zone by the carrier gas hydrogen that flow velocity is 10sccm
Carry out chemical vapor deposition；
6th, depositing temperature is 1050 DEG C, after time 30min, in source region and reaction zone temperature are down to room temperature in 10min,
It is 10sccm that hydrogen flow rate is remained during this；
7th, two groups of substrates are taken out, its surface topography are observed with scanning electron microscope (SEM), as a result such as Fig. 3 institutes
Show.
Interpretation of result：
Pass through Fig. 2, it can be clearly seen that, the nucleation density of a figures in picture will be far above b and scheme, this is illustrated, nickel foam
Nucleation densities of the h-BN in copper foil surface can be substantially reduced, so as to go out in this copper foil Grown compared with large single crystal h-BN.
Therefore, the h-BN compared with large single crystal has been obtained by adjusting condition, appropriate extension growth temperature, monocrystalline size is~15 μm of (figures
2c), though the size is not current maximum, it is more economically environmentally friendly that other methods are compared.
In addition, according to the step identical with the embodiment, nickel foam is only replaced with into parallel put with platinized platinum by vertical pile
Put, front and rear place (is specially that nickel foam is placed in air-flow upstream, or copper foil is placed in air-flow upstream, acquired results and a in Fig. 2
Figure, c figures and Fig. 3 have no essential distinction, repeat no more.
Embodiment 2
Experimental procedure
Such as embodiment 1, processing nickel foam, platinized platinum, will be positioned in the small quartz ampoule of half opening before and after nickel foam and platinized platinum
(such as Fig. 1 b), and nickel foam is placed in air-flow upstream end, prepares containing nickel foam and two groups of substrates without nickel foam, and by this two groups
Substrate is put into the reaction zone of tube furnace；Wherein, the aperture of nickel foam is 0.1mm；PPI is 120；Porosity 98%；
Tubular type furnace system is closed, opens mechanical pump, after system vacuum is evacuated to 0.2Pa, the hydrogen for being passed through 10sccm is (whole
Preparation process is passed through the hydrogen of this flow all the time), system pressure rises to 14Pa at this time, and at the same time by the temperature of reaction zone by room temperature
In 30min, 1050 DEG C are risen to, and is kept at this temperature to two groups of substrate annealing 30min so that the crystal grain ruler of metal substrate
Very little increase, is more easy to the growth of h-BN；
After the completion of annealing, keep the hydrogen of 1050 DEG C of reaction zone temperature and 10sccm flows constant, be passed through the gas of 5sccm
State borazine (gas vacuum rises to 16Pa at this time), carries out chemical vapor deposition；
Depositing temperature is 1050 DEG C, time 30min, in reaction temperature is down to room temperature in 10min, and is begun in the process
Keep hydrogen and borazine flow velocity constant eventually；
Two groups of substrates are taken out, its pattern are observed with SEM, the results are shown in Figure 3.
Interpretation of result
Pass through Fig. 3, it can be clearly seen that, the nucleation density of a figures in picture will be far above b and scheme, this illustrates nickel foam
Nucleation densities of the h-BN on platinized platinum surface can be substantially reduced, it is larger so as to be grown in the upper and lower surface of this platinized platinum substrate
Monocrystalline h-BN.Therefore, by adjusting condition, appropriate extension growth temperature, has obtained the h-BN compared with large single crystal.To determine monocrystalline
Size, after transferring the sample on TEM grid, by TEM image and SAED images (such as Fig. 4), it can be found that in 100 μm of rulers
In the range of degree, the angle of diffraction spot is consistent, this explanation this method can prepare the h-BN monocrystalline of hundred micron levels.
According to the step identical with the embodiment, replaced with only by the position relationship of nickel foam and platinized platinum by front and rear placement flat
Row is placed or vertical pile, and acquired results, without substantive difference, are repeated no more with a figures and Fig. 4 in Fig. 3.
Above-described embodiment 1-2 prepare sample xps energy spectrum as shown in Figure 5,6, in two figures spectrum peak position be respectively~
396.55eV and~189.99eV, meets the XPS standard values of h-BN, and the ratio of two kinds of elements is B:N=1.09, proves this hair
The product of bright preparation is h-BN crystal, namely individual layer hexagonal boron nitride monocrystalline.
Claims (10)
1. a kind of method for preparing individual layer hexagonal boron nitride monocrystalline, includes the following steps：
Using the compound containing boron element and nitrogen as raw material, chemical vapor deposition is carried out on substrate, and deposition finishes to obtain institute
State individual layer hexagonal boron nitride monocrystalline；
Also contain foamed material in the system of the chemical vapor deposition.
2. according to the method described in claim 1, it is characterized in that：The position relationship of the foamed material and the substrate is vertical
Directly stack, be placed in parallel or front and rear placement.
3. method according to claim 1 or 2, it is characterised in that：The method further includes following steps：In the chemistry
Before vapor deposition step, the substrate and foamed material are placed in the container of half opening.
4. according to any method in claim 1-3, it is characterised in that：Form the material of the substrate for platinum, copper,
Nickel, iron or corronil；
The foamed material is nickel foam, foam copper or foamed iron；
The aperture of the foamed material is 0.1mm-1mm；
PPI is 50-120；
Porosity is 70%-98%.
5. according to any method in claim 1-4, it is characterised in that：The raw material be selected from it is following any one：
1) ammonia borine；
2) borazine；
3) diborane and ammonia；
4) halogenation boron and ammonia；
The halogenation boron is specially boron chloride, boron fluoride or boron bromide.
6. according to any method in claim 1-5, it is characterised in that：In the chemical vapor deposition step, carrier gas
For hydrogen；
The flow velocity of carrier gas is 10sccm-30sccm, is specially 10sccm；
The flow velocity of gaseous feed is 5-20sccm, is specially 5sccm；
System pressure is 14Pa-44Pa, is specially 14Pa or 16Pa；
Depositing temperature is 1030 DEG C -1100 DEG C, is specially 1050 DEG C；
Sedimentation time is 30min-75min, is specially 30min.
7. according to any method in claim 1-6, it is characterised in that：By chemical vapor deposition greenhouse cooling to room temperature
Time be 10min.
8. according to any method in claim 1-7, it is characterised in that：The method further includes following steps：
Before the chemical vapour deposition reaction, first system is annealed.
9. according to the method described in claim 8, it is characterized in that：In the annealing steps, annealing temperature is 1030 DEG C -1100
DEG C, it is specially 1050 DEG C；
Annealing time is 30min-75min, is specially 30min；
The time that annealing temperature is risen to by room temperature is 20-60min or 30min.
10. according to any method in claim 1-9, it is characterised in that：The individual layer hexagonal boron nitride monocrystalline is most long
The length on side is 15-100 μm.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110055589A (en) * | 2018-05-17 | 2019-07-26 | 南方科技大学 | Large-size single-layer hexagonal boron nitride single crystal or film and preparation method thereof |
| CN110616454A (en) * | 2019-03-07 | 2019-12-27 | 北京大学 | Method for vertical heteroepitaxy monocrystal metal film based on monocrystal two-dimensional material/monocrystal copper |
| CN111826712A (en) * | 2019-04-15 | 2020-10-27 | 中国科学院化学研究所 | Method for preparing wafer-level uniform hexagonal boron nitride film |
| CN113148997A (en) * | 2021-06-01 | 2021-07-23 | 大连理工大学 | Large-area thickness-controllable two-dimensional material nanosheet and general preparation method thereof |
| CN113380603A (en) * | 2021-05-18 | 2021-09-10 | 厦门大学 | High-boron-component two-dimensional III-group multi-element nitride mixed crystal and preparation method thereof |
| CN115613130A (en) * | 2022-08-29 | 2023-01-17 | 海南大学 | Method for preparing hexagonal boron nitride film by chemical vapor deposition under normal pressure |
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| CN1717508A (en) * | 2003-07-31 | 2006-01-04 | Si晶体股份公司 | Method and device for AIN single crystal production with gas-permeable crucible walls |
| CN104129763A (en) * | 2014-06-12 | 2014-11-05 | 南京航空航天大学 | Preparation method of large-grain single-layer hexagonal boron nitride |
| US20150059641A1 (en) * | 2013-09-04 | 2015-03-05 | Nitride Solutions, Inc. | Bulk diffusion crystal growth process |
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| CN1717508A (en) * | 2003-07-31 | 2006-01-04 | Si晶体股份公司 | Method and device for AIN single crystal production with gas-permeable crucible walls |
| US20150059641A1 (en) * | 2013-09-04 | 2015-03-05 | Nitride Solutions, Inc. | Bulk diffusion crystal growth process |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110055589A (en) * | 2018-05-17 | 2019-07-26 | 南方科技大学 | Large-size single-layer hexagonal boron nitride single crystal or film and preparation method thereof |
| CN110616454A (en) * | 2019-03-07 | 2019-12-27 | 北京大学 | Method for vertical heteroepitaxy monocrystal metal film based on monocrystal two-dimensional material/monocrystal copper |
| CN111826712A (en) * | 2019-04-15 | 2020-10-27 | 中国科学院化学研究所 | Method for preparing wafer-level uniform hexagonal boron nitride film |
| CN113380603A (en) * | 2021-05-18 | 2021-09-10 | 厦门大学 | High-boron-component two-dimensional III-group multi-element nitride mixed crystal and preparation method thereof |
| CN113148997A (en) * | 2021-06-01 | 2021-07-23 | 大连理工大学 | Large-area thickness-controllable two-dimensional material nanosheet and general preparation method thereof |
| US11572279B2 (en) | 2021-06-01 | 2023-02-07 | Dalian University Of Technology | Two-dimensional material nanosheets with large area and controllable thickness and general preparation method therefor |
| CN115613130A (en) * | 2022-08-29 | 2023-01-17 | 海南大学 | Method for preparing hexagonal boron nitride film by chemical vapor deposition under normal pressure |
| CN115613130B (en) * | 2022-08-29 | 2024-06-04 | 海南大学 | Method for preparing hexagonal boron nitride film by chemical vapor deposition under normal pressure |
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