CN103031516A - Preparation method of hexagonal phase boron nitride film - Google Patents
Preparation method of hexagonal phase boron nitride film Download PDFInfo
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- CN103031516A CN103031516A CN2013100199129A CN201310019912A CN103031516A CN 103031516 A CN103031516 A CN 103031516A CN 2013100199129 A CN2013100199129 A CN 2013100199129A CN 201310019912 A CN201310019912 A CN 201310019912A CN 103031516 A CN103031516 A CN 103031516A
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Abstract
The invention discloses a preparation method of a hexagonal phase boron nitride film. The preparation method comprises the following steps: by a physical vapor deposition method, providing boron atoms by a solid boron source, and forming the hexagonal phase boron nitride film on a substrate, wherein the deposition speed of physical vapor deposition is 0.01 nm/min-20 nm/min, and in the film forming process, the substrate temperature is controlled at 20-1600 DEG C; and the temperature is reduced to room temperature at a speed of 10-400 DEG C/min. when the hexagonal phase boron nitride film is prepared by the preparation method, the solid boron source is used, so that the safety is high, and the preparation method is simple, and easy to implement; the prepared hexagonal phase boron nitride film consists of 1-200 hexagonal phase boron nitride unit layers; and the two-dimensional hexagonal phase boron nitride film prepared by the preparation method has excellent insulating property and flatness and can be used for improving performance of a graphene optoelectronic device.
Description
Technical field
The present invention relates to a kind of preparation method of boron nitride pellicle, particularly a kind of preparation method of hexagonal phase boron nitride pellicle of the two dimension that adopts solid-state boron source growth.
Background technology
III-V compounds of group boron nitride (BN) is similar with the C of IV family, the existing sp that is similar to diamond lattic structure
3The phase that key consists of has again the sp that is similar to graphite-structure
2The phase that consists of.Have four kinds of main isomer, their this is not the cubic boron nitride (cubicboron nitride:c-BN), the six side's phase boron nitrides (wurtzite boron nitride:w-BN) with wurtzite structure corresponding to lonsdaleite, the hexagonal phase boron nitride (hexagonalboron nitride:h-BN) corresponding with hexagonal graphite, the rhombohedron boron nitride (rhombohedral boron nitride:r-BN) corresponding with tripartite rhombohedron structure graphite of the zincblende lattce structure corresponding with diamond.Wherein, h-BN and r-BN are the two-dimensional material of stratiform, are with sp between the boron nitrogen-atoms in same layer
2Bond is closed, and reactive force between layers is Van der Waals force; With sp between the boron nitrogen-atoms among w-BN and the c-BN
3Bond is closed, and different structure has determined that they have different character; Usually, only having h-BN and c-BN is stable phase.
Nano material comprises zero-dimension nano material, monodimension nanometer material and two-dimensional nano material, and nano material has the performances such as the photoelectricity different from the body material, chemistry, heat; One dimension and zero-dimension nano material have more than 20 year development history, and really the research of two-dimensional nano material are just carried out in recent years, particularly over 2004 years since the research to Graphene.The two-dimensional nano material mainly contains by the 4th main group element in the periodic table of elements and consists of laminar film such as Graphene (being comprised of carbon), silene (being comprised of element silicon) and germanium alkene (being comprised of element Ge), metal chalcogenide compound such as MoS
2, WS
2With GaS etc., and the stratified material such as hexagonal boron nitride.At present, studying more two-dimensional nano material is graphene film, is subjected to the impact of Graphene and special performance thereof research, and the two-dimensional film of other class Graphene also more and more receives investigator's concern.
Two dimension hexagonal phase boron nitride pellicle can improve performance of devices significantly because its excellent insulation characterisitic and planeness are used for the Graphene opto-electronic device.At present, the main method of the hexagonal phase boron nitride of preparation two dimension is chemical gaseous phase depositing process (CVD) [" Toward the controlled synthesisof hexagonal boron nitride films " ACS Nano 2012,6,6378], the CVD method is at a certain temperature with the nitrogenous and pure gas boron atom, perhaps contain respectively nitrogen and form the h-BN film with the decomposing gas that contains the boron atom at substrate, because boron-containing gas is obnoxious flavour, uses the CVD method to prepare two-dimentional hexagonal phase boron nitride pellicle and have potential safety hazard.
Publication number is that the Chinese patent literature of CN101913598A discloses a kind of employing physical vapor deposition (PVD) method such as thermal treatment, hot evaporation, sputter, electron beam deposition, laser deposition or plasma deposition discharge the technological method for preparing graphene film with carbon atom from solid-state carbon source.
Summary of the invention
For the deficiencies in the prior art, the object of the present invention is to provide a kind of simple to operate, be easy to realize, the method for the two-dimentional hexagonal phase boron nitride pellicle of preparation stratiform that security is good.
A kind of preparation method of hexagonal phase boron nitride pellicle adopts physical gas-phase deposite method, provides the boron atom by solid-state boron source, forms the hexagonal phase boron nitride pellicle at substrate; Sedimentation rate during physical vapor deposition is 0.01nm/min～20nm/min; The control underlayer temperature is 20～1600 ℃ in the film process, and the speed with 10～400 ℃/min is cooled to room temperature at last.
Adopt physical gas-phase deposite method, boron atomic radical and nitrogen-atoms group or boron nitride molecule are released into substrate, boron atomic radical and nitrogen-atoms group or boron nitride molecule are in substrate diffusion and film forming, here " group " not only refers to atom, also comprise other ion that contains this element etc., take nitrogen as example, comprise nitrogen-atoms, N
2 +, NH
3 +Deng.Boron atomic radical and the release of nitrogen-atoms group or boron nitride molecule and on substrate nucleating growth become orderly h-BN to need certain energy, these energy can also excite substrate to make substrate have certain catalysis, required energy can come from physical gas-phase deposite method itself, such as the particle beam (ionic fluid, electron beam, photon beam etc.) of the certain energy in the physical gas-phase deposite method etc., also can be by heating obtains to substrate.
Control h-BN is the key of controlled preparation h-BN or c-BN film with the phase co-conversion of c-BN, and this relates to the control of underlayer temperature and rate of temperature fall or to the energy of particle beam controls.The Basic Mechanism that adopts the standby c-BN film of PVD legal system of Assisted by Ion Beam often is that the h-BN film that will easily prepare makes h-BN be converted into c-BN by certain condition; Usually, high energy particle produces a large amount of heat energy such as boron ion, nitrogen ion and argon ion and substrate and existing boron nitride pellicle (amorphous or h-BN film) collision and temperature is improved rapidly and produces high pressure, and making film produce very large stress, this High Temperature High Pressure and large stress can make h-BN be converted into c-BN and obtain the c-BN film.Should stop h-BN to change to c-BN in order to prepare the h-BN film, this can be by realizing with lower sedimentation rate, to a certain extent, and the lower more low-energy particle flux of sedimentation rate meaning; Also can realize making heat, stress etc. in film, to discharge fast by the control to underlayer temperature and rate of temperature fall.Such as underlayer temperature being controlled at lower condition deposit boron nitride pellicle (the often hybrid films of amorphous boron nitride and h-BN), then be elevated to certain temperature and this hybrid films is heat-treated make it to form orderly h-BN film, cool the temperature to room temperature with certain rate of temperature fall at last; Perhaps in higher temperature deposit and form h-BN, then with certain rate of temperature fall cooling and suppress h-BN to the transformation of c-BN.Usually, under the High Temperature High Pressure, c-BN is more stable than h-BN.
The preparation method of hexagonal phase boron nitride pellicle of the present invention can be following steps:
(1) when 500 ℃～1600 ℃ underlayer temperature, on substrate, sedimentation rate is 0.01nm/min～20nm/min with boron atomic radical and nitrogen-atoms group or boron nitride molecule deposition;
(2) reduce the temperature to room temperature with 10 ℃/min of rate of temperature fall～400 ℃/min.
Preferably, the control underlayer temperature is 500～1200 ℃ in the film process, and sedimentation rate is 0.01nm/min～20nm/min, and the speed with 30～300 ℃/min is cooled to room temperature at last.The control underlayer temperature is 500～1200 ℃ in the film process, and the speed with 30～300 ℃/min is cooled to room temperature at last, forms easily the boron nitride pellicle of perfect pure hexagonal phase structure at substrate.
The preparation method of hexagonal phase boron nitride pellicle of the present invention can also comprise the steps:
(1) when 20 ℃～500 ℃ lower underlayer temperature, on substrate, sedimentation rate is 0.01nm/min～20nm/min with boron atomic radical and nitrogen-atoms group or boron nitride molecule deposition;
(2) substrate that deposits boron atomic radical and nitrogen-atoms group or boron nitride molecule is heat-treated at 500 ℃～1600 ℃;
(3) after the thermal treatment, reduce the temperature to room temperature with 10 ℃/min of rate of temperature fall～400 ℃/min.
Preferably, described heat treatment time is 1～180min.
Described substrate is Al, Ti, Cr, Mn, Fe, Co, Ni, Cu, Zr, Mo, Ru, Pd, Ta, W, Re, Pt, Mg, ZrB
2, SiC, Si, Ge, GaN, GaAs, SiO
2, BN, Si
3N
4, HfO
2, Al
2O
3, MgO, MoO
2, MoS
2, MoSe
2, MoTe
2, WO
2, WS
2, WSe
2, WTe
2, TiS
2, ZrS
2, SnO, SnS, SnSe, GeS, GeSe, SnS
2, SnSe
2, one or more the combination in GaS, GaSe, the graphene film.These substrate materials can be divided into metal, semi-conductor, isolator, can be three-dimensional also can be two-dimentional; Because the catalytic activity of substrate material is different, so can have influence on the height of required underlayer temperature to the selection of substrate.
Described physical gas-phase deposite method is one or more the combination in ion beam depositing, electron beam deposition, laser deposition, infrared heating deposition, sputtering sedimentation, hot vapor deposition, the molecular beam epitaxy deposition.Concrete which kind of physical gas-phase deposite method that adopts there is no strict demand, but generally speaking, physical vapor deposition carries out to ultrahigh vacuum(HHV) in rough vacuum; The air pressure that forms the h-BN film can be at normal pressure to ultrahigh vacuum(HHV).
Described solid-state boron source is one or both in boron, the boron nitride solid-state material.The powder that boron, boron nitride solid-state material can be comprised of shapes such as point, line, pieces, line, sheet, target etc. have difform solid-state material.The boron atom and the nitrogen-atoms that form the hexagonal phase boron nitride pellicle can come from solid-state boron source such as boron nitride, perhaps from solid-state boron source such as boron and nitrogenous gas, such as N
2And NH
3Deng.In a word, the inventive method prepares the hexagonal phase boron nitride pellicle, the boron source is solid material, has solved the problem that the harmful boron-containing gas of available technology adopting prepares the hexagonal phase boron nitride pellicle.
Preferably, when adopting described physical gas-phase deposite method to prepare the hexagonal phase boron nitride pellicle, pass at least a in nitrogen, the ammonia to deposition chambers.Owing to may there be the disappearance of N atom during preparation hexagonal phase boron nitride pellicle, in order to realize that better boron atom and nitrogen-atoms mol ratio are 1: 1 in the hexagonal boron nitride film, when preparation hexagonal boron nitride film, pass into nitrogenous gas to deposition chambers.In addition, physical gas-phase deposite method itself needs certain working gas, needs Ar, H during such as sputter
2, water vapour etc., the gas that passes into can also have other function, and the function of clean substrate etc. is arranged such as hydrogen.
For improving the electric property of hexagonal phase boron nitride pellicle, as preferably, the preparation method of hexagonal phase boron nitride pellicle of the present invention also comprises the hexagonal phase boron nitride pellicle mixed, and the atom of doping comprises one or more the combination among Be, C, Si, Ge, O, the S.The presoma of these foreign atoms or to be referred to as doped source can be gaseous state or solid-state.Usually with the doped source of gaseous state with pass into chamber after working gas mixes in gas mixing box; Solid-state doped source such as Si, C, Ge etc. produce foreign atom and are deposited on the substrate from solid-state doped source.
Described hexagonal phase boron nitride pellicle is comprised of 1～200 layer hexagonal phase boron nitride unit layer.
Be different from the CVD method, physical gas-phase deposite method of the present invention prepares the hexagonal phase boron nitride pellicle, adopts solid-state boron source, and security is good, the preparation method is simple, be easy to realization.The hexagonal phase boron nitride pellicle of the inventive method preparation is comprised of the hexagonal phase boron nitride unit layer of 1-200 layer, reactive force between layers is Van der Waals force, the two-dirnentional structure that described hexagonal phase boron nitride unit layer is formed by covalent linkage by boron atom and nitrogen-atoms.The two-dimentional hexagonal phase boron nitride pellicle that the present invention prepares has excellent insulation characterisitic and planeness, can be used for the Graphene opto-electronic device and improves device performance.
Description of drawings
Fig. 1 is the primary process synoptic diagram of preparation hexagonal phase boron nitride pellicle of the present invention;
Fig. 2 is the primary process synoptic diagram of the hexagonal phase boron nitride pellicle of preparation doping of the present invention;
Fig. 3 is the scanning electron microscope image of the hexagonal phase boron nitride pellicle of embodiment 1 preparation;
Fig. 4 is the Raman collection of illustrative plates of the hexagonal phase boron nitride pellicle of embodiment 2-5 preparation;
Wherein, curve a is the Raman collection of illustrative plates of hexagonal phase boron nitride pellicle of the individual layer of embodiment 2 preparation; Curve b is the Raman collection of illustrative plates of about 10 layers hexagonal phase boron nitride pellicle of embodiment 3 preparations; Curve
cRaman collection of illustrative plates for about 30 layers hexagonal phase boron nitride pellicle of embodiment 4 preparation; Curve d is the Raman collection of illustrative plates of about 100 layers hexagonal phase boron nitride pellicle of embodiment 5 preparations;
Fig. 5 is the Auger electron spectrum figure of about 200 layers hexagonal phase boron nitride pellicle of embodiment 6 preparations;
Fig. 6 is the Auger electron spectrum figure of about 10 layers carbon doping hexagonal phase boron nitride pellicle of embodiment 7 preparations.
Shown in the figure, 1: substrate; 2: gas; 3: solid-state boron source; 4: the hexagonal phase boron nitride pellicle; 5: doped source; 6: the hexagonal phase boron nitride pellicle of doping.
Embodiment
As shown in Figure 1, the preparation method of hexagonal phase boron nitride pellicle adopts physical gas-phase deposite method, in the atmosphere of gas 2, discharge boron atomic radical, nitrogen-atoms group or boron nitride molecule by solid-state boron source 3, form hexagonal phase boron nitride pellicle 4 by control sedimentation rate, temperature and rate of temperature fall at substrate 1.
As shown in Figure 2, the preparation method of the hexagonal phase boron nitride pellicle that mixes adopts physical gas-phase deposite method, in the atmosphere of gas 2, discharge boron atomic radical, nitrogen-atoms group or boron nitride molecule by solid-state boron source 3, and discharge foreign atom by doped source 5, form the hexagonal phase boron nitride pellicle 6 that mixes by control sedimentation rate, temperature and rate of temperature fall at substrate 1.
Solid-state boron source 3 is the solid material of boron or boron nitride, when solid-state boron source 3 is the solid material of boron, includes oxide gas in the gas 2.
Embodiment 1:
As shown in Figure 1, in 1 * 10
-8Under the base vacuum of Pa, adopt the method for electron beam deposition at copper sheet preparation hexagonal phase boron nitride pellicle.First in hydrogen atmosphere, copper sheet (a part among Fig. 1) was heat-treated 2 hours under 1000 ℃ the temperature; Then at N
2(operating air pressure is about 2 * 10 in the atmosphere of/Ar (50sccm/80sccm)
-2Pa), and when underlayer temperature is 850 ℃, be used to the electron beam evaporation boron powder from electron beam gun, evaporate boron atomic current (b part among Fig. 1) with 1.0nm/min speed; Keep identical temperature and atmospheric condition, thermal treatment 5 minutes (c part among Fig. 1), the rate of temperature fall with 200 ℃/min reduces the temperature to 20 ℃ at last, gets the hexagonal boron nitride film (the scanning electron microscope image is as shown in Figure 3) of number of plies inequality.
Embodiment 2:
In 1 * 10
-6Under the base vacuum of Pa, adopt the method for magnetron sputtering at graphene film/SiO
2Preparation hexagonal phase boron nitride pellicle on the substrate that/Si forms: be under 20 ℃ the condition, to pass into N in substrate temperature
2/ Ar (20sccm/50sccm), operating air pressure is approximately 10Pa, with the sputter rate sputter boron-nitride target of about 0.01nm/min; Then in identical atmosphere, temperature is risen to 1100 ℃, processed 45 minutes; Rate of temperature fall with 400 ℃/min cools the temperature to 20 ℃ at last, thereby obtains the hexagonal phase boron nitride pellicle (Raman spectrum is shown in curve a among Fig. 4) of individual layer at graphene film.
Embodiment 3:
In 2 * 10
-6Under the base vacuum of Pa, adopt the method for magnetron sputtering at Ni/Al
2O
3Preparation hexagonal phase boron nitride pellicle on the substrate that forms: at NH
3/ Ar (20sccm/100sccm) operating air pressure is approximately in the 100Pa atmosphere, is under 880 ℃ the condition, with the sputter rate Boron Sputtered target of about 0.6nm/min in substrate temperature; Then the rate of temperature fall with 150 ℃/min cools the temperature to 20 ℃, thereby obtains about 10 layers hexagonal phase boron nitride pellicle (Raman spectrum is shown in curve b among Fig. 4) at Graphene.
Embodiment 4:
As shown in Figure 1, in 4 * 10
-9Under the base vacuum of Pa, adopt infrared heating deposition and ion beam technology method to prepare the hexagonal phase boron nitride pellicle in the Fe-Co alloy substrate: take the solid boron source of boron powder as growth hexagonal phase boron nitride pellicle, be under 850 ℃ at underlayer temperature, utilize infrared beams with the vaporator rate evaporation boron powder of about 8nm/min; Pass into simultaneously N
2(30sccm), and with Ar (30sccm) ion gun with N
2Ionization; Then pass into N
2/ H
2(10sccm/100sccm), thermal treatment is 5 minutes when temperature is 1000 ℃, then cools to 20 ℃ with 100 ℃/min of rate of temperature fall, thereby obtains about 30 layers silene film 4 (Raman spectrum is shown in curve c among Fig. 4).
Embodiment 5:
In 2 * 10
-5Under the base vacuum of Pa, adopt the method for laser deposition to prepare the hexagonal phase boron nitride pellicle at the Si substrate: at NH
3(22sccm) under the atmosphere, take the solid boron source of boron nitride powder as growth hexagonal phase boron nitride pellicle, be under 1200 ℃ at underlayer temperature, utilize laser beam evaporation boron nitride powder (sedimentation rate is 15nm/min); Then cool to 20 ℃ with 50 ℃/min of rate of temperature fall, thereby obtain 100 layers silene film 4 (Raman spectrum is shown in curve d among Fig. 4).
In 1 * 10
-4Under the base vacuum of Pa, adopt the method for hot evaporation at HfO
2(30mm)/the Si substrate on preparation hexagonal phase boron nitride pellicle: take boron nitride powder as solid boron source, be under 20 ℃ at underlayer temperature, thermal evaporation boron nitride powder (sedimentation rate is 20nm/min); Then pass into N
2(100sccm), thermal treatment is 60 minutes when temperature is 1600 ℃, then cools to 20 ℃ with 10 ℃/min of rate of temperature fall, obtains about 200 layers hexagonal phase boron nitride pellicle (Auger electron spectrum as shown in Figure 5).
Embodiment 7: the hexagonal phase boron nitride pellicle that preparation carbon mixes
As shown in Figure 2, in 1 * 10
-10Under the base vacuum of Pa, adopt molecular beam epitaxy technique to prepare the hexagonal phase boron nitride pellicle at the GaN substrate: when temperature is 970 ℃, utilize electron beam that the boron atom is discharged from the boron powder, the control film deposition rate is 3nm/min; Simultaneously at H
2/ N
2Under the atmosphere of/Ar (200sccm/5sccm/120sccm), adopt magnetron sputtering technique, will carbon atom be discharged from the carbon target with sputter rate 0.05nm/min, like this, B, N and C atom together are deposited on (b part among Fig. 2) on the GaN substrate; Then at H
2/ N
2Under the atmosphere (80sccm/18sccm) in 1150 ℃ of thermal treatments 120 minutes; Be down to room temperature with the rate of temperature fall of 50 ℃/min at last and obtain the hexagonal phase boron nitride pellicle (c part among Fig. 2) that about 10 layers carbon mixes.(Auger electron spectrum as shown in Figure 6).
Claims (9)
1. the preparation method of a hexagonal phase boron nitride pellicle is characterized in that, adopts physical gas-phase deposite method, provides the boron atom by solid-state boron source, forms the hexagonal phase boron nitride pellicle at substrate; The sedimentation rate of physical vapor deposition is 0.01nm/min～20nm/min; The control underlayer temperature is 20～1600 ℃ in the film process, and the speed with 10～400 ℃/min is cooled to room temperature at last.
2. the preparation method of hexagonal phase boron nitride pellicle as claimed in claim 1 is characterized in that, the control underlayer temperature is 500～1200 ℃ in the film process, and the speed with 30～300 ℃/min is cooled to room temperature at last.
3. the preparation method of hexagonal phase boron nitride pellicle as claimed in claim 1 is characterized in that, comprises the steps: in the described film process
(1) when 20 ℃～500 ℃ lower underlayer temperature, on substrate, sedimentation rate is 0.01nm/min～20nm/min with boron atomic radical and nitrogen-atoms group or boron nitride molecule deposition;
(2) substrate that deposits boron atomic radical and nitrogen-atoms group or boron nitride molecule is heat-treated at 500 ℃～1600 ℃;
(3) after the thermal treatment, reduce the temperature to room temperature with 10 ℃/min of rate of temperature fall～400 ℃/min.
4. the preparation method of hexagonal phase boron nitride pellicle as claimed in claim 3 is characterized in that, the heat treatment time of described step (2) is 1～180min.
5. the preparation method of hexagonal phase boron nitride pellicle as claimed in claim 1, it is characterized in that described physical gas-phase deposite method is one or more the combination in ion beam depositing, electron beam deposition, laser deposition, infrared heating deposition, sputtering sedimentation, hot vapor deposition, the molecular beam epitaxy deposition.
6. the preparation method of hexagonal phase boron nitride pellicle as claimed in claim 1 is characterized in that, described solid-state boron source is one or both in boron, the boron nitride solid-state material.
7. such as the preparation method of claim 1 or 5 described hexagonal phase boron nitride pellicles, it is characterized in that, when adopting described physical gas-phase deposite method to prepare the hexagonal phase boron nitride pellicle, pass at least a in nitrogen, the ammonia to deposition chambers.
8. the preparation method of hexagonal phase boron nitride pellicle as claimed in claim 1 is characterized in that, also comprises the hexagonal phase boron nitride pellicle is mixed, and the atom of doping comprises one or more the combination among Be, C, Si, Ge, O, the S.
9. the hexagonal phase boron nitride pellicle of the method for claim 1 preparation is characterized in that described hexagonal phase boron nitride pellicle is comprised of 1～200 layer hexagonal phase boron nitride unit layer.
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| CN104060322A (en) * | 2014-06-05 | 2014-09-24 | 南京航空航天大学 | Preparation method for thick hexagonal boron nitride single crystal with large-size atom layer |
| CN104313684A (en) * | 2014-09-30 | 2015-01-28 | 中国科学院半导体研究所 | Method for preparing hexagonal boron nitride (h-BN) two-dimensional atomic crystal |
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| CN104060322A (en) * | 2014-06-05 | 2014-09-24 | 南京航空航天大学 | Preparation method for thick hexagonal boron nitride single crystal with large-size atom layer |
| CN104313684A (en) * | 2014-09-30 | 2015-01-28 | 中国科学院半导体研究所 | Method for preparing hexagonal boron nitride (h-BN) two-dimensional atomic crystal |
| CN105984858A (en) * | 2015-01-27 | 2016-10-05 | 中国科学院苏州纳米技术与纳米仿生研究所 | Self-supporting boron nitride nano sheet flexible thin film and preparation method thereof |
| CN105483646A (en) * | 2016-01-20 | 2016-04-13 | 杭州电子科技大学 | Preparing method for ultraviolet absorbing thin film |
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