CN116103609A - Preparation method of hexagonal boron nitride heterostructure - Google Patents

Preparation method of hexagonal boron nitride heterostructure Download PDF

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CN116103609A
CN116103609A CN202111335874.9A CN202111335874A CN116103609A CN 116103609 A CN116103609 A CN 116103609A CN 202111335874 A CN202111335874 A CN 202111335874A CN 116103609 A CN116103609 A CN 116103609A
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boron nitride
hexagonal boron
dielectric substrate
diamond
nitride heterostructure
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张兴旺
陈镜壬
王高凯
尹志岗
吴金良
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Abstract

The disclosure provides a preparation method of a hexagonal boron nitride heterostructure, comprising: s1, heating a dielectric substrate, and introducing ammonia gas into a deposition chamber; s2, sputtering a boron nitride target material by an ion source, and depositing the obtained nitrogen and boron atoms on a dielectric substrate for growth; s3, cooling to obtain the hexagonal boron nitride heterostructure. According to the preparation method disclosed by the invention, the ideal stoichiometric ratio of hexagonal boron nitride is ensured by introducing ammonia gas into the auxiliary gas path, and the growth of low-temperature hexagonal boron nitride is realized; and the direct growth of hexagonal boron nitride on the dielectric substrate is realized, the transfer process is avoided, the original property change of the dielectric substrate such as graphitization transformation of diamond at a higher growth temperature is avoided, and the method has very important significance for the application of electron and optoelectronics of the hexagonal boron nitride diamond heterostructure.

Description

Preparation method of hexagonal boron nitride heterostructure
Technical Field
The disclosure relates to the technical field of semiconductor material preparation, in particular to a preparation method of a hexagonal boron nitride heterostructure.
Background
The hexagonal boron nitride and the diamond belong to ultra-wide band-gap semiconductors, and compared with gallium nitride and silicon carbide, the hexagonal boron nitride and the diamond have larger band-gap width and higher breakdown field intensity, and have outstanding application prospects in the field of high-power and high-efficiency power electronic devices. In addition, the photoelectric device has obvious advantages in the aspect of short-wavelength photoelectric devices.
Hexagonal boron nitride is a layered material in which boron and nitrogen atoms pass through sp 2 The hybridization forms covalent bonds to form a honeycomb structure, van der Waals force acts between layers, and boron atoms correspond to nitrogen atoms in adjacent atomic layers to form A-A' stacks. The hexagonal boron nitride has similar properties as graphite with lamellar material, such as extremely high in-plane elastic modulus, high thermal conductivity, chemical stability and the like, but unlike graphite, electrons of hexagonal boron nitride are firmly bound around boron and nitrogen atoms due to the action of polar covalent bonds, so that the hexagonal boron nitride has good insulativity, high breakdown field strength and high forbidden band width of 5.97eV. In theory, no dangling bond exists at the hexagonal boron nitride interface, and the hexagonal boron nitride has very few charge traps, and has wide application prospect as a protective layer, a gate dielectric layer or a substrate material of other two-dimensional and three-dimensional materials because of the stable chemical property.
Diamond is a three-dimensional material in which carbon atoms are arranged in a diamond structure, the carbon atoms pass through sp 3 The hybridization forms a regular tetrahedral structure, valence electrons are bound around carbon atoms, the device has good insulativity, the forbidden bandwidth is as high as 5.4eV, the mobility of theoretical carriers is high, and the current method for forming two-dimensional hole gas on the surface by using the hydrogen-terminated diamond has great value in device application because the diamond doping is in an experimental stage. The stability of the hydrogen terminal is poor, and the stability of the hydrogen terminal diamond can be improved by using hexagonal boron nitride as a protective layer, so that the service life of a carrier is prolonged, and the performance of a device is further improved. In addition, the hexagonal boron nitride and the diamond have good development prospect in the field of deep ultraviolet photoelectric devices.
The hexagonal boron nitride band gap is larger than that of diamond, and has a larger breakdown electric field, when the heterostructure is formed to prepare an electronic or photoelectric device, the hexagonal boron nitride is mostly used as a cover layer of the diamond, so that the preparation of high-quality hexagonal boron nitride on a diamond medium substrate is a basis and a precondition for the property research and the device application. The hexagonal boron nitride prepared by various transfer means generally has the problems of impurity introduction, mechanical damage, uncontrollable shape, poor repeatability, difficult realization of large-scale production and the like, so that the direct growth of the hexagonal boron nitride on a diamond medium substrate has great significance for preparing the hexagonal boron nitride diamond heterostructure.
Because hexagonal boron nitride grown on a medium substrate such as diamond lacks catalytic activity and is not easy to nucleate, the growth is often required to be carried out under extremely high temperature conditions, so that the diamond is graphitized and converted, the problem that nitrogen in the hexagonal boron nitride is lost usually exists, the surface morphology and the original property of the substrate are damaged, and the crystallization quality of the hexagonal boron nitride is limited.
Disclosure of Invention
First, the technical problem to be solved
Aiming at the problems, the disclosure provides a preparation method of a hexagonal boron nitride heterostructure, which is used for at least partially solving the technical problems of severe growth conditions, poor product quality and the like of the traditional preparation method.
(II) technical scheme
In one aspect, the disclosure provides a method for preparing a hexagonal boron nitride heterostructure, including: s1, heating a dielectric substrate, and introducing ammonia gas into a deposition chamber; s2, sputtering a boron nitride target material by an ion source, and depositing the obtained nitrogen and boron atoms on a dielectric substrate for growth; s3, cooling to obtain the hexagonal boron nitride heterostructure.
Further, the dielectric substrate comprises one of diamond, sapphire, silicon oxide, and silicon.
Further, S1 includes: heating the dielectric substrate to 500-1000 ℃; the flow rate of the ammonia gas introduced into the deposition chamber is 5sccm to 15sccm.
Further, S2 includes: reducing the flow of ammonia gas into the deposition chamber; argon is introduced into the ion source, and the ion source ionizes the argon to generate an argon ion beam.
Further, S2 includes: reducing the flow rate of ammonia gas introduced into the deposition chamber to be 2-8 sccm; the flow rate of argon gas introduced into the ion source is 2sccm to 10sccm.
Further, S2 includes: the working voltage of the ion source sputtering is 800V-1500V; the ion beam current density of the argon ion beam is 0.1mA/cm 2 ～0.4mA/cm 2 。
Further, S2 includes: the time from the deposition of nitrogen and boron atoms to the growth of the dielectric substrate is 10 min-60 min.
Further, the purity of the boron nitride target material in S2 is more than 99.5 percent.
Further, S1 further includes: and S01, sequentially placing the dielectric substrate in acetone, isopropanol and ethanol for ultrasonic cleaning, and drying by nitrogen.
Further, S1 further includes: s02, pre-pumping the deposition chamber to a back vacuum degree of 1×10 - 4 Pa or below.
(III) beneficial effects
The preparation method of the hexagonal boron nitride heterostructure grown directly at low temperature can avoid the complex transfer process during preparation of the hexagonal boron nitride layer, and the problems of film damage and pollution caused by transfer, and is beneficial to realizing controllable large-scale production; the ammonia gas is used for assisting in providing a nitrogen-rich atmosphere, and the argon ion beam is used for sputtering and depositing hexagonal boron nitride, so that the growth of hexagonal boron nitride with stoichiometric ratio can be realized at low temperature, and the crystal quality of hexagonal boron nitride prepared by a physical vapor deposition method at low temperature is effectively improved; meanwhile, as boron nitride grows at a lower temperature, graphitization transformation of the diamond dielectric substrate at a high temperature is prevented, the original properties of the dielectric substrate can be ensured to the maximum extent, and the method has important significance for electronics and optoelectronics application.
Drawings
FIG. 1 schematically illustrates a flow chart of a method of fabricating a hexagonal boron nitride heterostructure in accordance with an embodiment of the present disclosure;
FIG. 2 schematically illustrates an X-ray photoelectron spectrum of boron atom 1s electrons for two samples of hexagonal boron nitride grown on a diamond media substrate in accordance with an embodiment of the present disclosure;
FIG. 3 schematically illustrates Raman spectra of two samples of hexagonal boron nitride grown on a diamond media substrate in accordance with an embodiment of the present disclosure;
fig. 4 schematically shows absorption spectra of two samples of hexagonal boron nitride grown on a diamond media substrate in accordance with an embodiment of the present disclosure.
Detailed Description
For the purposes of promoting an understanding of the principles and advantages of the disclosure, reference will now be made to the embodiments illustrated in the drawings and specific language will be used to describe the same.
In the drawings or description, like or identical parts are provided with the same reference numerals. Implementations not shown or described in the drawings are forms known to those of ordinary skill in the art. Additionally, although examples of parameters including particular values may be provided herein, it should be appreciated that the parameters need not be exactly equal to the corresponding values, but rather approximate the corresponding values within acceptable error margins or design constraints.
The embodiment of the disclosure provides a method for preparing a hexagonal boron nitride heterostructure, please refer to fig. 1, including: s1, heating a dielectric substrate, and introducing ammonia gas into a deposition chamber; s2, sputtering a boron nitride target material by an ion source, and depositing the obtained nitrogen and boron atoms on a dielectric substrate for growth; s3, cooling to obtain the hexagonal boron nitride heterostructure.
The hexagonal boron nitride diamond heterostructure is directly grown at low temperature by adopting the ion beam sputtering deposition technology, ammonia gas is introduced into an auxiliary gas path while the hexagonal boron nitride target is sputtered by the argon ion beam, so that boron and nitrogen atoms are deposited on a diamond medium substrate to grow hexagonal boron nitride, nitrogen-rich atmosphere is provided by ammonia gas decomposition, the crystallization quality of the hexagonal boron nitride is improved, the growth temperature of the hexagonal boron nitride is effectively reduced, and the hexagonal boron nitride diamond heterostructure is directly prepared at low temperature.
On the basis of the above embodiment, the dielectric substrate includes one of diamond, sapphire, silicon oxide, and silicon.
The preparation method of the hexagonal boron nitride patrolling structure is applicable to all dielectric substrates, and the boron nitride is grown at the lower temperature of 500-1000 ℃ due to the lower temperature of ion beam sputtering, so that the original properties of the dielectric substrates can be ensured to the maximum extent, and the preparation method has important significance for electronics and optoelectronics application.
On the basis of the above embodiment, S1 includes: heating the dielectric substrate to 500-1000 ℃; the flow rate of the ammonia gas introduced into the deposition chamber is 5sccm to 15sccm.
The medium substrate is heated to 500-1000 ℃ so as to be beneficial to decomposing ammonia gas in a lower pressure environment, a nitrogen-rich atmosphere is provided, nitrogen atoms are supplemented for boron nitride to be grown, and the original properties of the medium substrate are not changed at a relatively low temperature.
The flow of the introduced ammonia gas is in the range, which is favorable for ensuring the high vacuum degree of the chamber, ensuring the normal operation of the vacuum system and simultaneously providing enough nitrogen concentration.
On the basis of the above embodiment, S2 includes: reducing the flow of ammonia gas into the deposition chamber; argon is introduced into the ion source, and the ion source ionizes the argon to generate an argon ion beam.
When the deposition chamber is in the nitrogen-rich atmosphere, the flow of ammonia in the auxiliary gas path is reduced so as to meet the high vacuum environment required by the operation of the ion source and prevent the argon ion beam from excessively scattering with boron and nitrogen atoms to be sputtered.
Argon is continuously introduced, and argon ion beams are generated by the action of a sputtering ion source to sputter a boron nitride target so as to obtain nitrogen and boron atoms.
On the basis of the above embodiment, S2 includes: reducing the flow rate of ammonia gas introduced into the deposition chamber to be 2-8 sccm; the flow rate of argon gas introduced into the ion source is 2sccm to 10sccm.
The ammonia gas is continuously supplied to replenish the nitrogen atoms that are continuously consumed, continuously providing a nitrogen-rich atmosphere.
The flow rate of argon in this range is advantageous for ionization to obtain a sufficient amount of argon ions for sputtering the boron nitride target on the one hand and for ensuring that the argon ions are less affected by back scattering on the other hand.
On the basis of the above embodiment, S2 includes: the working voltage of the ion source sputtering is 800V-1500V; the ion beam current density of the argon ion beam is 0.1mA/cm 2 ～0.4mA/cm 2 。
Under the condition of 800V-1500V, ionized argon ions can obtain kinetic energy with proper size, and after sputtering a boron nitride target material, the angle and radial distribution of boron and nitrogen atoms matched with the equipment size are generated.
The ion beam current density of the argon ion beam in this range has the technical effects of obtaining a sufficient yield of boron and nitrogen atoms and preventing the argon ions from excessively back-scattering to affect the lifetime of the apparatus.
On the basis of the above embodiment, S2 includes: the time from the deposition of nitrogen and boron atoms to the growth of the dielectric substrate is 10 min-60 min.
The time of growth is in this range to facilitate control of the boron nitride growth thickness, which may be, for example, 5 to 10nm.
Based on the above embodiment, the purity of the boron nitride target in S2 is greater than 99.5%.
The purity of the boron nitride target material is more than 99.5%, which is beneficial to ensuring the purity of the prepared boron nitride, thereby maintaining the original performance of the boron nitride.
On the basis of the above embodiment, S1 further includes: and S01, sequentially placing the dielectric substrate in acetone, isopropanol and ethanol for ultrasonic cleaning, and drying by nitrogen.
The medium substrate is sequentially placed in acetone, isopropanol and ethanol for ultrasonic cleaning, so that organic pollutants on the surface of the medium substrate can be removed, and organic solvent residues are avoided.
On the basis of the above embodiment, S1 further includes: s02, pre-pumping the deposition chamber to a back vacuum degree of 1×10 -4 Pa or below.
The vacuum degree of the back bottom is 1 multiplied by 10 -4 Pa or below to ensure that there is no oxygen interference within the deposition chamber, while ensuring ultra-high vacuum conditions required for operation of the ion source.
The method adopts a single ion source to carry out sputtering, and ammonia gas is introduced through an auxiliary gas path in a medium substrate heating stage and a boron nitride target sputtering stage to successfully supplement nitrogen vacancy defects in boron nitride, so that the preparation of hexagonal boron nitride with high quality and ideal stoichiometric ratio is realized.
The present disclosure is further illustrated by the following detailed description. Taking a method for directly growing a hexagonal boron nitride diamond heterostructure at a low temperature as an example, the method comprises the following specific steps:
steps S01 to S02 prepare a diamond dielectric substrate.
In some embodiments, the steps S01 to S02 include:
sequentially placing a diamond medium substrate in acetone, isopropanol and ethanol for ultrasonic cleaning, drying by nitrogen, and installing into an ion beam sputtering deposition chamber for standby, wherein the deposition chamber comprises a boron nitride target, an auxiliary gas path and a sputtering ion source, and the deposition chamber is pre-pumped to a back vacuum degree, wherein the back vacuum degree of the deposition chamber is 1 multiplied by 10 -4 Pa or less;
preferably, the diamond dielectric substrate material is a diamond single crystal.
And S1, introducing ammonia gas into the auxiliary gas path to heat the diamond medium substrate. Growing hexagonal boron nitride needs to be carried out under the condition that the temperature of the diamond medium substrate is higher than room temperature, and ammonia gas is introduced into the deposition chamber by an auxiliary gas path in the heating process of the diamond medium substrate to provide a nitrogen-rich atmosphere.
In some embodiments, the step S1 further includes:
step S11, introducing ammonia gas into the deposition chamber through an auxiliary gas path, wherein the flow rate of the ammonia gas is between 5sccm and 15sccm, and the preferred flow rate of the ammonia gas is 10sccm;
in a substep S12, the diamond dielectric substrate is heated to a target temperature, wherein the target temperature is between 500 ℃ and 1000 ℃, and preferably, in this embodiment, the temperature of the diamond dielectric substrate is 700 ℃.
In this example, in the specific preparation process, based on the above-mentioned optimal embodiment, the flow rate of ammonia gas is 10sccm, and the temperature of the diamond medium substrate is 700 ℃, so as to implement the temperature condition of growth of hexagonal boron nitride on the diamond surface and the nitrogen-rich atmosphere.
And S2, sputtering boron nitride by a sputtering ion source to obtain nitrogen and boron atoms, and depositing the nitrogen and boron atoms on the diamond dielectric substrate to grow hexagonal boron nitride.
In some embodiments, the step S2 further includes:
s21, reducing the flow of ammonia in the auxiliary gas circuit to ensure the normal operation of the sputtering ion source;
step S22, ensuring the temperature stability of the diamond medium substrate, introducing argon into the deposition chamber, generating an argon ion beam by the action of a sputtering ion source, sputtering a boron nitride target to obtain nitrogen and boron atoms, and in the step:
the temperature of the diamond medium substrate is between 500 ℃ and 1000 ℃, the temperature of the medium substrate is preferably 700 ℃, the flow rate of ammonia is between 2sccm and 8sccm, the flow rate of ammonia is preferably 5sccm, the flow rate of argon is between 2sccm and 10sccm, the flow rate of argon is preferably 5sccm, the working voltage of a sputtering ion source is between 800V and 1500V, the working voltage is preferably 1000V, and the ion beam current density of an argon ion beam is 0.1mA/cm 2 To 0.4mA/cm 2 Between them, the preferred ion beam current density is 0.2mA/cm 2 The growth time of the hexagonal boron nitride is between 10min and 60min, and the preferred growth time is 40min.
In this example, in the specific preparation process, based on the above-described preferred embodiment, the flow rate of ammonia gas was 5sccm, the flow rate of argon gas was 5sccm, the temperature of the dielectric substrate was 700 ℃, the operating voltage of the sputter ion source was 1000V, and the ion beam current density of the argon ion beam was 0.2mA/cm 2 The growth time is 40min, so that the hexagonal boron nitride diamond heterostructure can be directly grown at low temperature, the original physical properties of the diamond dielectric substrate are guaranteed, graphitization transformation is prevented, and the crystallization quality of the hexagonal boron nitride film is improved.
And S3, after the growth is finished, cooling to obtain the hexagonal boron nitride diamond heterojunction material.
Based on the above embodiments, another aspect of the present disclosure provides a hexagonal boron nitride diamond heterostructure, where the heterostructure is directly grown at a low temperature by the above method, and a specific growth method is shown in the above examples and is not described herein.
According to the method for directly growing the hexagonal boron nitride diamond heterostructure at the low temperature provided by the disclosure and the embodiment thereof, as shown in fig. 2, namely an X-ray photoelectron spectrum of boron atom 1s electrons of two samples of hexagonal boron nitride grown on a diamond dielectric substrate according to the embodiment of the disclosure, wherein the ammonia flow of an auxiliary gas path in the sample preparation process of fig. 2 (a) is 0, and the ammonia flow of the auxiliary gas path in the sample preparation process of fig. 2 (b) is set according to parameters in the technical scheme of the disclosure; in both fig. 2 (a) and fig. 2 (b), a peak can be observed at 190eV, corresponding to a boron-nitrogen bond, while in fig. 2 (a) there is another peak at 188eV, corresponding to a boron-boron bond, and since the flow of ammonia gas in the auxiliary gas path is 0 when the sample is grown, the ideal stoichiometric ratio of hexagonal boron nitride cannot be ensured, boron enrichment phenomenon exists in boron nitride, and no characteristic peak of boron-boron bond is observed in fig. 2 (b), which proves that hexagonal boron nitride maintains the ideal stoichiometric ratio. FIG. 3 is a Raman spectrum of two samples of hexagonal boron nitride grown on a diamond media substrate, which may be at 1370cm, in accordance with an embodiment of the present disclosure -1 A Raman frequency shift peak is observed, the Raman frequency shift peak corresponds to a hexagonal boron nitride Raman characteristic peak, the ammonia flow of an auxiliary gas path of a sample corresponding to a lower curve in the drawing is 0 in the growth process, the half-width of the corresponding Raman characteristic peak is large, the signal-to-noise ratio is low, in contrast, the half-width of the Raman characteristic peak is small, and the signal-to-noise ratio is high when the upper curve corresponds to sample preparation conditions and is set according to parameters in the technical scheme. Fig. 4 is an absorption spectrum diagram of two samples of hexagonal boron nitride grown on a diamond medium substrate according to an embodiment of the disclosure, where the flow rate of ammonia in an auxiliary gas path in the sample preparation process in fig. 4 (a) is 0, and the flow rate of ammonia in the auxiliary gas path in the sample preparation process in fig. 4 (b) is set according to parameters in the technical scheme of the disclosure; in both FIG. 4 (a) and FIG. 4 (b), a peak can be observed at 200nm, which corresponds to the characteristic light absorption peak of hexagonal boron nitride forbidden band width, while the tailing of FIG. 4 (a) on the long wavelength side of the absorption peak is obvious, because the ammonia flow of the auxiliary gas path in the preparation process of the sample is that0, resulting in poor quality of hexagonal boron nitride crystals, compared with the sample preparation conditions corresponding to fig. 4 (b) according to the parameters set in the technical scheme of the disclosure, the obtained absorption peak is sharper, which indicates that the quality of hexagonal boron nitride crystals is higher.
In summary, the method for directly growing the hexagonal boron nitride diamond heterostructure at low temperature can simply and efficiently realize the direct growth of the hexagonal boron nitride on the diamond dielectric substrate, avoid the problems of complicated transfer process, mechanical damage caused by transfer, impurity introduction and the like, ensure the ideal stoichiometric ratio of the hexagonal boron nitride by supplying ammonia gas to an auxiliary gas path, realize the growth of the hexagonal boron nitride at lower temperature, avoid graphitization transformation of the diamond dielectric substrate at high temperature, and have very important significance for the application of the electronic and optoelectronics of the hexagonal boron nitride diamond heterostructure.
While the foregoing embodiments have been described in some detail for purposes of clarity of understanding, it will be understood that the foregoing embodiments are merely illustrative of the invention and are not intended to limit the invention, and that any modifications, equivalents, improvements, etc. that fall within the spirit and principles of the present disclosure are intended to be included within the scope of the present disclosure.

Claims (10)

1. The preparation method of the hexagonal boron nitride heterostructure is characterized by comprising the following steps of:
s1, heating a dielectric substrate, and introducing ammonia gas into a deposition chamber;
s2, sputtering a boron nitride target material by an ion source, and depositing the obtained nitrogen and boron atoms on the dielectric substrate for growth;
s3, cooling to obtain the hexagonal boron nitride heterostructure.
2. The method of fabricating a hexagonal boron nitride heterostructure according to claim 1, wherein the dielectric substrate comprises one of diamond, sapphire, silicon oxide, silicon.
3. The method for preparing a hexagonal boron nitride heterostructure according to claim 1, wherein the S1 includes:
heating the dielectric substrate to 500-1000 ℃; the flow rate of the ammonia gas introduced into the deposition chamber is 5sccm to 15sccm.
4. The method for preparing a hexagonal boron nitride heterostructure according to claim 1, wherein the S2 includes:
reducing the flow rate of the ammonia gas introduced into the deposition chamber;
argon is introduced into an ion source, and the ion source ionizes the argon to generate an argon ion beam.
5. The method of fabricating a hexagonal boron nitride heterostructure according to claim 4, wherein the S2 includes:
reducing the flow rate of the ammonia gas introduced into the deposition chamber to be 2-8 sccm;
and introducing argon into the ion source at a flow rate of 2-10 sccm.
6. The method of fabricating a hexagonal boron nitride heterostructure according to claim 4, wherein the S2 includes:
the working voltage of the ion source sputtering is 800V-1500V;
the ion beam current density of the argon ion beam is 0.1mA/cm 2 ～0.4mA/cm 2 。
7. The method for preparing a hexagonal boron nitride heterostructure according to claim 1, wherein the S2 includes:
and depositing nitrogen and boron atoms on the dielectric substrate and growing for 10-60 min.
8. The method of fabricating a hexagonal boron nitride heterostructure according to claim 1, wherein the purity of the boron nitride target in S2 is greater than 99.5%.
9. The method for preparing a hexagonal boron nitride heterostructure according to claim 1, wherein the S1 further includes:
and S01, sequentially placing the dielectric substrate in acetone, isopropanol and ethanol for ultrasonic cleaning, and drying by nitrogen.
10. The method of fabricating a hexagonal boron nitride heterostructure according to claim 9, wherein the S1 further includes:
s02, pre-pumping the deposition chamber to a back vacuum degree, wherein the back vacuum degree is 1 multiplied by 10 -4 Pa or below.
CN202111335874.9A 2021-11-11 2021-11-11 Preparation method of hexagonal boron nitride heterostructure Pending CN116103609A (en)

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