CN109161844B - Boron-carbon-nitrogen film enveloping high-orientation boron nitride nanocrystalline and preparation method thereof - Google Patents
Boron-carbon-nitrogen film enveloping high-orientation boron nitride nanocrystalline and preparation method thereof Download PDFInfo
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- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
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- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0641—Nitrides
- C23C14/0647—Boron nitride
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
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Abstract
The invention discloses a boron carbon nitrogen film enveloping high-orientation boron nitride nanocrystals and a preparation method thereof, belonging to the technical field of film materials and preparation thereof. The boron carbon nitride film is an amorphous structure containing boron nitride nanocrystals grown on a silicon substrate. The preparation method is that the target material containing carbon boron nitride is prepared in a deposition chamber of a radio frequency magnetron sputtering device; wherein the substrate temperature is room temperature-600 ℃, the working gas is argon and nitrogen, the flow rate is 50sccm and 0-50 sccm respectively, and the working pressure is 1-3 Pa. The orientation of the boron nitride nanocrystalline in the film can realize ordered controllable growth by adjusting the process parameters, and the optical band gap of the prepared boron carbon nitride film is about 2.7-4.5 eV, and the boron carbon nitride film has good adjustable optical characteristics. The invention has the advantages of simple and safe process, mature technology, high sputtering rate, uniform deposited film, controllable size and the like, and is suitable for industrial mass production and popularization.
Description
Technical Field
The invention belongs to the technical field of film materials and preparation thereof, and particularly relates to a boron-carbon-nitrogen film enveloping oriented boron nitride nanocrystals and a preparation method of the film with controllable orientation of the boron nitride nanocrystals.
Background
Boron carbon nitride materials are widely concerned due to the excellent properties of carbon materials and boron nitride materials such as high hardness, wear resistance, low friction coefficient, low dielectric constant, thermal stability and chemical stability, can be used as hard protective coatings, can realize band gap adjustability by adjusting the components and chemical bond content of the materials, and have important value for the applications of the materials in the aspects of semiconductor devices, luminescent materials, sensors, optical energy conversion materials, field effect transistors, electromagnetic storage, vacuum microelectronics and the like.
At present, the common preparation methods of the boron carbon nitride film include hot filament assisted chemical vapor deposition, cold wall chemical vapor deposition, plasma assisted chemical vapor deposition, pulsed laser deposition, ion beam assisted deposition, reactive co-sputtering, magnetron sputtering and the like. Boron-carbon-nitrogen films obtained by different preparation methods are different, most of the films are of amorphous structures, phase separation exists in part of the films, and the stability of the films is poor. In the past, the content and chemical bonds of each element of the film are mostly adjusted by controlling a target source, precursor gas and other growth parameters, and the research on the growth theory and the practical application of the film is still immature.
The method carries out systematic research on the growth mode of the boron nitride nanocrystals contained in the film while adjusting the components of the film, can induce the high-orientation controllable growth of the boron nitride nanocrystals, can regulate and control the optical properties of the obtained boron-carbon-nitrogen film, and provides beneficial references for exploring the growth mechanism of the boron-carbon-nitrogen film, the reaction among film-forming atoms and the application of the boron-carbon-nitrogen film in the fields of photoelectricity, semiconductors and the like.
In addition, the radio frequency magnetron sputtering method adopted by the invention is a common preparation means in industry, the structure and growth of the boron nitride nanocrystalline in the boron carbon nitride film are controlled by changing the process parameters, and compared with other methods, the method has the advantages of simple and safe process, mature technology, high sputtering rate, uniform deposited film, controllable size and the like.
Disclosure of Invention
The invention aims to solve the technical problem of overcoming the defects in the controllable growth research of the film in the prior art, and provides a method for preparing a boron-carbon-nitrogen film of boron nitride nanocrystals with controllable envelope orientation.
In order to achieve the purpose, the invention adopts the following technical scheme.
A boron-carbon-nitrogen film enveloping highly-oriented boron nitride nanocrystals is characterized in that an amorphous boron-carbon-nitrogen film with an amorphous structure grows on a silicon substrate, the boron-carbon-nitrogen film contains boron nitride nanocrystals, and the size of the nanocrystal grains is 3-6 nanometers; the boron nitride nanocrystal comprises hexagonal boron nitride nanocrystals and cubic boron nitride nanocrystals, wherein the c-axis directions of the hexagonal boron nitride nanocrystals tend to be consistent.
The boron carbon nitride film enveloping the high-orientation boron nitride nanocrystal has an optical band gap of about 2.7-4.5 eV.
The technical scheme for preparing the boron-carbon-nitrogen film is as follows.
A method for preparing a boron-carbon-nitrogen film enveloping high-orientation boron nitride nanocrystals takes a mixed pressing block of carbon powder and boron nitride powder as a target material, and prepares the boron-carbon-nitrogen film enveloping the boron nitride nanocrystals in a deposition chamber of a radio frequency magnetron sputtering device; the method comprises the following specific steps:
(1) using a silicon single crystal wafer cut according to a (100) crystal face as a substrate, ultrasonically cleaning the substrate in acetone, ethanol and deionized water in sequence, blowing the substrate to dry by using nitrogen, sending the substrate into a deposition chamber, and vacuumizing the deposition chamber until the vacuum degree of the deposition chamber is 3 × 10-5Pa, heating the substrate to room temperature-600 ℃;
(2) continuing to vacuumize, and reaching the vacuum degree of the back bottom of the deposition chamber to 3 × 10 again-5And when Pa is needed, introducing reaction working gases of argon and nitrogen until the working pressure is 1-3 Pa. Wherein the argon flow is 50sccm, and the nitrogen flow is 0-50 sccm;
(3) and (3) adding a substrate negative bias, setting the sputtering power of the target and starting, moving the target baffle away after pre-sputtering for 2 minutes, and continuing sputtering for 1.5-4 hours.
In the above scheme, the distance between the substrate and the target is 8 cm.
In the scheme, the sputtering power is 80W to 200W.
In the scheme, the negative bias voltage of the substrate is-100V to-150V.
In the scheme, the magnetron sputtering deposition chamber is self-built or commercially available, and the frequency of the radio frequency source is 13.56 MHz.
In the scheme, the sputtering time only influences the thickness of the film, and the thickness of the prepared boron carbon nitrogen film is about 100-600 nanometers.
The boron-carbon-nitrogen film is an amorphous structure containing boron nitride nanocrystals, and the growth orientation of hexagonal phase boron nitride can be orderly and controllable by adjusting process parameters.
The invention has the beneficial effects that:
1. the method is a common industrial preparation method, has the advantages of simple and safe process, mature technology, high sputtering rate, uniform deposited film, controllable size and the like, and is very suitable for industrial mass production and popularization.
2. The prepared boron-carbon-nitrogen film contains high-quality boron nitride nanocrystals with uniform particle size, and the boron nitride nanocrystals can be fully regulated and controlled to grow in a high orientation mode through process parameters, so that the optical band gap of the boron-carbon-nitrogen film can be further regulated and controlled in a larger range, an important scientific basis is provided for the growth mechanism of the boron nitride film or the boron-carbon-nitrogen film and the bonding reaction of each atom in the film, and a new thought is provided for the application of the boron-carbon-nitrogen film in the industrial field.
Drawings
FIG. 1 is a Fourier transform infrared spectrum of a boron carbon nitride film prepared in example 1 of the present invention.
FIG. 2 is a high-resolution TEM image of a cross-section of a B-C-N film prepared at a substrate temperature of 600 ℃ in example 1 of the present invention.
FIG. 3 is a comparative scanning electron microscope image of boron carbon nitride films prepared at different substrate temperatures in example 1 of the present invention (wherein the substrate temperatures shown in a and b are room temperature and 600 ℃, respectively, and c is an oblique scanning electron microscope image with an inclination angle of 45 ℃ at the substrate temperature of 600 ℃).
FIG. 4 is a Fourier transform infrared spectrum of a boron carbon nitride film prepared in example 2 of the present invention.
FIG. 5 is a transmission electron microscope image of a cross section of a boron carbon nitride film prepared under the condition of nitrogen flow rate of 50sccm in example 2 of the present invention with high resolution.
FIG. 6 is a comparison of scanning electron microscope images of boron carbon nitride films prepared by different nitrogen flow rates in example 2 of the present invention (wherein the nitrogen flow rates shown in a and b are 0sccm and 50sccm, respectively).
FIG. 7 is a schematic cross-sectional structure diagram of a boron carbon nitride film of silicon-based enveloping highly-oriented boron nitride nanocrystals in accordance with the present invention. The prepared boron carbon nitride film is an amorphous structure containing boron nitride nanocrystals. By changing the substrate temperature and the components of the reaction working gas, the c axis of the prepared hexagonal boron nitride nanocrystal is approximately parallel to the surface of the substrate.
Detailed Description
The present invention will be described in further detail with reference to the following examples in conjunction with the accompanying drawings.
EXAMPLE 1 preparation of boron carbon nitride films at different substrate temperatures
(1) Ultrasonically cleaning silicon (100) single chip cut according to required size in acetone, ethanol and deionized water in sequence, blow-drying with nitrogen, and vacuum-pumping to 3 × 10 degree in deposition chamber-5Pa, setting the substrate temperature at room temperature, 250 ℃, 400 ℃, 500 ℃ and 600 ℃.
(2) Continuing to vacuumize, the back vacuum of the chamber to be deposited reaches 3 × 10 again-5When Pa, introducing reaction working gas argon until the working pressure is 2Pa, and the flow of the working gas argon is 50sccm (without adding nitrogen).
(3) The distance between the substrate and the target is 8 cm, substrate negative bias voltage-100V is added, the sputtering power of the target is set to be 150W, then the glow is started, after 2 minutes of pre-sputtering, the target baffle is moved away, and the sputtering time is 2 hours.
The Fourier transform infrared spectrogram of the product obtained at each substrate temperature is shown in FIG. 1, 773cm-1、1066cm-1The peak is respectively bending vibration of B-N-B bond between hexagonal boron nitride planes and characteristic peak of B-N bond of cubic boron nitride, 1235cm-1The peak is considered to be generated by the superposition of the peaks of B-C bond and C-N bond, which shows that the prepared boron-carbon-nitrogen film contains B-C bond, B-N bond and C-N bond and is a typical boron-carbon-nitrogen structure. It can be seen from the infrared spectrum that the cubic boron nitride content gradually decreases and the hexagonal boron nitride content significantly increases with increasing temperature. Hexagonal boron nitride has a structure similar to graphite, and the atoms of each layer are arranged in the direction of the c-axis in the manner of ABAB … …. For hexagonal boron nitride, when the infrared source is unpolarized and is incident normal to the substrate, in-plane B-N stretching vibrations and in-plane B-N-B bending vibrations provide orientation information. As shown in fig. 1, when the substrate temperature was gradually raised from room temperature to 600 c, only the vibration mode of B-N-B between the planes was activated by infrared light, and thus it was confirmed that the c-axis of the hexagonal boron nitride produced was nearly parallel to the base surface. FIG. 2 is a high-resolution transmission electron microscope image of a cross section of a boron-carbon-nitrogen film prepared under the substrate temperature of 600 ℃ in the present example, which shows that the microstructure of the film is an amorphous structure containing boron nitride nanocrystals (the portion of the film with circles in FIG. 2 is the boron nitride nanocrystals), and the average size of the nanocrystal grains is about 5 nm. As can be seen from the scanning electron micrograph of fig. 3, the roughness of the boron carbon nitride film gradually increases as the temperature increases. When the temperature is raised to 600 ℃, the surface appearance of the film has conical protrusions, which shows that the temperature rise induces the growth speed of the film in the longitudinal direction to be obviously higher than that in the transverse direction. Table 1 shows the optical band gaps of the boron carbon nitride films prepared at different substrate temperatures of example 1.
TABLE 1
| Temperature of the substrate | At room temperature | 250℃ | 400℃ | 500 |
600℃ |
| Optical bandgap (eV) | 3.8 | 3.9 | 3.7 | 3.7 | 4.0 |
Table 1 shows that the optical band gap of the boron-carbon-nitrogen film prepared at different substrate temperatures is between 3.5-4.5eV, and impurity levels related to boron-carbon-nitrogen appear in the forbidden band.
EXAMPLE 2 preparation of boron carbon nitride films at different Nitrogen flows
(1) Ultrasonically cleaning silicon (100) single chip cut according to required size in acetone, ethanol and deionized water in sequence, blow-drying with nitrogen, and vacuum-pumping to 3 × 10 degree in deposition chamber-5Pa, heating the substrate to 500 ℃.
(2) Continuing to vacuumize, the back vacuum of the chamber to be deposited reaches 3 × 10 again-5When Pa, introducing reaction working gases of argon and nitrogen until the working pressure is 2 Pa. The flow rate of the working gas argon gas was set to 50sccm, and the flow rates of the nitrogen gas were set to 0sccm, 10sccm, 20sccm, 30sccm, 40sccm, and 50sccm, respectively.
(3) The distance between the substrate and the target is 8 cm, substrate negative bias voltage-150V is added, the sputtering power of the target is set to be 150W, then the glow is started, after 2 minutes of pre-sputtering, the target baffle is moved away, and the sputtering time is 2 hours.
The Fourier transform infrared spectrum of the product obtained at each nitrogen flow is shown in FIG. 4, 780cm-1、1066cm-1、1380cm-1The peak is respectively bending vibration of B-N-B bond between hexagonal boron nitride planes, and stretching vibration characteristic peak of B-N bond in cubic boron nitride planes and hexagonal boron nitride planes, and is 1235cm-1The peak is considered to be generated by the superposition of the peaks of B-C bond and C-N bond, which shows that the prepared boron-carbon-nitrogen film contains B-C bond, B-N bond and C-N bond, and is typical boron-carbon-nitrogen filmAnd (5) structure. According to the infrared spectrum, after the nitrogen is added, the content of the cubic boron nitride in the film is higher than that of a sample without the nitrogen, the content of the cubic boron nitride has no obvious influence along with the increase of the proportion of the nitrogen, the content of the hexagonal boron nitride is slightly increased along with the increase of the nitrogen, and the c axis of the hexagonal boron nitride is obliquely crossed with the surface of the substrate. FIG. 5 is a high-resolution transmission electron microscope image of a cross section of a boron-carbon-nitrogen film prepared under a nitrogen flow rate of 50sccm, showing that the microstructure of the film is an amorphous structure including boron nitride nanocrystals (the portion of FIG. 5 where the circles are drawn is the boron nitride nanocrystals), and the average size of the nanocrystal grains is about 3.3 nm. FIG. 6 is a scanning electron micrograph showing that the resulting film was smooth and free of protrusions after the addition of nitrogen; the surface of the boron carbon nitride film becomes smooth by adding a sufficient amount of nitrogen gas no matter how high the substrate temperature is at the time of growth. Table 2 shows the optical band gap of the boron carbon nitride films prepared in example 2 with different nitrogen flow rates.
TABLE 2
| Flow of nitrogen (sccm) | 0 | 10 | 20 | 30 | 40 | 50 |
| Optical bandgap (eV) | 2.7 | 4.4 | 4.2 | 4.35 | 4.25 | 4.16 |
Table 2 shows that the optical band gap of the prepared boron carbon nitride films was about 2.7eV before the nitrogen gas was added, while the optical band gap of the films was between 4.16-4.5eV after the nitrogen gas was added, which significantly improved the optical band gap of the boron carbon nitride films, and that impurity levels no longer existed inside the band gap of these films after the nitrogen gas was introduced, compared to the samples in which the substrate temperature was changed.
The invention adopts a radio frequency magnetron sputtering method to prepare the amorphous boron carbon nitrogen film containing the boron nitride nanocrystal on the silicon substrate. The boron nitride phase contained in the film can be orderly and controllably grown by adjusting the substrate temperature and the nitrogen flow rate, and the optical property of the film can be further adjusted and controlled.
The foregoing is a detailed description of the present invention with reference to specific embodiments, and various changes and modifications made within the scope of the present invention should be covered by the appended claims.
Claims (4)
1. A boron-carbon-nitrogen film enveloping highly-oriented boron nitride nanocrystals is characterized in that an amorphous boron-carbon-nitrogen film with an amorphous structure grows on a silicon substrate, the boron-carbon-nitrogen film contains boron nitride nanocrystals, and the size of the nanocrystal grains is 3-6 nanometers; the boron nitride nanocrystal comprises hexagonal boron nitride nanocrystals and cubic boron nitride nanocrystals, wherein the c-axis directions of the hexagonal boron nitride nanocrystals tend to be consistent; the boron carbon nitride film enveloping the high-orientation boron nitride nanocrystal has an optical band gap of 3.7-4.5 eV.
2. A method for preparing the boron-carbon-nitrogen film enveloping the high-orientation boron nitride nanocrystals according to claim 1, which comprises the steps of preparing the boron-carbon-nitrogen film enveloping the boron nitride nanocrystals in a deposition chamber of a radio frequency magnetron sputtering device by taking a mixed pressed block of carbon powder and boron nitride powder as a target material; the method comprises the following specific steps:
(1) using a silicon single crystal wafer cut according to a (100) crystal face as a substrate, ultrasonically cleaning the substrate in acetone, ethanol and deionized water in sequence, blowing the substrate to dry by using nitrogen, sending the substrate into a deposition chamber, and vacuumizing the deposition chamber until the vacuum degree of the deposition chamber is 3 × 10-5Pa, heating the substrate to room temperature-600 ℃;
(2) continuing to vacuumize until the vacuum degree of the deposition chamber reaches 3 × 10 again-5And when Pa is needed, introducing reaction working gases of argon and nitrogen until the working pressure is 1-3 Pa. Wherein the argon flow is 50sccm, and the nitrogen flow is 0-50 sccm;
(3) applying a substrate negative bias voltage, wherein the substrate negative bias voltage is-100V to-150V; setting target sputtering power and starting, moving the target baffle away after pre-sputtering for 2 minutes, and continuing sputtering for 1.5-4 hours.
3. The method for preparing a boron carbon nitride film enveloping highly oriented boron nitride nanocrystals according to claim 2, wherein in the step (1), the distance between the substrate and the target is 8 cm.
4. The method for preparing a boron carbon nitride film enveloping highly oriented boron nitride nanocrystals according to claim 2, wherein in the step (3), the sputtering power is 80-200W; the radio frequency source frequency is 13.56 MHz.
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| CN109750266B (en) * | 2019-02-27 | 2019-12-31 | 吉林大学 | Method for regulating and controlling growth of boron nitride crystals in boron-carbon-nitrogen film |
| CN110061046B (en) * | 2019-05-09 | 2020-08-18 | 吉林大学 | N-type boron-carbon-nitrogen film/p-type monocrystalline silicon heterogeneous pn junction prototype device and preparation method thereof |
| CN110085679A (en) * | 2019-05-09 | 2019-08-02 | 吉林大学 | N-shaped boron nitride pellicle/p-type monocrystalline silicon heterogenous pn junction antetype device and preparation method |
| CN113151803A (en) * | 2021-03-15 | 2021-07-23 | 杭州电子科技大学 | Preparation method of boron-carbon-nitrogen film |
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