CN107217242B - Surface modification method for dielectric substrate of electronic device - Google Patents
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- CN107217242B CN107217242B CN201710360173.8A CN201710360173A CN107217242B CN 107217242 B CN107217242 B CN 107217242B CN 201710360173 A CN201710360173 A CN 201710360173A CN 107217242 B CN107217242 B CN 107217242B
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/34—Nitrides
- C23C16/342—Boron nitride
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/50—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02109—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates
- H01L21/02112—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02225—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer
- H01L21/0226—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process
- H01L21/02263—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase
- H01L21/02271—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase deposition by decomposition or reaction of gaseous or vapour phase compounds, i.e. chemical vapour deposition
- H01L21/02274—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase deposition by decomposition or reaction of gaseous or vapour phase compounds, i.e. chemical vapour deposition in the presence of a plasma [PECVD]
Abstract
The invention belongs to the technical field of electronic devices, and particularly relates to a surface modification method of a dielectric substrate of an electronic device. The invention is that the hexagonal boron nitride film with two-dimensional structure is directly grown on the surface of the dielectric substrate, the thickness is between 1 nm and 100nm, and the hexagonal boron nitride film is used for modifying the interface between the electronic device semiconductor and the dielectric layer. According to the invention, by controlling the concentration of the raw materials, the quasi-balance of growth and etching in the plasma vapor deposition process is achieved, so that the non-catalytic growth of the hexagonal boron nitride film with the two-dimensional structure on the dielectric surface is realized. The method is simple and low in cost, does not need a transfer process in application, is compatible with a semiconductor process, and is operated at a low temperature in the whole process. The invention can also modify the hexagonal boron nitride film on the three-dimensional surface in a conformal way and can be prepared in a large area. The invention can improve the mobility of carriers at the interface of the semiconductor and the dielectric layer of the electronic device, reduce the thermal contact resistance of the interface of the semiconductor and the dielectric layer, and improve the heat conduction property and the stability of the device.
Description
Technical Field
The invention belongs to the technical field of electronic devices, and particularly relates to a surface modification method of a dielectric substrate of an electronic device.
Background
In the past decades, with the rapid development of modern electronic technology and the demand for increased device computing power, increasing carrier mobility and decreasing interface thermal resistance have become very important. Charge transfer in electronic devices occurs between a dielectric layer and a layer of semiconductor material, and joule heating is also generated at the interface. Therefore, the dielectric interface is very important in improving the mobility of the device and the heat dissipation. However, there are few methods for improving both mobility and heat dissipation by modifying the interface of the medium.
Hexagonal boron nitride filmThe film is a graphene-like material, and nitrogen atoms and boron atoms pass through sp2Hybridization is carried out to form a hexagonal lattice honeycomb two-dimensional structure. It is a wide band gap insulator with good mechanical strength, electrical insulation, thermal conductivity and chemical stability. Therefore, boron nitride has wide applications as a protective layer and a dielectric layer. At present, the hexagonal boron nitride film is grown by a catalyst-free chemical vapor deposition method, and high energy consumption and high cost are caused by the high growth temperature. Although the hexagonal boron nitride can be grown at low temperature by plasma chemical vapor deposition, the product presents hexagonal boron nitride with amorphous granular, disordered or three-dimensional structure. At present, the non-catalytic growth of large-area hexagonal boron nitride films with two-dimensional structures at low temperature is still difficult. Furthermore, while there has been much work to improve electronic device mobility by applying hexagonal boron nitride to dielectric surfaces, there is no precedent for applying it to semiconductor/dielectric substrate interfaces to improve heat dissipation performance.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a surface modification method of a dielectric substrate of an electronic device, which can improve the stability of the device under high power.
We find that reversible balance between hexagonal boron nitride growth and etching can be realized by controlling the precursor concentration in the growth process of the plasma chemical vapor deposition method, so that a high-quality two-dimensional hexagonal boron nitride film can be grown under the quasi-balance condition of the reversible reaction. The plasma modification technology provided by the invention can modify a two-dimensional hexagonal boron nitride film on the surface of a dielectric substrate in a conformal manner, and can also modify a two-dimensional hexagonal boron nitride film on the surface of the dielectric substrate with a three-dimensional structure in a conformal manner. The invention can improve the carrier mobility of the electronic device and reduce the thermal contact resistance of the interface of the semiconductor and the dielectric layer, thereby improving the stability of the device under high power.
The invention provides a surface modification method of a dielectric substrate of an electronic device, which comprises the following specific steps:
firstly, placing a clean dielectric substrate in a reaction cavity of a plasma chemical vapor deposition system; introducing carrier gas into the system, controlling the gas pressure to be in the range of 1 mTorr-100 Torr, heating to 200-800 ℃, and slowly introducing a reaction precursor;
secondly, applying plasma in a growth area of the material, wherein the power is 0.1-1000 watts and the duration is 1-200 minutes; the preferred power is 1-500 watts, and the duration is 20-100 minutes;
and thirdly, stopping heating, naturally cooling to room temperature, and obtaining the hexagonal boron nitride film with the two-dimensional structure on the surface of the dielectric substrate.
The dielectric substrate modified with the hexagonal boron nitride film can be directly used for preparing electronic devices.
Wherein the thickness of the hexagonal boron nitride film with the two-dimensional structure is 1-100nm, and the preferable thickness is 20-100 nm.
Wherein the carrier gas is selected from hydrogen, argon, nitrogen, oxygen, helium, air, and a mixture thereof.
The dielectric substrate is a silicon substrate with an oxide layer, mica, quartz, silicon nitride, hafnium oxide, aluminum oxide and the dielectric substrate with a three-dimensional structure.
Wherein the precursor for growing the hexagonal boron nitride film by the plasma method is N2，BNH6, NH3, BH3,B3N3H6, BNH4，BH2BH2Etc. molecules having boron and nitrogen elements.
Wherein, the reaction precursor is introduced in the following way: introducing the gaseous precursor into the reaction cavity through a gas flowmeter; putting the solid precursor into a reaction cavity and introducing the solid precursor into the reaction cavity in a heating and slow sublimation mode; the liquid precursor is put into a reaction cavity and is introduced into the reaction cavity in a heating volatilization or carrier gas carrying mode.
The plasma method is used for modifying the surface of the substrate, the concentration of a precursor is required to be accurately controlled, the range is that 0.0001-10mol of boron nitrogen source is introduced per minute, the quasi-balance of growth and etching in the plasma vapor deposition process is achieved, and the non-catalytic large-area growth of the hexagonal boron nitride film with the two-dimensional structure on the dielectric surface is realized.
The electronic devices include field effect transistors, light emitting diodes, photosensors, chemical sensors, and the like, having an interface of a dielectric layer and a semiconductor material. The semiconductor material is two-dimensional materials such as transition metal disulfide, graphene and the like, inorganic semiconductor materials such as silicon, germanium, selenium, gallium nitride, gallium arsenide, gallium phosphide, indium phosphide and the like, and organic semiconductor materials such as pentacene, metal phthalocyanine, metal porphyrin, polythiophene and the like.
Compared with the prior method, the method has the advantages that: (1) the technical method is simple and easy to operate, has low cost and can realize large-area decoration; (2) the two-dimensional hexagonal boron nitride film can be conformally modified on a dielectric surface with a three-dimensional structure; (3) the technology can improve the carrier mobility of an electronic device and reduce the contact thermal resistance of the interface of a semiconductor and a dielectric layer.
Drawings
FIG. 1 is a Raman (Raman) spectrum and an X-ray photoelectron spectrum of a two-dimensional hexagonal boron nitride film grown in example 1. Wherein, the left graph is the Raman spectrum of the hexagonal boron nitride, the middle graph is the X-ray photoelectron spectrum of the boron atom, and the right graph is the X-ray photoelectron spectrum of the nitrogen atom.
Fig. 2 is a graph of Atomic Force (AFM) of the tungsten selenide material in example 1, wherein (a) is a topographic map, (b) is a Raman (Raman) spectrum, and (c) is a fluorescence (PL) spectrum.
Fig. 3 is a schematic diagram of a field effect transistor as described in the present invention.
Fig. 4 is a transfer characteristic curve of a tungsten diselenide field-effect transistor prepared by modifying the substrate of the two-dimensional hexagonal boron nitride thin film in example 1, and a transfer characteristic curve of a tungsten diselenide field-effect transistor prepared by a substrate without modifying the two-dimensional hexagonal boron nitride thin film.
FIG. 5 is data related to the interfacial thermal resistance test in example 1.
FIG. 6 is data related to the interfacial thermal resistance test in example 2.
FIG. 7 is SiO with three-dimensional structure in example 32Scanning after growth of two-dimensional hexagonal boron nitride film on Si substrateElectron microscopy images and X-ray photoelectron spectroscopy. Wherein, (a) is three-dimensional SiO2A scanning electron microscope image of a Si substrate, (b) is an X-ray photoelectron spectrum of boron atoms in hexagonal boron nitride grown on the a substrate, (c) is an X-ray photoelectron spectrum of nitrogen atoms in hexagonal boron nitride grown on the a substrate, and (d) is another three-dimensional SiO2A scanning electron microscope image of the/Si substrate, (e) is an X-ray photoelectron spectrum of boron atoms in hexagonal boron nitride grown on the d substrate, and (f) is an X-ray photoelectron spectrum of nitrogen atoms in hexagonal boron nitride grown on the d substrate.
Reference numbers in the figures: 1 a gold electrode; 2, tungsten selenide; 3 hexagonal boron nitride film; 4 an insulating layer; 5 grid electrode.
Detailed Description
The invention is further illustrated by the following specific examples.
Example 1:
firstly, preparing a 1cm multiplied by 1cm p-type heavily doped silicon slice with a layer of post-silicon dioxide with the thickness of 300nm on the surface. Cleaned by ultrasonic cleaning (100 watt cleaning for 60 minutes) with isopropanol and deionized water. Then, the clean silicon chip is placed in a plasma chemical vapor deposition system;
second, the plasma CVD system is evacuated to 10 deg.C-3Torr, then introducing stable gas flow with the ratio of argon to hydrogen being 100 sccm/10 sccm into the device, and starting heating;
thirdly, heating the plasma chemical vapor deposition system to 500 ℃ and simultaneously carrying out BNH6Slowly heating the precursor to 110 ℃ for sublimation;
fourthly, applying plasma intensity to a growth area of the material, wherein the power intensity is 30 watts and the duration is 30 minutes;
step five, turning off a heating power supply, naturally cooling to room temperature, and obtaining a two-dimensional hexagonal boron nitride film on the surface of the silicon wafer with silicon dioxide (figure 1);
sixthly, placing the substrate for modifying the two-dimensional hexagonal boron nitride in a chemical vapor deposition system to grow a two-dimensional tungsten diselenide material (figure 3);
step seven, directly using the material prepared in the step six to prepare the field effect transistor, and the concrete construction steps are as follows: and (1) preparing an electrode pair on the two-dimensional tungsten selenide by using an electron beam exposure and thermal evaporation method, wherein the electrode pair is a gold electrode, is connected with the two-dimensional tungsten selenide material and has the thickness of 30 nm. The field effect transistor structure is shown in fig. 3. (2) The electrical properties of the field effect transistor are measured. The mobility of the field effect transistor adopting the hexagonal boron nitride modified substrate is 77 cm2V-1S-1The mobility is obviously higher than that of a field effect transistor without a hexagonal boron nitride modified substrate and is 1.4 cm2V-1S-1. Fig. 4 is a transfer characteristic curve. (3) And measuring the heat dissipation performance of the field effect transistor. The test data is shown in fig. 5. After the hexagonal boron nitride modification is adopted, the interface thermal resistance of the tungsten diselenide and the dielectric substrate is reduced by (4.55 +/-0.25) multiplied by 10-8m2KW-1。
Example 2:
the process of example 1 was followed with the following exceptions: and sixthly, placing the substrate for modifying the two-dimensional hexagonal boron nitride in a chemical vapor deposition system to grow the two-dimensional molybdenum diselenide material. And seventhly, measuring the heat dissipation performance of the field effect transistor. The test data is shown in fig. 6. After the hexagonal boron nitride modification is adopted, the thermal interface resistance of the molybdenum diselenide and the dielectric substrate is reduced by (1.21 +/-0.20) multiplied by 10-7m2KW-1。
Example 3:
the process of the first to fifth steps in example 1 was followed except that: using SiO with a three-dimensional structure2a/Si substrate. Fig. 7 shows a scanning electron microscope image of the substrate and an X-ray photoelectron spectrum of the hexagonal boron nitride film after modification by the plasma chemical vapor deposition method.
Claims (3)
1. A preparation method of an electronic device element is characterized by comprising the following specific steps:
firstly, placing a dielectric substrate in a reaction cavity of a plasma chemical vapor deposition system; introducing carrier gas into the system, controlling the gas pressure to be in the range of 1 mTorr-100 Torr, heating to 200-800 ℃, and introducing a reaction precursor for growing the hexagonal boron nitride film;
secondly, applying plasma in a growth area of the material, wherein the power is 0.1-1000 watts and the duration is 1-200 minutes;
thirdly, stopping heating, naturally cooling to room temperature, and obtaining a hexagonal boron nitride film with a two-dimensional structure on the surface of the dielectric substrate;
fourthly, directly using the dielectric substrate modified with the hexagonal boron nitride film for preparing the electronic device;
the dielectric substrate is silicon nitride, hafnium oxide, aluminum oxide or the dielectric substrate with a three-dimensional structure;
the reaction precursor for growing the hexagonal boron nitride film is N2、BNH6、NH3、BH3、B3N3H6、BNH4、BH2BH2；
The electronic device is an electrical element with a dielectric layer and a semiconductor material interface; the semiconductor material is selected from transition metal disulfide, graphene two-dimensional materials, silicon, germanium, selenium, gallium nitride, gallium arsenide, gallium phosphide and indium phosphide inorganic semiconductor materials, or pentacene, metal phthalocyanine, metalloporphyrin and polythiophene organic semiconductor materials;
the reaction precursor is introduced in the following mode: introducing the gaseous precursor into the reaction cavity through a gas flowmeter; putting the solid precursor into a reaction cavity and introducing the solid precursor into the reaction cavity in a heating and slow sublimation mode; putting the liquid precursor into a reaction cavity by heating and volatilizing or carrying in a carrier gas;
the concentration of the precursor is controlled to be 0.0001-10mol per minute, so that the quasi-balance of growth and etching in the plasma vapor deposition process is achieved, and the non-catalytic large-area growth of the hexagonal boron nitride film with the two-dimensional structure on the dielectric surface is realized.
2. The method of claim 1, wherein the carrier gas is selected from the group consisting of hydrogen, argon, nitrogen, oxygen, helium, air, and mixtures thereof.
3. The method of producing an electronic device element according to claim 1 or 2, wherein the thickness of the hexagonal boron nitride thin film of the two-dimensional structure is between 1 and 100 nm.
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| US20220165568A1 (en) * | 2019-03-15 | 2022-05-26 | Tokyo Electron Limited | Method and device for forming hexagonal boron nitride film |
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| CN109518278B (en) * | 2018-11-12 | 2020-12-08 | 厦门大学 | Method for enhancing p-type conductive doping of boron nitride film by nitrogen-rich atmosphere |
| CN117550621B (en) * | 2024-01-11 | 2024-03-22 | 恒泰军航高分子材料(山东)有限公司 | Method and device for preparing high-purity BN ceramic precursor |
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