CN110373636B - Preparation method of molybdenum silicide transition metal compound film material - Google Patents

Preparation method of molybdenum silicide transition metal compound film material Download PDF

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CN110373636B
CN110373636B CN201910821464.1A CN201910821464A CN110373636B CN 110373636 B CN110373636 B CN 110373636B CN 201910821464 A CN201910821464 A CN 201910821464A CN 110373636 B CN110373636 B CN 110373636B
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molybdenum
silicon substrate
molybdenum silicide
film
transition metal
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CN110373636A (en
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任卫
朱楠楠
张永超
杨朝宁
杨炎翰
李璐
姚国光
商世广
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Xian University of Posts and Telecommunications
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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
    • 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
    • C23C14/14—Metallic material, boron or silicon
    • C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
    • 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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24—Vacuum evaporation
    • C23C14/28—Vacuum evaporation by wave energy or particle radiation
    • C23C14/30—Vacuum evaporation by wave energy or particle radiation by electron bombardment
    • 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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/58—After-treatment
    • C23C14/5806—Thermal treatment
    • 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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/58—After-treatment
    • C23C14/5846—Reactive treatment

Abstract

The invention relates to a preparation method of a molybdenum silicide transition metal compound film material, which is characterized by comprising the following steps: heating a high-purity metal molybdenum target material by using a high-energy electron beam under a vacuum condition to gasify the metal molybdenum target material, depositing evaporated molybdenum vapor on the surface of a high-purity silicon substrate, and finally performing annealing treatment at 350-900 ℃ in air to form a molybdenum silicide film; the preparation method of the molybdenum silicide transition metal compound thin film material is characterized in that a layer of molybdenum metal is directly evaporated on the surface of a silicon substrate, the method is easy, the process is convenient, the deposition thickness of the thin film is controllable, the film forming quality is good, the elements are uniformly distributed, and the molybdenum silicide transition metal oxide thin film is obtained through annealing treatment; compared with the film prepared by the magnetron sputtering method adopted in the prior art, the film has the advantages of high purity, good quality, low annealing temperature, good repeatability and the like.

Description

Preparation method of molybdenum silicide transition metal compound film material
Technical Field
The invention relates to the technical field of preparation and characterization of materials, in particular to a preparation method of a molybdenum silicide transition metal compound thin film material.
Background
Molybdenum disilicide, a transition metal compound, is also called "an interstitial compound" because it cannot become interstitial atoms in the metal lattice because of the large atomic radius of silicon atoms. The special structure leads to the special physical and chemical properties of the compound, so that the melting point and the hardness of the compound greatly exceed those of a matrix material. The high-temperature-resistant alloy material has the advantages of high melting point, low density, high hardness, low resistivity, stable high-temperature property, good electric conductivity and good thermal conductivity, and high-temperature-resistant property and the like. The molybdenum silicide material is fully applied to the fields of aerospace, energy, military and the like, and is often used for manufacturing high-temperature heating elements, turbine blades, combustion chambers, high-temperature protective coating materials, wear-resistant and corrosion-resistant materials and the like. The search for high temperature stability has progressed to some extent. The characteristic research and application of the two-dimensional molybdenum silicide film material are also promising.
As semiconductor technology has matured, molybdenum silicide has become more tightly integrated with semiconductor processing. The molybdenum silicide film material has excellent conductivity, so that the molybdenum silicide film material can possibly replace Al, Cu and polysilicon to become the inner lead and outer connecting material of a new generation of deep submicron 3D super large scale integrated circuit (3 DVLSI). Meanwhile, the molybdenum silicide quartz mask plate as a novel photomask plate is superior to the conventional chromium mask in the aspects of chemical durability and dry etching characteristics. The amorphous molybdenum silicide film is made into a superconducting single photon detector SSPD and the like. The general integrated circuit is processed at a high temperature of more than 1000 ℃ in the manufacturing process, and MoSi with high temperature resistance characteristic is required2Is one of the ideal materials for manufacturing the grid of the integrated circuit. Therefore, the research and exploration on the integration of the molybdenum silicide thin film material and the semiconductor process have far-reaching significance.
Disclosure of Invention
The invention aims to provide a preparation method of a molybdenum silicide transition metal compound thin film material, which is characterized in that a high-purity molybdenum target material is heated by a high-energy electron beam under a vacuum condition to be gasified, evaporated molybdenum vapor is deposited on the surface of a high-purity silicon substrate, and finally annealing treatment at 350-900 ℃ is carried out in the air to form a molybdenum silicide thin film.
The specific process of the preparation method of the molybdenum silicide transition metal compound film material is as follows:
s1, placing the cleaned high-purity silicon substrate in an electron beam evaporation device, and placing a high-purity metal molybdenum target material in a copper crucible;
s2, vacuumizing the cavity to 1 × 10-3Pa or less while heating the high purity silicon substrate to 300 deg.C with resistance wireWarming;
s3, pre-melting the metal molybdenum target material by using an electron gun to emit electron beams;
s4, after the pre-melting is finished, carrying out ion source treatment, wherein the ion source treatment is used for cleaning residual gas in the cavity and waste molybdenum steam generated in the pre-melting process;
s5, setting coating process parameters and starting coating;
s6, annealing the prepared sample in air at 350-900 ℃ to form a molybdenum silicide film.
The purities of the high-purity metal molybdenum target material and the high-purity silicon substrate are more than 99.95%.
The high-purity silicon substrate is a single-side polished Si (100) single crystal wafer with the resistivity of 10k cm.
The area of the high-purity silicon substrate is 4 x 4cm2。
The specific process of the cleaned high-purity silicon substrate is as follows: and (3) putting the silicon substrate into a mixed solution containing concentrated sulfuric acid and hydrogen peroxide in a ratio of 3:1, and heating the silicon substrate on a high-temperature furnace until the silicon substrate is boiled at 120 ℃ for 8 minutes. Then ultrasonically cleaned in acetone, absolute ethyl alcohol and deionized water for 15 minutes respectively.
The concentrated sulfuric acid concentration is 96%, and the hydrogen peroxide concentration is 30%.
The distance between the metal molybdenum target and the silicon substrate is 75-100 cm.
The working voltage of the electron gun is 7.8-8.2 kv, and the current is 390-410 mA.
The invention has the beneficial effects that: the preparation method of the molybdenum silicide transition metal compound film material provided by the invention is characterized in that a layer of molybdenum metal is directly evaporated on the surface of a silicon substrate, and then a molybdenum silicide film is formed through annealing treatment. The preparation method is easy, the process is convenient, the deposition thickness of the film is controllable, the film forming quality is good, and the elements are uniformly distributed; compared with the molybdenum silicide film prepared by the magnetron sputtering method adopted by the prior art, the molybdenum silicide film has the advantages of high purity, good quality, low annealing temperature, good repeatability and the like; the prepared molybdenum silicide transition metal compound film material can be used as a raw material for manufacturing high-temperature-resistant materials, in particular to a grid material which is required by a transistor high-temperature treatment process in a semiconductor integrated circuit process.
The present invention will be described in further detail below with reference to the accompanying drawings.
Drawings
FIG. 1 is an X-ray diffraction pattern of the molybdenum silicide transition metal compound thin film produced.
FIG. 2 is a Raman spectrum of the prepared molybdenum silicide transition metal compound thin film.
FIG. 3 is a first scanning electron microscope image of the prepared molybdenum silicide transition metal compound film.
FIG. 4 is a second scanning electron micrograph of the prepared molybdenum silicide transition metal compound thin film.
FIG. 5 is a scanning electron microscope photograph III of the prepared molybdenum silicide transition metal compound thin film.
FIG. 6 is a scanning electron micrograph of the prepared molybdenum silicide transition metal compound thin film.
Fig. 7 is a scanning electron microscope image five of the prepared molybdenum silicide transition metal compound thin film.
FIG. 8 is a first scanning electron microscope image of a cross section of the prepared molybdenum silicide transition metal compound film.
FIG. 9 is a second scanning electron micrograph of a cross-section of the prepared molybdenum silicide transition metal compound thin film.
FIG. 10 is a scanning electron microscope photograph III of a cross section of the prepared molybdenum silicide transition metal compound thin film.
FIG. 11 is a scanning electron micrograph of a cross section of the prepared molybdenum silicide transition metal compound thin film.
FIG. 12 is a scanning electron micrograph of a cross-section of the prepared molybdenum silicide transition metal compound thin film.
Detailed Description
To further explain the technical means and effects of the present invention adopted to achieve the intended purpose, the following detailed description of the embodiments, structural features and effects of the present invention will be made with reference to the accompanying drawings and examples.
Example 1
In this embodiment, a method for preparing a molybdenum silicide transition metal compound thin film material as shown in fig. 1 to 12 is provided, in which a high-purity molybdenum target is heated by a high-energy electron beam under a vacuum condition to vaporize the molybdenum target, evaporated molybdenum vapor is deposited on the surface of a high-purity silicon substrate, and finally, an annealing treatment at 350 to 900 ℃ is performed in air to form a molybdenum silicide thin film.
The preparation method of the molybdenum silicide transition metal compound film material comprises the following specific processes of preparing a molybdenum silicide film:
s1, placing the cleaned high-purity silicon substrate in an electron beam evaporation device, and placing a high-purity metal molybdenum target material in a copper crucible;
s2, vacuumizing the cavity to 1 × 10-3Heating the high-purity silicon substrate to 300 ℃ by using a resistance wire and maintaining the constant temperature, so that the poor film quality caused by stress factors during film coating is reduced;
s3, pre-melting the molybdenum target material by using an electron gun to emit electron beams, so that the surface of the pre-melted metal is uniform and flat, and more uniform and stable evaporation gas can be improved;
s4, after the pre-melting is finished, carrying out ion source treatment, wherein the ion source treatment is used for cleaning residual gas in the cavity and waste molybdenum steam generated in the pre-melting process;
s5, setting coating process parameters, controlling the evaporation rate of molybdenum vapor and monitoring the deposition thickness of the film by using a crystal oscillator, and starting coating; the specific process is as follows: the current density of the electron beam is adjusted to control the evaporation rate of the molybdenum vapor, a crystal oscillator plate arranged in a cavity of the molybdenum vapor evaporation crystal wafer is arranged in the cavity body, and the crystal oscillator plate can detect deposition evaporation; resistance wires surrounding the vacuum cavity for a circle are arranged around the silicon substrate, and the resistance wires can play a role in heating the substrate after being electrified; in the evaporation process, the temperature of the silicon substrate is maintained at 300 ℃ by using the upper baking method so as to reduce the film stress and improve the film forming quality.
S6, annealing the prepared sample in air at 350-900 ℃ to form a molybdenum silicide film; annealing in air to promote mutual diffusion of the molybdenum metal and the silicon substrate to form molybdenum silicide; in addition, oxygen in the air also undergoes an oxidation reaction with the metal molybdenum film or silicon atoms diffused into the molybdenum film to form molybdenum trioxide and silicon dioxide. Molybdenum trioxide is formed at low temperatures and vaporization is initiated at 500 ℃. While the silica begins to form at about 600 degrees, the silica film is formed mainly on the surface of the film, and is relatively dense, which prevents oxygen from further penetrating into the film, thereby preventing the formation of molybdenum trioxide and the process of vaporization and evaporation. Molybdenum silicide is present as the annealing temperature is increased to 1400 degrees. Therefore, the annealing treatment is carried out on the sample at 350-900 ℃, and the main purpose is to observe the solid phase reaction of the film along with the change of the annealing temperature. As for the annealing time, we chose 1 hour, mainly for the film phase to be able to proceed sufficiently.
Furthermore, the purities of the high-purity metal molybdenum target material and the high-purity silicon substrate are both more than 99.95%.
Further, the high-purity silicon substrate is a single-side polished Si (100) single crystal wafer with the resistivity of 10k cm.
Further, the area of the high-purity silicon substrate is 4 x 4cm2。
The specific process of the cleaned high-purity silicon substrate is as follows: mixing 4X 4cm2The silicon substrate with the size is put into a mixed solution containing concentrated sulfuric acid with the concentration of 96% and hydrogen peroxide with the concentration of 30% in a ratio of 3:1, and heated to 120 ℃ on a high-temperature furnace for boiling for 8 minutes. Then ultrasonically cleaned in acetone, absolute ethyl alcohol and deionized water for 15 minutes respectively.
The distance between the metal molybdenum target and the silicon substrate is 75-100 cm. The distance between the metal molybdenum target and the filament of the electron gun is 20-30 mm; because the electron beam heats the molybdenum metal, under the condition that the silicon substrate is too close to the metal molybdenum target, the film forming rate of the molybdenum steam which is just evaporated is difficult to control due to too high rate, and the film forming quality and uniformity can be influenced. In addition, some evaporation materials are heated unevenly, so that the evaporation materials are cracked and broken up, and the broken evaporation materials are splashed onto a substrate, so that the film forming quality is influenced. When the distance between the substrate and the evaporation material is 75-100 cm, the rising rate of the molybdenum vapor and the relative gas density of the molybdenum vapor are more uniform, and the molybdenum vapor has a beneficial effect on the growth of a film.
The working voltage of the electron gun is 7.8-8.2 kv, the current is 390-410 mA, and the deposition rate can be maintained to be about 0.06 nm/s; the deposition rate may have some effect on the growth mode of the film. If the thickness of the film is larger, the quality of the film can be improved by adopting a small speed first and a large speed later; however, if the thickness is small (30 nm), the effect on the film is small.
Example 2
The method comprises the steps of adopting an electron beam evaporation method, filling metal molybdenum powder with the purity of 99.95% in a graphite crucible, fixing a silicon substrate subjected to surface cleaning treatment on a base frame, keeping the temperature of the substrate at 300 ℃, controlling the filament current of an electron gun to be 400mA, and controlling the deposition rate to be 0.06nm/s, so that the thickness of a metal molybdenum film deposited on the silicon substrate is 30 nm.
Example 3
In the embodiment, annealing treatment is carried out for 1 hour in an air atmosphere at 350 ℃, the temperature rise rate is set to be 5 ℃/min in the annealing process, heat preservation is carried out for 10 minutes when the temperature reaches 300 ℃, and the temperature is naturally reduced along with the furnace.
Example 4
In the embodiment, annealing treatment is carried out for 1 hour in an air atmosphere of 500 ℃, the temperature rise rate is set to be 5 ℃/min in the annealing process, heat preservation is carried out for 10 minutes when the temperature reaches 300 ℃, and the temperature is naturally reduced along with the furnace.
Example 5
In the embodiment, annealing treatment is carried out for 1 hour in an air atmosphere at 600 ℃, the temperature rise rate is set to be 5 ℃/min in the annealing process, heat preservation is carried out for 10 minutes when the temperature reaches 300 ℃, and the temperature is naturally reduced along with the furnace.
Example 6
In the embodiment, annealing treatment is carried out for 1 hour in an air atmosphere of 700 ℃, the temperature rise rate is set to be 5 ℃/min in the annealing process, heat preservation is carried out for 10 minutes when the temperature reaches 300 ℃, and the temperature is naturally reduced along with the furnace.
Example 7
In the embodiment, annealing treatment is carried out for 1 hour in an air atmosphere of 900 ℃, the temperature rise rate is set to be 5 ℃/min in the annealing process, heat preservation is carried out for 10 minutes when the temperature reaches 300 ℃, and then the temperature is naturally reduced along with the furnace.
Example 8
The molybdenum silicide films prepared in examples 2 to 6 were analyzed by an X-ray diffractometer, a raman spectrometer, and a scanning electron microscope, and the characterization results are shown in fig. 1 to 12. The results in FIG. 1 show that MoSi with orientation (202) is prepared at a lower annealing temperature2The diffraction peak of the film gradually decreases with the gradual increase of the annealing temperature. FIG. 2 shows the result at 521cm-1And 950cm-1The absorption peak represents Si peak, and MoO is obtained at annealing temperature of 600 deg.C or higher3The induced vibration peak disappears due to the two-dimensional film structure MoO3A boiling point of (2) is lowered, resulting in MoO3Upon annealing at 500 c, the vapors evaporated and left the film. The results of fig. 3-7 show that as the annealing temperature increases, the porosity of the film becomes smaller and the densification improves. This may be due to MoO3The evaporation is formed at the annealing temperature of 500 ℃, and a compact silicon dioxide protective layer is gradually formed on the surface of the sample along with the increase of the annealing temperature, and the protective layer can prevent external oxygen from permeating into the film to form MoO3Thus MoO3Less evaporation and smaller pores. The results of fig. 8 to 12 show that, at an annealing temperature of 500 ℃, molybdenum absorbs a large amount of oxygen to thicken the film, and as the annealing temperature increases, the deep molybdenum easily permeates into the silicon layer, and the generated silicon dioxide protective layer isolates the oxygen from slightly thickening the film. The molybdenum silicide film is prepared by an electron beam evaporation method, and a high-energy electron gun is adopted to bombard a metal target material, so that the metal molybdenum is gasified and evaporated and deposited on the surface of the silicon substrate. The particles obtained are smaller and more homogeneous compared to the magnetron sputtering method. The growth mode of the film is optimized by accurately controlling the deposition rate of the molybdenum vapor, and the quality of the film is improved.
The foregoing is a more detailed description of the invention in connection with specific preferred embodiments and it is not intended that the invention be limited to these specific details. For those skilled in the art to which the invention pertains, several simple deductions or substitutions can be made without departing from the spirit of the invention, and all shall be considered as belonging to the protection scope of the invention.

Claims (5)

1. A preparation method of a molybdenum silicide transition metal compound film material is characterized by comprising the following steps: heating a high-purity metal molybdenum target material by using a high-energy electron beam under a vacuum condition to gasify the metal molybdenum target material, depositing evaporated molybdenum vapor on the surface of a high-purity silicon substrate, and finally performing annealing treatment at 600 ℃ in air to form a molybdenum silicide film;
the specific process for preparing the molybdenum silicide film is as follows:
s1, placing the cleaned high-purity silicon substrate in an electron beam evaporation device, and placing a high-purity metal molybdenum target material in a copper crucible;
s2, vacuumizing the cavity to 1 × 10-3Heating the high-purity silicon substrate to 300 ℃ by using a resistance wire and maintaining the temperature to be constant below Pa;
s3, pre-melting the metal molybdenum target material by using an electron gun to emit electron beams;
s4, after the pre-melting is finished, carrying out ion source treatment, wherein the ion source treatment is used for cleaning residual gas in the cavity and waste molybdenum steam generated in the pre-melting process;
s5, setting coating process parameters and starting coating; the method specifically comprises the following steps: controlling the filament current of the electron gun to be 400mA, and controlling the deposition rate to be 0.06nm/s, so that the thickness of the metal molybdenum film deposited on the silicon substrate is 30 nm;
s6, annealing the prepared sample in the air at 600 ℃ to form a molybdenum silicide film; the purities of the high-purity metal molybdenum target material and the high-purity silicon substrate are more than 99.95 percent;
the distance between the metal molybdenum target and the silicon substrate is 75-100 cm.
2. The method for preparing the molybdenum silicide transition metal compound thin film material as claimed in claim 1, which is characterized in thatCharacterized in that: the high-purity silicon substrate is a single-side polished Si (100) single crystal wafer with the resistivity of 10k omega cm-1。
3. The method for preparing a molybdenum silicide transition metal compound thin film material as claimed in claim 1, wherein: the area of the high-purity silicon substrate is 4 x 4cm2。
4. The method for preparing a molybdenum silicide transition metal compound thin film material as claimed in claim 1, wherein: the specific process of the cleaned high-purity silicon substrate is as follows: putting the silicon substrate into a mixed solution containing concentrated sulfuric acid and hydrogen peroxide in a ratio of 3:1, heating the mixed solution on a high-temperature furnace to 120 ℃ for boiling for 8 minutes, and then ultrasonically cleaning the silicon substrate in acetone, absolute ethyl alcohol and deionized water for 15 minutes respectively.
5. The method for producing a molybdenum silicide transition metal compound thin film material as claimed in claim 4, wherein: the concentrated sulfuric acid concentration is 96%, and the hydrogen peroxide concentration is 30%.
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