CN110983445A - Preparation method of porous silicon carbide film - Google Patents

Preparation method of porous silicon carbide film Download PDF

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Publication number
CN110983445A
CN110983445A CN201911393517.0A CN201911393517A CN110983445A CN 110983445 A CN110983445 A CN 110983445A CN 201911393517 A CN201911393517 A CN 201911393517A CN 110983445 A CN110983445 A CN 110983445A
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silicon carbide
etching
porous silicon
preparation
carbide film
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黄其煜
王舒瑭
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Shanghai Jiaotong University
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    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B33/00—After-treatment of single crystals or homogeneous polycrystalline material with defined structure
    • C30B33/08—Etching
    • C30B33/10—Etching in solutions or melts
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10—Inorganic compounds or compositions
    • C30B29/36—Carbides
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
    • C30B29/64—Flat crystals, e.g. plates, strips or discs

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Weting (AREA)

Abstract

The invention provides a preparation method of a porous silicon carbide film, and belongs to the field of micro-nano processing. The invention provides a preparation method of a porous silicon carbide film, which comprises the following steps: and (3) carrying out anodic oxidation on the silicon carbide wafer by using electrochemical etching to obtain the porous silicon carbide film. The method can realize the control of the nano morphology and the thickness of the porous silicon carbide film by changing the parameters of the applied voltage, the current, the frequency, the duty ratio and the like in the electrochemical etching process. The data of the embodiment show that the thickness of the porous silicon carbide film prepared by the invention is 100-300 microns, the diameter of the nano-pore is 0.5-50 nanometers, and the controllable preparation of the porous silicon carbide film is realized.

Description

Preparation method of porous silicon carbide film
Technical Field
The invention relates to the technical field of micro-nano processing, in particular to a preparation method of a porous silicon carbide film.
Background
With the rapid development of economy and technology and the increasingly accelerated industrialization process, people have higher and higher requirements for the operation of electronic devices, the traditional silicon semiconductor materials can not meet the requirements, and third-generation semiconductors gradually obtain higher and higher attention due to the unique inherent advantages of the third-generation semiconductors. Silicon carbide, which is a representative third-generation semiconductor, has characteristics such as a large forbidden band width, high hardness, and high electron mobility, and can be normally and stably operated at high temperature, high pressure, and high frequency. Due to the above significant advantages, more and more researches on processing and preparing silicon carbide materials are being carried out recently.
In recent years, the main methods for processing and preparing the silicon carbide micro-nano structure are dry etching methods, such as a Thermal Plasma PVD (TPPVD) technology and laser chemical vapor deposition, and the structure of the silicon carbide micro-nano structure obtained by the methods is not controllable.
Disclosure of Invention
In view of the above, the present invention is directed to a method for preparing a porous silicon carbide thin film. The preparation method provided by the invention can realize the controllable preparation of the porous silicon carbide film.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of a porous silicon carbide film, which comprises the following steps:
and carrying out anodic oxidation on the silicon carbide wafer by utilizing electrochemical etching to obtain the porous silicon carbide film.
Preferably, the electrochemical etching is constant voltage etching, constant current etching, pulsed voltage etching or pulsed current etching.
Preferably, the voltage of the constant voltage etching is 5-20V.
Preferably, the current of the constant current etching is 50-500 mA/cm2。
Preferably, the amplitude of the pulse voltage etching is 5-20V, the frequency is 0.1-100 Hz, and the duty ratio is 10% -90%.
Preferably, the amplitude of the pulse current etching is 50-500 mA/cm2The frequency is 0.1-100 Hz, and the duty ratio is 10-90%.
Preferably, the etching solution used in the electrochemical etching is an aqueous solution containing hydrofluoric acid and/or an ethanol solution containing hydrofluoric acid.
Preferably, the mass percentage concentration of the aqueous solution containing hydrofluoric acid is 0.1-40%, and the mass percentage concentration of the ethanol solution containing hydrofluoric acid is 0.1-40%.
Preferably, the electrochemical etching is carried out under the condition of stirring, and the rotating speed of the stirring is 50-2000 rpm.
Preferably, the silicon carbide wafer further comprises pretreatment before electrochemical etching, and the pretreatment sequentially comprises hydrofluoric acid aqueous solution soaking, water washing, drying, ultrasonic cleaning and re-drying.
The invention provides a preparation method of a porous silicon carbide film, which comprises the following steps: and (3) carrying out anodic oxidation on the silicon carbide wafer by using electrochemical etching to obtain the porous silicon carbide film. The method can realize the control of the nano morphology and the thickness of the porous silicon carbide film by changing the parameters of the applied voltage, the current, the frequency, the duty ratio and the like in the electrochemical etching process. The data of the embodiment show that the porous silicon carbide film prepared by the invention has the diameter of 0.5-50 nm and the diameter of 100-300 microns, and the controllable preparation of the porous silicon carbide film is realized.
Drawings
FIG. 1 is a schematic diagram of the electrical circuit connection during the electrochemical etching of the present invention;
FIG. 2 shows the results of example 2 at 400mA/cm2A macroscopic scanning electron microscope image of the porous silicon carbide film prepared by electrochemical etching under constant current density;
FIG. 3 is a scanning electron micrograph of a porous silicon carbide thin film prepared according to example 1 at a constant voltage of 10.5V;
FIG. 4 is a graph of sidewall thickness measurements of a porous silicon carbide film made according to example 1 at a constant voltage of 10.5V;
FIG. 5 is a graph showing pore diameter measurement of a porous silicon carbide thin film prepared in example 1 at a constant voltage of 10.5V;
FIG. 6 is a scanning electron micrograph of a porous silicon carbide thin film prepared according to example 1 under a constant voltage of 12V;
FIG. 7 is a graph showing measurement of sidewall thickness of a porous silicon carbide film obtained in example 1 under a constant voltage of 12V;
FIG. 8 is a graph showing the measurement of the pore diameter of a porous silicon carbide thin film prepared in example 1 at a constant voltage of 12V;
FIG. 9 is a scanning electron micrograph of a porous silicon carbide thin film prepared according to example 1 at a constant voltage of 14V;
FIG. 10 is a graph showing sidewall thickness measurements of a porous silicon carbide film prepared according to example 1 at a constant voltage of 14V;
FIG. 11 is a graph showing pore diameter measurement of a porous silicon carbide thin film prepared in example 1 at a constant voltage of 14V;
FIG. 12 is a scanning electron micrograph of a porous silicon carbide thin film prepared according to example 1 at a constant voltage of 15V;
FIG. 13 is a graph showing sidewall thickness measurements of a porous silicon carbide film prepared according to example 1 at a constant voltage of 15V;
FIG. 14 is a graph showing pore diameter measurement of a porous silicon carbide thin film prepared in example 1 at a constant voltage of 15V;
FIG. 15 is a graph showing the relationship between the etching rate and the constant voltage etching in example 1;
fig. 16 is a graph showing the change in pore size and constant voltage of the porous silicon carbide thin film obtained in example 1.
Detailed Description
The invention provides a preparation method of a porous silicon carbide film, which comprises the following steps:
and carrying out anodic oxidation on the silicon carbide wafer by utilizing electrochemical etching to obtain the porous silicon carbide film.
In the invention, the silicon carbide wafer preferably further comprises pretreatment before electrochemical etching, and the pretreatment sequentially comprises hydrofluoric acid aqueous solution soaking, water washing, drying, ultrasonic cleaning and re-drying. In the present invention, the hydrofluoric acid aqueous solution preferably has a mass concentration of 4%, and the hydrofluoric acid aqueous solution immersion enables removal of native oxides on the surface of the silicon carbide wafer. The source of the silicon carbide wafer is not particularly limited in the present invention, and commercially available products known to those skilled in the art may be used. In the present invention, the ultrasonic cleaning is preferably performed in acetone, ethanol, and deionized water in this order.
In the invention, the electrochemical etching is preferably carried out in an electrolytic tank, the silicon carbide wafer is preferably fixed at the bottom of the electrolytic tank through a copper plate and a screw, and the electrochemical etching is carried out through full contact of the hollowed circular holes below the electrolytic tank and an etching solution.
In the present invention, the electrochemical etching is preferably constant voltage etching, constant current etching, pulse voltage etching or pulse current etching.
In the invention, the voltage of the constant voltage etching is preferably 5-20V, and more preferably 10.5V, 12V, 14V or 15V. In the present invention, the diameter of the nano-pores of the porous silicon carbide thin film increases with an increase in voltage.
In the invention, the current of the constant current etching is preferably 50-500 mA/cm2More preferably 400mA/cm2。
In the invention, the amplitude of the pulse voltage etching is preferably 5-20V, the frequency is preferably 0.1-100 Hz, more preferably 0.8Hz, and the duty ratio is preferably 10-90%, more preferably 30%.
In the invention, the amplitude of the pulse current etching is preferably 50-500 mA/cm2The frequency is preferably 0.1 to 100Hz, more preferably 0.8Hz, and the duty ratio is preferably 10 to 90 percent, more preferably 30 percent.
In the present invention, the etching solution used in the electrochemical etching is preferably an aqueous solution containing hydrofluoric acid and/or an ethanol solution containing hydrofluoric acid, the mass percentage concentration of the aqueous solution containing hydrofluoric acid is preferably 0.1% to 40%, and more preferably 10% to 30%, and the mass percentage concentration of the ethanol solution containing hydrofluoric acid is preferably 0.1% to 40%, and more preferably 10% to 30%.
In the invention, the electrochemical etching is preferably carried out under the condition of stirring, and the rotating speed of the stirring is preferably 50-2000 rpm, and more preferably 500-1000 rpm. In the present invention, it is preferable to continuously grow a porous silicon carbide thin film by stirring.
In the invention, after the electrochemical etching is finished, the external voltage is preferably increased to more than 20V or the current is increased to 500mA/cm within 0.01-10 s2The side wall of the nano hole of the porous silicon carbide film is thinned, so that the peeling of the porous silicon carbide film is realized.
In the present invention, after the electrochemical etching is completed, it is preferable to obtain a porous silicon carbide film attached to a silicon carbide wafer by stopping the application of voltage or current.
FIG. 1 is a schematic diagram of the circuit connection during electrochemical etching of the present invention, showing the details of the circuit connection during the etching process.
In order to further illustrate the present invention, the following will describe the preparation method of the porous silicon carbide thin film provided by the present invention in detail with reference to examples, but they should not be construed as limiting the scope of the present invention.
The first embodiment is as follows:
cutting a four-inch silicon carbide wafer to 2.5 x 2.5cm by using a femtosecond laser cutting method2Square small wafers. The sliced wafer was immersed in a hydrofluoric acid aqueous solution having a mass concentration of 4% for 1 minute to remove natural oxides on the surface, and then rinsed with flowing deionized water and dried under a nitrogen atmosphere. And ultrasonically cleaning the dried silicon carbide wafer for 10min by using acetone, ethanol and deionized water in sequence, then washing the silicon carbide wafer by using flowing deionized water, and drying the silicon carbide wafer in a nitrogen atmosphere. The silicon carbide wafer after cleaning and drying is fixed at the bottom of an electrolytic bath through a copper plate and a screw, and is fully contacted with an etching solution (containing hydrofluoric acid and an aqueous solution with the mass percentage concentration of preferably 15%) through a hollow round hole below the electrolytic bath. The method comprises the steps of providing an external constant voltage through a power supply, carrying out constant-voltage electrochemical etching on a silicon carbide wafer (the rotating speed of stirring is 50rpm), carrying out electrochemical etching for 20 minutes under the constant voltages of 10.5V, 12V, 14V and 15V respectively, and after the electrochemical etching is finished, rapidly increasing the external voltage to 50V within 10s to realize the stripping of the porous silicon carbide film and obtain the porous silicon carbide film.
Fig. 3 is a scanning electron microscope image of the porous silicon carbide film obtained under the constant voltage of 10.5V according to the present embodiment, fig. 4 is a side wall thickness measurement chart of the porous silicon carbide film obtained under the constant voltage of 10.5V according to the present embodiment, and fig. 5 is a pore diameter measurement chart of the porous silicon carbide film obtained under the constant voltage of 10.5V according to the present embodiment.
Fig. 6 is a scanning electron microscope image of the porous silicon carbide film obtained under the constant voltage of 12V according to the present example, fig. 7 is a side wall thickness measurement chart of the porous silicon carbide film obtained under the constant voltage of 12V according to the present example, and fig. 8 is a pore diameter measurement chart of the porous silicon carbide film obtained under the constant voltage of 12V according to the present example.
Fig. 9 is a scanning electron microscope image of the porous silicon carbide film obtained at a constant voltage of 14V according to the present example, fig. 10 is a side wall thickness measurement chart of the porous silicon carbide film obtained at a constant voltage of 14V according to the present example, and fig. 11 is a pore diameter measurement chart of the porous silicon carbide film obtained at a constant voltage of 14V according to the present example.
Fig. 12 is a scanning electron microscope image of the porous silicon carbide film obtained under the constant voltage of 15V according to the present example, fig. 13 is a side wall thickness measurement chart of the porous silicon carbide film obtained under the constant voltage of 15V according to the present example, and fig. 14 is a pore diameter measurement chart of the porous silicon carbide film obtained under the constant voltage of 15V according to the present example.
3-14 show that the diameter of the nanopore in the silicon carbide thin film increases with the applied voltage, and the size of the nanopore can be kept relatively uniform at the same voltage.
FIG. 15 is a graph showing the relationship between the etching rate and the constant etching voltage in this example.
Fig. 16 is a graph showing the relationship between the pore size of the porous silicon carbide thin film prepared in this example and the constant etching voltage.
Example two:
cutting a four-inch silicon carbide wafer to 2.5 x 2.5cm by using a femtosecond laser cutting method2Square small wafers. The sliced wafer was immersed in a hydrofluoric acid aqueous solution having a mass concentration of 4% for 1 minute to remove natural oxides on the surface, and then rinsed with flowing deionized water and dried under a nitrogen atmosphere. And ultrasonically cleaning the dried silicon carbide wafer for 10min by using acetone, ethanol and deionized water in sequence, then washing the silicon carbide wafer by using flowing deionized water, and drying the silicon carbide wafer in a nitrogen atmosphere. The cleaned and dried silicon carbide wafer is fixed at the bottom of an electrolytic bath through a copper plate and a screw, passes through a hollow round hole below the electrolytic bath and an etching solution (containing hydrofluoric acid and with the mass percentage concentration of preferably 12.5 percent)Aqueous solution) are sufficiently contacted. Constant current electrochemical etching (stirring speed of 100rpm) is carried out on the silicon carbide wafer by applying constant current from a power supply at 80 mA/cm, 200 mA/cm, 300mA/cm and 400mA/cm2The electrochemical etching is carried out for 2 minutes under the constant current, and after the electrochemical etching is finished, the current application is stopped to obtain the porous silicon carbide film attached to the silicon carbide wafer. The thicknesses of the prepared porous silicon carbide films are 8.7 micrometers, 11.0 micrometers, 12.6 micrometers and 15.6 micrometers respectively, and the diameters of the nano holes are small and large, the minimum is 1 nanometer, and the maximum is 35 nanometers.
FIG. 2 shows the results of example 2 at 400mA/cm2And (3) performing electrochemical etching under constant current density to obtain a low-power scanning electron microscope image of the porous silicon carbide film.
Example three:
cutting a four-inch silicon carbide wafer to 2.5 x 2.5cm by using a femtosecond laser cutting method2Square small wafers. The sliced wafer was immersed in a hydrofluoric acid aqueous solution having a mass concentration of 4% for 1 minute to remove natural oxides on the surface, and then rinsed with flowing deionized water and dried under a nitrogen atmosphere. And ultrasonically cleaning the dried silicon carbide wafer for 10min by using acetone, ethanol and deionized water in sequence, then washing the silicon carbide wafer by using flowing deionized water, and drying the silicon carbide wafer in a nitrogen atmosphere. The silicon carbide wafer after being cleaned and dried is fixed at the bottom of an electrolytic bath through a copper plate and a screw, and is fully contacted with an etching solution (containing hydrofluoric acid and ethanol solution with the mass percentage concentration of preferably 10%) through a hollow round hole below the electrolytic bath. The silicon carbide wafer is electrochemically etched (the rotating speed of stirring is 100rpm) for 10 minutes by applying an external pulse voltage (the amplitude is 20V, the frequency is 0.8Hz and the duty ratio is 30%) through a power supply, and after the electrochemical etching is finished, the voltage application is stopped to obtain the porous silicon carbide film. The thickness of the prepared porous silicon carbide film is 8.1 microns, and the diameter of the pores is 34.5 nanometers.
Example four:
cutting a four-inch silicon carbide wafer to 2.5 x 2.5cm by using a femtosecond laser cutting method2Square small wafers. Placing the cut wafer in hydrogen with the mass concentration of 4%The surface was cleaned by soaking in aqueous hydrofluoric acid for 1 minute, followed by rinsing with running deionized water and drying under a nitrogen atmosphere. And ultrasonically cleaning the dried silicon carbide wafer for 10min by using acetone, ethanol and deionized water in sequence, then washing the silicon carbide wafer by using flowing deionized water, and drying the silicon carbide wafer in a nitrogen atmosphere. The silicon carbide wafer after cleaning and drying is fixed at the bottom of an electrolytic bath through a copper plate and a screw, and is fully contacted with an etching solution (aqueous solution containing hydrofluoric acid and with the mass percentage concentration of preferably 20%) through a hollow round hole below the electrolytic bath. An external pulse current (with the amplitude of 300 mA/cm) is provided by a power supply2The frequency is preferably 0.1Hz, the duty ratio is 50 percent), the silicon carbide wafer is subjected to constant current electrochemical etching (the rotating speed of stirring is 1000rpm) for 5 minutes, and after the electrochemical etching is finished, the current is rapidly increased to 600mA/cm within 0.01s2And obtaining the independent porous silicon carbide film. The thickness of the prepared porous silicon carbide film is 15.5 micrometers, the diameter of the pores is increased from small to large, the minimum is 1 nanometer, and the maximum is 20 nanometers.
The foregoing is merely a preferred embodiment of the invention and is not intended to limit the invention in any manner. It should be noted that, for those skilled in the art, without departing from the principle of the present invention, several improvements and modifications can be made, and these improvements and modifications should also be construed as the protection scope of the present invention.

Claims (10)

1. A preparation method of a porous silicon carbide film is characterized by comprising the following steps:
and carrying out anodic oxidation on the silicon carbide wafer by utilizing electrochemical etching to obtain the porous silicon carbide film.
2. The method of claim 1, wherein the electrochemical etching is constant voltage etching, constant current etching, pulsed voltage etching, or pulsed current etching.
3. The preparation method according to claim 2, wherein the voltage of the constant voltage etching is 5-20V.
4. The preparation method according to claim 2, wherein the constant current etching current is 50-500 mA/cm2。
5. The preparation method according to claim 2, wherein the amplitude of the pulse voltage etching is 5-20V, the frequency is 0.1-100 Hz, and the duty ratio is 10-90%.
6. The preparation method according to claim 2, wherein the amplitude of the pulse current etching is 50-500 mA/cm2The frequency is 0.1-100 Hz, and the duty ratio is 10-90%.
7. The method according to claim 1, wherein the etching solution used in the electrochemical etching is an aqueous solution containing hydrofluoric acid and/or an ethanol solution containing hydrofluoric acid.
8. The method according to claim 7, wherein the aqueous solution containing hydrofluoric acid has a concentration of 0.1 to 40% by mass, and the ethanol solution containing hydrofluoric acid has a concentration of 0.1 to 40% by mass.
9. The preparation method according to claim 1, wherein the electrochemical etching is carried out under stirring at a rotation speed of 50-2000 rpm.
10. The preparation method according to claim 1, characterized in that the silicon carbide wafer further comprises pretreatment before being subjected to electrochemical etching, wherein the pretreatment comprises soaking in hydrofluoric acid aqueous solution, water washing, drying, ultrasonic cleaning and re-drying in sequence.
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113130305A (en) * 2021-03-03 2021-07-16 哈尔滨工业大学 Method for constructing surface microstructure of silicon carbide single crystal

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Application publication date: 20200410