CN113106531B - Method for electrochemically etching diamond semiconductor film - Google Patents
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- CN113106531B CN113106531B CN202110437505.4A CN202110437505A CN113106531B CN 113106531 B CN113106531 B CN 113106531B CN 202110437505 A CN202110437505 A CN 202110437505A CN 113106531 B CN113106531 B CN 113106531B
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
- C25F3/00—Electrolytic etching or polishing
- C25F3/02—Etching
- C25F3/12—Etching of semiconducting materials
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Abstract
The invention belongs to the technical field of semiconductor manufacturing, and particularly discloses a method for electrochemically etching a diamond semiconductor film. According to the method, the diamond semiconductor film is immersed into electrolyte to serve as a cathode of an electrolytic cell, an inert electrode serves as an anode of an electrochemical electrolytic cell, direct current with voltage of 15-50V is applied between a cathode and an anode, the diamond semiconductor film is electrolyzed under the conditions of normal temperature and normal pressure, the surface of the diamond film is etched, and material reduction processing of the diamond semiconductor film is achieved. The invention is innovative from the principle of material reduction processing, provides a new method for etching the diamond semiconductor film by only one step at normal temperature and normal pressure by adopting simple equipment, and has great economic significance and popularization value.
Description
Technical Field
The invention relates to the technical field of semiconductor manufacturing, in particular to a method for electrochemically etching a diamond semiconductor film.
Background
Diamond by sp3The hybridized carbon element is a solid material with highest hardness and most stable chemical properties in the existing substances, and has irreplaceable application in various fields. In addition, diamond can become a semiconductor after being doped with a certain amount of elements such as boron, nitrogen and the like, the forbidden bandwidth can reach 5.5eV, and the diamond semiconductor has incomparable excellent properties such as high carrier mobility, ultrahigh frequency, excellent heat resistance and the like, so that the diamond semiconductor represents the future development direction of the semiconductor industry and is considered as one of fourth-generation semiconductor materials.
The mass production of various devices from semiconductor wafers involves many ultra-precision processing techniques, in which subtractive processing is an indelible process. However, the existing subtractive processing techniques cannot be applied to diamond semiconductors with ultra-high hardness and extremely inert chemical properties. Therefore, the development of new material reduction processing technology is one of the important points in the field of diamond semiconductor manufacturing. In this regard, new technologies have been proposed in the industry over the years, and the following types can be roughly classified from the processing machine:
(1) chemical mechanical polishing or buffing. Patents CN200810010281.3, cn202010115126.9cn201910387112.x, CN201010267938.1, CN200610134176.1 disclose that diamond films can be physically ground by using solid rare earth or hard solid substance containing diamond particles as a polishing disk. Patents CN201710679963.2, CN200310111774.3 and CN201010273591.1 report that diamond films can also be immersed in an oxidizing agent in a molten state at a high temperature on a polishing disk, and the two are subjected to a thermochemical oxidation reaction while the diamond film is subjected to thermochemical mechanical polishing by using diamond abrasives. In addition, the technical solutions adopted in the patents CN200410050364.7 and CN201210196311.0 are to vacuumize the polishing chamber, introduce active gas (e.g. oxygen) into the outer cover of the vacuum polishing chamber, chemically oxidize the diamond film at high temperature, and then remove the oxide by mechanical polishing.
(2) And (4) plasma etching. The technical proposal of patents CN98122855.0, CN200510019473.7, CN200710053016.9, CN201811618654.5 and CN20151062458. X is to ionize pure oxygen or gas containing fluorine or chlorine by adopting ultra-high voltage of more than 1000V in high vacuum to generate highly corrosive ions to etch diamond.
(3) And (5) laser etching. Patents CN201910397980.6, CN201810742445.5 and cn202010200371.x are directed to machining diamond material by high temperature cauterization using high energy laser beams.
(4) And (4) electric heating etching. The technical scheme of patent CN99104906.3 is to coat a conductive metal layer on the surface of a diamond film, and then to heat the diamond film by electrifying to realize electrothermal etching.
Therefore, the above techniques need to be performed under very high temperature and normal pressure, and expensive equipment and complex process flow are needed to oxidize or decompose the diamond, so as to achieve the purpose of material reduction processing. Therefore, how to provide a method for electrochemically etching a diamond semiconductor film, simplify processing equipment, and efficiently etch the diamond semiconductor film at normal temperature and normal pressure is a difficult problem to be solved in the field.
Disclosure of Invention
In view of the above, the invention provides a method for electrochemically etching a diamond semiconductor film, which does not involve extreme conditions such as high-temperature high-pressure vacuum and the like, has no harsh requirements on experimental equipment and experimental environment, and can realize high-efficiency etching of the diamond semiconductor film.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for electrochemically etching a diamond semiconductor film comprises the following specific operation steps: immersing the diamond semiconductor film into electrolyte as the cathode of an electrolytic cell, adopting an inert electrode as the anode of the electrolytic cell, and applying current between the anode and the cathode to etch the diamond film.
Preferably, the diamond semiconductor film is a diamond semiconductor film doped with one or two of boron and nitrogen.
Preferably, the area of the cathode plate is 1cm2In the above, the area of the anode plate is more than 2 times of the area of the cathode plate.
Preferably, the electrolyte contains iron ions, and the concentration of the iron ions is 5mmol/L or more.
Preferably, the current applied between the cathode and the anode is direct current.
Preferably, the applied direct current is a direct current in a constant voltage mode or a direct current in a unipolar pulse mode, and the direct current voltage is 15-50V.
Preferably, the diamond semiconductor film is connected to a power source through an electrode holder.
Preferably, the electrode clamp is an alloy electrode clamp formed by one or more of platinum, tantalum, ruthenium, iridium and titanium, and the electrode clamp is in conductive connection with the diamond semiconductor film.
Preferably, the anode electrode material of the electrolytic cell is graphite.
Preferably, the anode electrode material of the electrolytic cell is an alloy formed by one or more of platinum, tantalum, ruthenium, iridium and titanium.
The invention is based on a new principle of etching a diamond semiconductor film by electrochemical plasma, namely: forming a hydrogen thin layer with a micron scale on the surface of the cathode of the diamond semiconductor film by electrochemically electrolyzing water; when the area of the anode of the electrolytic cell is large enough and the electric conductance of the electrolyte is high enough, the applied direct current voltage is almost completely and directly loaded on the hydrogen thin layer, and extremely high electric field intensity is formed in the micron-scale thin gas layer, so that the thin gas layer is ionized to form a plasma layer. Because one side of the plasma layer is the surface of the diamond semiconductor film connected with the cathode of the external direct current power supply, and the other side is electrolyte equivalent to the anode, iron ions with positive charges on the interface of the electrolyte/ionization layer become high-kinetic energy ions under the acceleration of an ultra-strong electric field in the ionization layer and bombard the surface of the diamond semiconductor film; diamond openable by each high kinetic iron ionsp3The purpose of high-efficiency etching is achieved by the hybridized carbon-carbon bond.
According to the technical scheme, compared with the prior art, the invention has the following beneficial effects:
the novel method for processing the diamond semiconductor film by electrochemical etching is provided, does not relate to extreme conditions such as high-temperature high-pressure vacuum and the like, and has no strict requirements on experimental equipment and experimental environment; the diamond semiconductor can be etched by adopting simple equipment at normal temperature and normal pressure in one step; each high kinetic energy iron ion can open sp of diamond3The hybridized carbon-carbon bond realizes the high-efficiency etching of the diamond semiconductor film.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
FIG. 1 is a schematic diagram of an etching apparatus used in an embodiment of the present invention;
FIG. 2 is a scanning electron micrograph of a boron-doped diamond semiconductor film used in example 1 of the present invention before etching;
FIG. 3 is a scanning electron micrograph of a boron-doped diamond semiconductor thin film after etching, which is used in example 1 of the present invention;
FIG. 4 is a scanning electron micrograph of a boron-doped diamond semiconductor film used in example 2 of the present invention before etching;
FIG. 5 is a scanning electron micrograph of a boron-doped diamond semiconductor film used in example 2 of the present invention after etching.
Detailed Description
The invention provides a method for electrochemically etching a diamond semiconductor film, which comprises the following specific operation steps:
immersing the diamond semiconductor film into electrolyte as the cathode of an electrolytic cell, adopting an inert electrode as the anode of the electrolytic cell, and applying current between the anode and the cathode to etch the diamond film.
In the present invention, the diamond semiconductor film is preferably a diamond semiconductor film doped with one or both of boron and nitrogen elements, and more preferably a diamond semiconductor film doped with a boron element.
In the present invention, the electrolyte contains iron ions, and the concentration of iron ions is preferably 5mmol/L or more, and more preferably 50 mmol/L.
In the present invention, the area of the anode plate is preferably 1cm2Above, more preferably 1cm2(ii) a The area of the anode plate is more than 2 times of the area of the cathode plate, and preferably the area of the anode plate is 100 times of the area of the cathode plate.
In the present invention, the current applied between the anode and the cathode is a direct current, and the applied direct current is preferably a direct current in a constant voltage mode or a direct current in a unipolar pulse mode, and more preferably a direct current in a constant voltage mode.
In the present invention, the voltage of the direct current is preferably 15 to 50V, more preferably 25 to 40V, and still more preferably 30V.
In the present invention, the diamond semiconductor thin film is connected to a power supply through an electrode holder, the electrode holder is an alloy electrode holder formed by one or more of platinum, tantalum, ruthenium, iridium and titanium, the electrode holder is preferably further preferably a metal platinum electrode holder, and the electrode holder is in conductive connection with the diamond semiconductor thin film.
In the invention, the material of the anode electrode of the electrolytic cell is graphite or an alloy formed by one or more of platinum, tantalum, ruthenium, iridium and titanium, and graphite is further preferable.
In the invention, the anode plate is a thin sheet, the cathode plate and the anode plate are arranged in parallel, and the distance between the cathode and the anode is 3-9 cm, preferably 3-6 cm, and further preferably 3 cm.
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The etching time is not limited, and the types of the electrolytes adopted in the following embodiments are all convenient for experiments and are not considered to be limited.
Example 1
Clamping with a platinum electrode clamp of 1 × 1cm in size2The platinum sheet in the electrode clamp is directly in conductive contact with the surface of the diamond semiconductor film; according to the schematic diagram of the etching device adopted in fig. 1, a platinum electrode clamp is connected with the negative electrode of a direct current power supply, so that a diamond semiconductor film is used as the cathode of an electrochemical electrolytic cell; another 10X 10cm2The flake graphite electrode is connected with the positive electrode of a direct current power supply and is used as the anode of an electrochemical electrolytic cell, and the anode and the cathode are parallelly placed in a container, and the distance between the anode and the cathode is fixed to be 3 cm; adding a sulfuric acid solution containing 50mmol/L of iron ions into the container to serve as an electrolyte, and immersing the diamond semiconductor film; turning on a direct current power supply to adjust the voltage to a constant voltage mode, and etching for 1 hour at constant voltage of 30V; and (4) closing the direct current power supply after etching, taking out the diamond semiconductor film, cleaning the diamond semiconductor film by using clear water, and drying the diamond semiconductor film by using nitrogen. Comparing the electron scanning micrographs before (figure 2) and after (figure 3) the etching of the diamond semiconductor film, it can be seen that the surface morphology of the diamond semiconductor film is significantly changed after the etching, the existing grain boundary in figure 2 is obviously disappeared in figure 3, and the surface becomes smoother after the etching.
Example 2
Clamping with a platinum electrode clamp of 1 × 1cm in size2The platinum sheet in the electrode clamp is directly in conductive contact with the surface of the diamond semiconductor film; according to the schematic diagram of the etching device adopted in fig. 1, a platinum electrode clamp is connected with the negative electrode of a direct current power supply, so that a diamond semiconductor film is used as the cathode of an electrochemical electrolytic cell; another 10X 10cm2The flake graphite electrode is connected with the positive electrode of a direct current power supply and used as the anode of an electrochemical electrolytic cell, and the anode and the cathode are connectedThe two electrodes are parallelly arranged in a container, and the distance between the two electrodes is fixed to be 3 cm; adding a sulfuric acid solution containing 5mmol/L iron ions into the container to serve as an electrolyte, and immersing the diamond semiconductor film; turning on a direct current power supply to adjust to a unipolar pulse mode, fixing the voltage at 30V and fixing the pulse frequency at 1 Hz; etching for 1 hour; and (4) closing the direct current power supply after etching, taking out the diamond semiconductor film, cleaning the diamond semiconductor film by using clear water, and drying the diamond semiconductor film by using nitrogen. And fig. 5 is an electron scanning micrograph of the surface of the diamond semiconductor film after etching, and compared with fig. 4, the surface of the diamond semiconductor film after etching is etched with a plurality of nano-scale pits, so that the surface of the diamond semiconductor film is etched.
Example 3
Clamping with a platinum electrode clamp of 2cm2The platinum sheet in the electrode clamp is directly in conductive contact with the surface of the diamond semiconductor film; according to the schematic diagram of the etching device adopted in fig. 1, a platinum electrode clamp is connected with the negative electrode of a direct current power supply, so that a diamond semiconductor film is used as the cathode of an electrochemical electrolytic cell; another 50cm2The titanium platinum ruthenium alloy sheet-shaped mesh electrode is connected with the positive electrode of a direct current power supply to be used as the anode of an electrochemical electrolytic cell, and the anode and the cathode are arranged in a container in parallel, and the distance between the anode and the cathode is fixed to be 9 cm; adding hydrochloric acid solution containing 70mmol/L iron ions into the container as electrolyte, and immersing the diamond semiconductor film; turning on a direct current power supply to adjust the voltage to a constant voltage mode, and etching for 2 hours at a constant voltage of 15V; and (4) closing the direct current power supply after etching, taking out the diamond semiconductor film, cleaning the diamond semiconductor film by using clear water, and drying the diamond semiconductor film by using nitrogen. The surface appearance of the diamond semiconductor film is obviously changed after being etched, and the surface becomes smoother after being etched.
Example 4
Clamping with a platinum electrode clamp of 2cm2The platinum sheet in the electrode clamp is directly in conductive contact with the surface of the diamond semiconductor film; according to the schematic diagram of the etching device adopted in fig. 1, a platinum electrode clamp is connected with the negative electrode of a direct current power supply, so that a diamond semiconductor film is used as the cathode of an electrochemical electrolytic cell; another 4cm2Sheet-like titaniumThe tantalum alloy electrode is connected with the positive electrode of a direct current power supply and is used as the anode of an electrochemical electrolytic cell, and the anode and the cathode are placed in a container in parallel, and the distance between the anode and the cathode is fixed to be 6 cm; adding a sulfuric acid solution containing 50mmol/L of iron ions into the container to serve as an electrolyte, and immersing the diamond semiconductor film; turning on a direct current power supply to adjust the voltage to a constant voltage mode, and etching for 1.5 hours at a constant voltage of 50V; and (4) closing the direct current power supply after etching, taking out the diamond semiconductor film, cleaning the diamond semiconductor film by using clear water, and drying the diamond semiconductor film by using nitrogen. The surface appearance of the diamond semiconductor film is obviously changed after being etched, and the surface becomes smoother after being etched.
When the concentration of the iron ions is 50mmol/L, the etching is more violent and effective, the etching depth is deeper within the same time, and the surface obtained by etching is smoother.
The embodiments in the present description are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (8)
1. A method for electrochemically etching a diamond semiconductor film is characterized in that: the method comprises the following specific steps: immersing the diamond semiconductor film into electrolyte as a cathode of an electrolytic cell, adopting an inert electrode as an anode of the electrolytic cell, and applying current between the anode and the cathode to etch the diamond film;
the area of the anode plate is more than 2 times of that of the cathode plate;
the anode and the cathode are arranged in parallel, and the distance is 3-9 cm;
the electrolyte contains iron ions, and the concentration of the iron ions is more than 5 mmol/L.
2. The method for electrochemically etching a diamond semiconductor film according to claim 1, characterized in that: the diamond semiconductor film is a diamond semiconductor film doped with one or two of boron and nitrogen elements.
3. A method of electrochemically etching a diamond semiconductor film according to claim 1 or 2, characterized in that: the current applied between the anode and cathode is direct current.
4. A method of electrochemically etching a diamond semiconductor film according to claim 3, wherein: the applied direct current is direct current in a constant voltage mode or direct current in a unipolar pulse mode, and the voltage of the direct current is 15-50V.
5. A method of electrochemically etching a diamond semiconductor film according to claim 1 or 2, characterized in that: the diamond semiconductor film is connected with a power supply through an electrode clamp.
6. The method for electrochemically etching a diamond semiconductor film according to claim 5, wherein: the electrode clamp is an alloy electrode clamp formed by one or more of platinum, tantalum, ruthenium, iridium and titanium, and is in conductive connection with the diamond semiconductor film.
7. A method of electrochemically etching a diamond semiconductor film according to any one of claims 1, 2 or 4, wherein: the anode electrode material of the electrolytic cell is graphite.
8. A method of electrochemically etching a diamond semiconductor film according to any one of claims 1, 2 or 4, wherein: the anode electrode material of the electrolytic cell is one of platinum, tantalum, ruthenium and iridium or an alloy formed by more than two of platinum, tantalum, ruthenium, iridium and titanium.
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| GB1154934A (en) * | 1966-06-17 | 1969-06-11 | Gen Electric & English Elect | Improvements in or relating to the Surface Treatment of Silicon Carbide Crystals |
| CN1163948A (en) * | 1995-10-17 | 1997-11-05 | 佳能株式会社 | Etching method, process for producing semiconductor element using said etching method |
| CN1962431A (en) * | 2006-11-09 | 2007-05-16 | 北京科技大学 | Cathode gas film microarc discharging method for preparing carbon nanometer material in solution |
| CN101358356A (en) * | 2008-07-18 | 2009-02-04 | 武汉工程大学 | Method for preparing high specific surface diamond electrode |
| CN101880907A (en) * | 2010-07-07 | 2010-11-10 | 厦门大学 | Electrochemical levelling and polishing processing method with nanometer precision and device thereof |
| CN104164690A (en) * | 2014-06-19 | 2014-11-26 | 北京科技大学 | Method for large-area deposition of coating and surface modification by cathodic plasma electrolysis |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110127881A (en) * | 2019-05-31 | 2019-08-16 | 山东省科学院海洋仪器仪表研究所 | A kind of diamond thin purifier and its preparation method and application |
| CN110540200A (en) * | 2019-09-11 | 2019-12-06 | 河南工业大学 | method for etching diamond (100) surface in high orientation |
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1154934A (en) * | 1966-06-17 | 1969-06-11 | Gen Electric & English Elect | Improvements in or relating to the Surface Treatment of Silicon Carbide Crystals |
| CN1163948A (en) * | 1995-10-17 | 1997-11-05 | 佳能株式会社 | Etching method, process for producing semiconductor element using said etching method |
| CN1962431A (en) * | 2006-11-09 | 2007-05-16 | 北京科技大学 | Cathode gas film microarc discharging method for preparing carbon nanometer material in solution |
| CN101358356A (en) * | 2008-07-18 | 2009-02-04 | 武汉工程大学 | Method for preparing high specific surface diamond electrode |
| CN101880907A (en) * | 2010-07-07 | 2010-11-10 | 厦门大学 | Electrochemical levelling and polishing processing method with nanometer precision and device thereof |
| CN104164690A (en) * | 2014-06-19 | 2014-11-26 | 北京科技大学 | Method for large-area deposition of coating and surface modification by cathodic plasma electrolysis |
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