CN114134569B - Cu-SnO 2 Single crystal film, preparation method and application thereof - Google Patents

Cu-SnO 2 Single crystal film, preparation method and application thereof Download PDF

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CN114134569B
CN114134569B CN202111449351.7A CN202111449351A CN114134569B CN 114134569 B CN114134569 B CN 114134569B CN 202111449351 A CN202111449351 A CN 202111449351A CN 114134569 B CN114134569 B CN 114134569B
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metal electrode
electrode layer
film
substrate
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CN114134569A (en
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何云斌
黎明锴
刘凤新
卢寅梅
陈剑
尹向阳
郭启利
李永昌
刘伟
邓云
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Hubei University
Mornsun Guangzhou Science and Technology Ltd
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Mornsun Guangzhou Science and Technology Ltd
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    • C30B1/00—Single-crystal growth directly from the solid state
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Abstract

The invention discloses a Cu-SnO 2 A monocrystalline film, a preparation method and application thereof relate to the technical field of semiconductors. The Cu-SnO provided by the invention 2 The preparation method of the monocrystalline film comprises the following steps: preparation of Cu-SnO 2 A ceramic target; providing a substrate using Cu-SnO 2 Preparing Cu-SnO on the surface of the substrate by using a ceramic target material 2 A thin film layer; in the atmosphere of oxygen, to Cu-SnO 2 Film annealing, and finally annealing Cu-SnO 2 Film Process O 2 And (5) plasma treatment. Cu-SnO of the invention 2 The single crystal film is used as a semiconductor layer to prepare a Schottky diode, the Schottky contact between the metal electrode and the tin dioxide single crystal film can be realized, and the designed annular electrode can adjust the size of leakage current by adjusting the distance between the two metal electrodes, so that the reverse withstand voltage value of the diode is adjusted. Cu-SnO prepared by the invention 2 Schottky diodes have a high schottky barrier height, good rectifying characteristics, and a high reverse breakdown voltage.

Description

Cu-SnO 2 Single crystal film, preparation method and application thereof
Technical Field
The invention relates to the technical field of semiconductors, in particular to a Cu-SnO 2 Single crystal thin film, preparation method and application thereof, and particularly Cu-SnO 2 The monocrystalline film is used as a semiconductor layer in a schottky diode.
Background
SnO 2 As a typical direct band gap wide bandgap semiconductor material, the material has the characteristics of a forbidden band width of 3.6eV, very high permeability to visible light, rich earth reserves and the like, compared with other wide bandgap semiconductor materials, snO 2 The semiconductor power device has the advantages of stable physical and chemical properties, high mechanical strength, high electron mobility and the like, and has great application potential in the field of semiconductor power devices. Metals and snos having high work functions have long been known 2 The type of contact tends to be ohmic, i.e. metal and SnO 2 The schottky contact is formed, and the problems of lower schottky barrier, large ideal factor, low rectification ratio and the like still exist. Furthermore, snO for the preparation of Schottky diodes 2 The film is polycrystalline or amorphous, and the uneven distribution of the Schottky barrier can cause larger reverse leakage current, which is unfavorable for SnO 2 The reverse breakdown voltage of the schottky diode is improved. Due to metal and SnO 2 Poor Schottky contact quality, leading to current improvements in SnO 2 The performance of schottky diodes has great limitations and is difficult to be studied and applied in the field of semiconductor power devices.
For the current SnO 2 The schottky diode has the defects of low schottky barrier height, low rectification ratio, low reverse breakdown voltage and the like, and is necessary to solve the existing SnO 2 Schottky diodes are improved.
Disclosure of Invention
In view of this, it is possible,the invention provides a Cu-SnO 2 Monocrystalline film, preparation method thereof and application thereof in Schottky diode to solve the problem of SnO shortage in the prior art 2 Single crystal thin film, snO 2 The schottky diode has the defects of low schottky barrier height, low rectification ratio, low reverse breakdown voltage and the like.
In one aspect, the present invention provides a Cu-SnO 2 A method for producing a single crystal thin film, comprising:
preparation of Cu-SnO 2 A ceramic target;
providing a substrate using Cu-SnO 2 Preparing Cu-SnO on the surface of the substrate by using a ceramic target material 2 A thin film layer;
in the atmosphere of oxygen, to Cu-SnO 2 Annealing the film, and finally annealing the annealed Cu-SnO 2 Film Process O 2 Plasma treatment to obtain Cu-SnO 2 A single crystal thin film.
Optionally, the Cu-SnO 2 The preparation method of the ceramic target comprises the following steps:
SnO is prepared 2 Mixing the powder with CuO powder, ball milling, and drying to obtain mixed powder;
pressing the mixed powder into Cu-SnO 2 Ceramic green sheets;
in an oxygen atmosphere, cu-SnO is treated in a vacuum tube furnace at the temperature of 700-1300 DEG C 2 Sintering the ceramic green sheet to obtain Cu-SnO 2 And (3) a target material.
Optionally, the SnO 2 The molar ratio of the powder to the CuO powder is 99:1-90:10. In one embodiment of the invention, the SnO 2 The molar ratio of powder to CuO powder was 99:1.
Optionally, the mixed powder is pressed into a ceramic blank under the pressure of 3-5 MPa, wherein the thickness of the ceramic blank is 2-4 mm, and the diameter of the ceramic blank is 2-4 cm.
Specifically, the substrate comprises a sapphire substrate, a quartz glass substrate, a silicon substrate, a GaN substrate and Nb-doped SrTiO 3 Substrate, mgO substrate, ga 2 O 3 A substrate or the like, the main component of which is alumina (Al 2 O 3 ). At the bookIn one embodiment of the invention, the substrate is a c-plane sapphire substrate.
Optionally, before the substrate is placed in the vacuum cavity of the pulse laser deposition system, the substrate is cleaned by acetone, absolute ethyl alcohol and deionized water in sequence.
In particular, the use of Cu-SnO 2 Preparing Cu-SnO on the surface of the substrate by using a ceramic target material 2 The method of the film layer comprises sol-gel method, spray pyrolysis method, chemical vapor deposition method, molecular beam epitaxy growth, magnetron sputtering method, pulse laser deposition method, ion beam coating, vacuum evaporation coating, etc.
In one embodiment of the invention, cu-SnO is prepared by pulse laser deposition 2 The film layer comprises the following specific processes: placing the substrate in a vacuum cavity of a pulse laser deposition system, heating the substrate to 300-1000 ℃, then introducing oxygen into the vacuum cavity, regulating the pressure of a growth chamber to 0-5 Pa, and utilizing Cu-SnO 2 The ceramic target material is prepared on the substrate by adopting a pulse laser ablation method to obtain Cu-SnO 2 A thin film layer.
Alternatively, to Cu-SnO 2 Film annealing is to anneal Cu-SnO in a vacuum tube furnace 2 The film is put in oxygen atmosphere and is heated to 600 ℃ for Cu-SnO 2 And annealing the film for 10-120 min.
Optionally, for annealed Cu-SnO 2 Film Process O 2 The plasma treatment specifically includes: the Cu-SnO is treated with 2 Placing the film horizontally in a plasma cleaner, pumping the plasma cleaner to a vacuum state below 1Pa, then introducing oxygen into the vacuum cavity, adjusting the pressure in the cavity to be 1-10 Pa, and selecting output power to Cu-SnO 2 Film Process O 2 And (5) plasma treatment.
Alternatively, to Cu-SnO 2 Film Process O 2 The output power of the plasma treatment may optionally range from 10 to 1000W. In one embodiment of the invention, an output power of 29.6W is selected.
In a second aspect, the present invention also provides a Cu-SnO 2 A single crystal thin film using the aboveThe preparation method is used for preparing the product.
In a third aspect, the present invention also provides the Cu-SnO 2 Use of single crystal thin films in schottky diodes.
In a fourth aspect, the present invention also provides a Cu-SnO 2 A schottky diode comprising:
a substrate;
Cu-SnO 2 a monocrystalline film layer located on the surface of the substrate;
a first metal electrode layer positioned on Cu-SnO 2 The monocrystalline film layer is far away from the substrate;
a second metal electrode layer with the same ring center as the first metal electrode layer and located at Cu-SnO 2 The monocrystalline film layer is far away from the part of the substrate side which is not covered by the first metal electrode layer.
Specifically, the Cu-SnO 2 The single crystal film layer is made of Cu-SnO according to the invention 2 The monocrystalline film is prepared by a preparation method.
Optionally, the Cu-SnO 2 The thickness of the monocrystalline film layer is 10-3000 nm.
Optionally, the thickness of the first metal electrode layer is 30-300 nm, and the thickness of the second metal electrode layer is 30-100 nm.
Optionally, the first metal electrode layer comprises a high work function metal such as platinum, gold, nickel and the like in a selectable range; in one embodiment of the invention, the first metal electrode layer is a platinum electrode layer.
Optionally, the optional range of the second metal electrode layer includes low work function metals such as titanium, aluminum, copper, indium, silver, tin, and the like, and in one embodiment of the present invention, the second metal electrode layer is an aluminum electrode layer.
Optionally, the shape of the first metal electrode layer may be selected from square, rectangle, circle, triangle, etc.; in one embodiment of the invention, the first metal electrode layer is circular in shape, and the center of the circle is located in Cu-SnO 2 The monocrystalline film layer is remote from the center of the substrate side surface.
Optionally, the shape selectable range of the second metal electrode layer comprises a ring shape corresponding to the shape of the first metal electrode layer, the center of the ring is the same as the center of the first metal electrode layer, and the inner diameter is larger than the diameter of the first metal electrode layer; in one embodiment of the present invention, the second metal electrode layer is in a shape of a ring, and the center of the circle is the same as the center of the circle of the first metal electrode layer, and the inner diameter is larger than the inner diameter of the first metal electrode layer.
In a fifth aspect, the present invention also provides the Cu-SnO 2 The preparation method of the Schottky diode comprises the following steps:
at the Cu-SnO 2 Preparing a first metal electrode layer on the surface of one side of the monocrystalline film layer, which is far away from the substrate;
at the Cu-SnO 2 Preparing a second metal electrode layer on the part, which is far away from the substrate, of the monocrystalline film layer and is not covered by the first metal electrode layer; wherein:
the Cu-SnO 2 The single crystal film is made of Cu-SnO according to the invention 2 The monocrystalline film is prepared by a preparation method.
Optionally, in the Cu-SnO 2 The process for preparing the first metal electrode layer on the surface of the monocrystalline film layer far away from the substrate specifically comprises the following steps: using a spin coater to mix Cu-SnO 2 Preparing uniform photoresist film on the surface of the monocrystalline film layer far away from the substrate, copying the pattern on the mask onto the photoresist film by using the mask with circular pattern and photoetching technology, and preparing Cu-SnO 2 Preparing a first metal electrode layer on the surface of the monocrystalline film layer far away from the substrate and the surface of the photoresist film far away from the substrate, and dissolving the photoresist film with acetone solution to obtain Cu-SnO 2 The monocrystalline film layer is far away from the first metal electrode layer on one side surface of the substrate.
Alternatively, in Cu-SnO 2 The process for preparing the second metal electrode layer by the surface part of the monocrystalline film layer, which is far away from the side of the substrate and is not covered by the first metal electrode layer, specifically comprises the following steps: using a spin coater to mix Cu-SnO 2 Preparing uniform photoresist film on the surface of the monocrystalline film layer and the first metal electrode layer far away from the substrate, and masking by using a mask plate with a circular pattern and a photoetching technologyThe pattern on the mask is copied to the photoresist film, and the pattern is formed on Cu-SnO 2 Preparing a second metal electrode layer on the surface of the monocrystalline film layer far away from the substrate and the surface of the photoresist film far away from the substrate, and dissolving the photoresist film with acetone solution to obtain Cu-SnO 2 And a second metal electrode layer of a surface portion of the monocrystalline film layer, which is not covered by the first metal electrode layer, on a side away from the substrate.
Optionally, the Cu-SnO 2 The method for preparing the first metal electrode layer and the second metal electrode layer on the surface of the monocrystalline film layer far away from the substrate comprises chemical vapor deposition, physical vapor deposition, vacuum evaporation and the like.
Cu-SnO of the invention 2 Compared with the prior art, the monocrystalline film and the preparation method and application thereof have the following beneficial effects:
(1) Cu-SnO of the invention 2 Schottky diode, cu-SnO 2 A monocrystalline film layer as the semiconductor layer, wherein acceptor doping of Cu partially counteracts n-type SnO 2 Background electrons in (D), follow-up O 2 The plasma treatment reduces SnO 2 Oxygen vacancy concentration in (a), both of which are effective in reducing SnO 2 The background carrier concentration of the substrate is used for achieving the purpose of achieving good Schottky contact; the first metal electrode layer is higher than SnO 2 Work function of (C) and Cu-SnO 2 The single crystal film layers form Schottky contact, and the second metal electrode layer is lower than SnO 2 Work function of (C) and Cu-SnO 2 Ohmic contact is formed between the monocrystalline film layers, cu-SnO 2 Schottky diodes have lower reverse leakage current and higher reverse breakdown voltage.
(2) Cu-SnO of the invention 2 The Schottky diode adopts the photoetching technology to precisely control the size and the distance between the first metal electrode layer and the second metal electrode layer, and the annular second metal electrode layer is beneficial to dispersing the electric field intensity of the edges of the metal electrodes when reverse bias voltage is applied, thereby improving Cu-SnO 2 Reverse breakdown voltage of schottky diode. While the inner ring of the second metal electrode layer is connected with the first metalBetween the circumferences of the electrode layers is a voltage-resistant region, thereby realizing the increase of Cu-SnO by adjusting the width of the voltage-resistant region 2 A method for reverse breakdown voltage of schottky diode.
(3) Cu-SnO of the invention 2 The Schottky diode grows by adopting the conventional pulse laser deposition technology, has simple equipment and operation process and is easy to control Cu-SnO 2 Growth quality of thin film layer, metal electrode and Cu-SnO 2 The single crystal thin film layer has a high quality contact.
(4) The invention realizes the Schottky contact of the metal and the tin dioxide monocrystal film, and the designed annular electrode can adjust the size of leakage current by adjusting the distance between the two metal electrodes, thereby adjusting the reverse withstand voltage value of the diode. Cu-SnO prepared by the invention 2 Schottky diodes have a high schottky barrier height, good rectifying characteristics, and a high reverse breakdown voltage.
Drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions in the prior art, the following description will briefly explain the drawings used in the embodiments or the description of the prior art, and it is obvious that the drawings in the following description are only some embodiments of the invention, and that other drawings can be obtained according to these drawings without inventive effort to a person skilled in the art.
FIG. 1 shows Cu-SnO obtained in example 1 of the present invention 2 XRD full spectrum of single crystal film layer;
FIG. 2 shows Cu-SnO obtained in example 1 of the present invention 2 XRD rocking plot of single crystal thin film layer;
FIG. 3 shows Cu-SnO obtained in example 1 of the present invention 2 A single crystal thin film layer transmission spectrum;
FIG. 4 shows Cu-SnO obtained in example 1 of the present invention 2 Single crystal thin film layer (alpha h v) 2 A graph of the relationship with the energy of the incident photon;
FIG. 5 shows Cu-SnO prepared in practical example 1 and practical example 2 of the present invention 2 A structural schematic diagram of the schottky diode;
FIG. 6 shows Cu-SnO prepared in practical example 1 and practical example 2 of the present invention 2 A process flow diagram of a schottky diode manufacturing method;
FIG. 7 shows Cu-SnO obtained by the method of application example 1 and application example 2 of the present invention 2 Metal electrode patterns of the schottky diode are (a) and (b), respectively;
FIG. 8 shows Cu-SnO obtained by the method of application example 1 of the present invention 2 A current-voltage plot of a schottky diode;
FIG. 9 shows Cu-SnO obtained by the method of application example 1 of the present invention 2 A current density-voltage plot of a schottky diode;
FIG. 10 shows Cu-SnO obtained by the method of application example 1 of the present invention 2 A current-reverse voltage plot of a schottky diode;
FIG. 11 shows Cu-SnO obtained by the method of application example 2 of the present invention 2 A current-voltage plot of a schottky diode;
FIG. 12 shows Cu-SnO obtained in accordance with application example 2 of the present invention 2 A current density-voltage plot of a schottky diode;
FIG. 13 shows Cu-SnO obtained in accordance with application example 2 of the present invention 2 Current-reverse voltage graph of schottky diode.
Detailed Description
The following description of the embodiments of the present invention will be made in detail and with reference to the embodiments of the present invention, but it should be apparent that the described embodiments are only some embodiments of the present invention, and not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the present invention without making any inventive effort, are intended to fall within the scope of the present invention.
Example 1
Cu-SnO of this embodiment 2 A method for producing a single crystal thin film, comprising the steps of:
s1, providing Cu-SnO 2 A ceramic target;
S2、providing a substrate using Cu-SnO 2 Preparing Cu-SnO on the surface of the substrate by using a ceramic target material 2 A thin film layer;
s3, in the oxygen atmosphere, cu-SnO 2 Annealing the film, and finally annealing the annealed Cu-SnO 2 Film Process O 2 Plasma treatment to obtain Cu-SnO 2 A single crystal thin film.
In particular, in the examples of the present application, cu-SnO 2 The preparation method of the ceramic target comprises the following steps: snO with the molar ratio of 99:1 is weighed 2 The powder and CuO powder are put in a ball milling tank to obtain mixed powder, and then ethanol accounting for 150% of the total mass of the powder is added into the mixed powder for ball milling for 8 hours; placing the ball-milled mixed powder into a vacuum drying oven, and drying for 8 hours at the temperature of 80 ℃; then adding absolute ethanol accounting for 3 percent of the total mass of the powder into the dried powder, grinding and stirring uniformly to obtain ceramic blanks which are mixed and bonded together, and pressing the ceramic blanks into Cu-SnO with the thickness of 3mm and the diameter of 3cm in a tabletting machine under the pressure of 4MPa 2 Ceramic green sheets; in an oxygen atmosphere, in a vacuum tube furnace, the obtained Cu-SnO is treated at 700-1300 DEG C 2 Sintering the ceramic blank to obtain Cu-SnO 2 A ceramic target. The sintering temperature in this application is 1200 ℃.
In the embodiment of the present application, the substrate includes a sapphire substrate, a quartz glass substrate, a silicon substrate, a GaN substrate, and Nb-doped SrTiO 3 Substrate, mgO substrate, ga 2 O 3 A substrate or the like, the main component of which is alumina (Al 2 O 3 ) Specifically, the substrate in the application is a c-plane sapphire substrate.
In the examples of the present application, cu-SnO was prepared 2 The method of the film layer comprises sol-gel method, spray thermal decomposition method, chemical vapor deposition method, molecular beam epitaxy growth, magnetron sputtering method, pulse laser deposition method, ion beam coating, vacuum evaporation coating and the like, and specifically, the pulse laser deposition method is selected to prepare Cu-SnO in the application 2 A thin film layer.
In the embodiment of the application, the sapphire with the c-plane is a substrate for film growth, and the substrate is sequentially coated with the C-plane sapphireCleaning ketone, absolute ethanol, and deionized water for 15min, drying with high-purity nitrogen gas to obtain clean substrate, placing into vacuum cavity of pulse laser deposition system, and vacuumizing to 1×10 -4 Pa, heating the substrate to 700 ℃, and introducing high-purity O 2 In the vacuum cavity, the air pressure of the growth chamber is regulated to be 2Pa, cu-SnO is utilized 2 Cu-SnO is carried out on the substrate by adopting a pulse laser ablation method for the ceramic target material 2 Growing the film to obtain Cu-SnO 2 A thin film layer.
In the examples of the present application, the composition was prepared from Cu-SnO 2 Film annealing is to anneal Cu-SnO in a vacuum tube furnace 2 The film is put in oxygen atmosphere and is heated to 600 ℃ for Cu-SnO 2 And annealing the film for 10-120 min. Specifically, the annealing time selected in the present application is 30min.
In addition, for Cu-SnO after annealing 2 Film Process O 2 The plasma treatment includes: annealing the Cu-SnO 2 Placing the film horizontally in a plasma cleaner, pumping the plasma cleaner to a vacuum state below 1Pa, then introducing oxygen into the vacuum cavity, adjusting the pressure in the cavity to be 1-10 Pa, and selecting output power to Cu-SnO 2 Film Process O 2 And (5) plasma treatment.
Specifically, the pressure in the cavity selected in the embodiment of the application is 3Pa.
Specifically, for annealed Cu-SnO 2 Film Process O 2 An alternative range of output power for the plasma treatment includes 10 to 1000W, with 29.6W being selected for the present application.
Specifically, cu-SnO in the examples of the present application 2 The thickness of the film layer is 500nm, and the film layer is annealed and O 2 Cu-SnO after plasma treatment 2 The thickness of the film layer is not changed.
For Cu-SnO prepared in the examples of the present application 2 The single crystal thin film was subjected to a test for crystallization quality, as shown in FIG. 1, and by phase analysis with XRD, it was revealed that Cu-SnO 2 The single crystal film is a film with a single orientation of a (100) crystal face; as shown in FIG. 2, the XRD rocking curve test shows Cu-SnO 2 The rocking curve full width at half maximum (FWHM) of the single crystal thin film is 0.162 DEG, and has high crystallization quality. As shown in FIG. 3, cu-SnO 2 The transmission spectrum of the single crystal film shows that the transmittance of the film in near ultraviolet and visible wave bands reaches more than 90%, the film has weak light absorption in the wavelength range of 2000-3000nm, and the free carrier concentration in the film is lower. As shown in FIG. 4, cu-SnO 2 The optical band gap of the single crystal film was 4.18eV.
Based on the same inventive concept, the embodiment of the application also provides a Cu-SnO 2 Single crystal thin film of Cu-SnO 2 The monocrystalline film is prepared by adopting the preparation method.
Based on the same inventive concept, the embodiment of the application also provides the Cu-SnO prepared by the method 2 Single crystal film for preparing Cu-SnO 2 Application in schottky diodes.
The following application examples are Cu-SnO obtained in example 1 2 Single crystal film for preparing Cu-SnO 2 A schottky diode.
Application example 1
As shown in FIG. 5, the present invention provides a Cu-SnO 2 The schottky diode includes:
a substrate 1;
Cu-SnO 2 A thin film layer 2 positioned on the surface of the substrate;
third, a first metal electrode layer 3 located at Cu-SnO 2 The side of the film layer 2 far away from the substrate;
fourth, the second metal electrode layer 4, the ring center is the same as the first metal electrode layer 3, is located in Cu-SnO 2 The film layer 2 is remote from the substrate at a portion not covered by the first metal electrode layer.
In the present application, the thickness of the first metal electrode layer 3 is 30 to 300nm, and the thickness of the second metal electrode layer 4 is 30 to 100nm. Specifically, in this application embodiment, the thickness of the first metal electrode layer 3 is 100nm, and the thickness of the second metal electrode layer 4 is 40nm.
In the application embodiment of the present application, the selectable range of the shape of the first metal electrode layer 3 includes square, rectangle, circle, triangle, etc., and the shape of the first metal electrode layer 3 is circular; the optional range of the shape of the second metal electrode layer 4 includes a ring shape corresponding to the shape of the first metal electrode layer 3, and the shape of the second metal electrode layer 4 is a ring shape, and the center of the circle is the same as the center of the circle of the first metal electrode layer 3.
In the application example, the first metal electrode layer 3 and Cu-SnO 2 The film layer 2 forms schottky contact, the optional range of the first metal electrode layer 3 comprises high work function metals such as platinum, gold, nickel and the like, and the first metal electrode layer 3 is a platinum electrode layer.
In the application example, the second metal electrode layer 4 and Cu-SnO 2 The thin film layer 2 forms ohmic contact, the second metal electrode layer 4 can be selected from low work function metals such as titanium, aluminum, copper, indium, silver, tin and the like, and the second metal electrode layer 4 is selected from aluminum.
In the application example of the present application, as shown in FIG. 7 (a), the first metal electrode layer 3 is located at Cu-SnO 2 The surface of the film layer 2 far away from the substrate is round in shape and 3mm in diameter; the second metal electrode layer 4 is positioned at Cu-SnO 2 The surface of the film layer 2, which is far from the substrate and is not covered by the first metal electrode layer, is annular in shape, and has an inner diameter of 3.1mm and an outer diameter of 5mm.
Cu-SnO in application examples of the present application 2 Schottky diode, cu-SnO 2 The film layer is monocrystalline, can form high-quality contact with the first electrode layer, has high stability, and is favorable for improving the Schottky barrier; the circular first metal electrode layer and the circular second metal electrode layer are beneficial to dispersing the electric field intensity of the edges of the metal electrodes and improving Cu-SnO 2 Reverse breakdown voltage of schottky diode.
Based on the same inventive concept, the embodiment of the application also provides the Cu-SnO 2 The preparation method of the schottky diode, as shown in fig. 6, comprises the following steps:
s1, providing Cu-SnO 2 A ceramic target;
s2, providing a substrate, utilizingCu-SnO 2 Preparing Cu-SnO on the surface of the substrate by using a ceramic target material 2 A thin film layer;
s3, pair Cu-SnO 2 Annealing the film, and finally annealing the annealed Cu-SnO 2 Film Process O 2 Plasma treatment to obtain Cu-SnO 2 A single crystal thin film;
s4, at the Cu-SnO 2 Preparing a first metal electrode layer on the surface of one side of the film layer, which is far away from the substrate;
s5 is Cu-SnO 2 Preparing a second metal electrode layer at a part of the side, far away from the substrate, of the film layer, which is not covered by the first metal electrode layer;
in this application embodiment, steps S1, S2, S3 are the same as embodiment 1.
In an application embodiment of the present application, a method for preparing a first metal electrode layer includes:
using a spin coater to mix Cu-SnO 2 Preparing a uniform photoresist film on the surface of the film layer far away from the substrate, copying the pattern on the mask onto the photoresist film by using the mask with circular patterns and the photoetching technology, and forming a Cu-SnO film on the surface of the film layer far away from the substrate 2 Preparing a first metal electrode layer on the surface of the film layer far away from the substrate and the surface of the photoresist film far away from the substrate, dissolving and removing the photoresist film by using acetone solution to obtain Cu-SnO 2 The surface of the thin film layer far from the substrate side is provided with a circular first metal electrode layer, and the diameter of the circular first metal electrode layer is 3mm.
In an application embodiment of the present application, the preparation method of the second metal electrode layer includes:
using a spin coater to mix Cu-SnO 2 Preparing a uniform photoresist film on the surfaces of the film layer and the first metal electrode layer far away from the substrate, copying the pattern on the mask onto the photoresist film by using the mask with circular pattern and the photoetching technology, and forming a Cu-SnO film on the surface of the film layer and the first metal electrode layer far away from the substrate 2 Preparing a second metal electrode layer on the surface of the film layer far away from the substrate and the surface of the photoresist film far away from the substrate, dissolving and removing the photoresist film by using acetone solution to obtain Cu-SnO 2 The surface of the thin film layer, which is far from the substrate and is not covered by the first metal electrode layer, is annularAnd the second metal electrode layer has an inner diameter of 3.1mm and an outer diameter of 5mm.
In the application embodiment of the application, the first metal electrode layer and the second metal electrode layer can be prepared by chemical vapor deposition, physical vapor deposition, evaporation and other methods.
Cu-SnO prepared in example 1 was applied to the present application 2 The performance of the schottky diode was tested as shown in fig. 8, where the current-voltage curve shows Cu-SnO 2 The Schottky diode has good rectifying effect, and the leakage current is 57pA when the starting voltage is 5.7V and the rectifying ratio is 2.4,5V; as shown in fig. 9, the current density-voltage curve shows that the schottky barrier height of the diode is 0.91eV and the ideal factor is 11.28; as shown in fig. 10, a breakdown phenomenon occurs at a reverse bias of 5V; cu-SnO 2 Schottky diodes have a high schottky barrier height and good unidirectional conductivity.
Application example 2
As with application example 1, the present invention provides a Cu-SnO 2 The schottky diode includes:
a substrate 1;
Cu-SnO 2 A thin film layer 2 positioned on the surface of the substrate;
third, a first metal electrode layer 3 located at Cu-SnO 2 The side of the film layer 2 far away from the substrate;
fourth, the second metal electrode layer 4, the ring center is the same as the first metal electrode layer 3, is located in Cu-SnO 2 The film layer 2 is remote from the substrate at a portion not covered by the first metal electrode layer.
In the present application, the thickness of the first metal electrode layer 3 is 30 to 300nm, and the thickness of the second metal electrode layer 4 is 30 to 100nm. Specifically, in this application embodiment, the thickness of the first metal electrode layer 3 is 100nm, and the thickness of the second metal electrode layer 4 is 40nm.
In the application embodiment of the present application, the selectable range of the shape of the first metal electrode layer 3 includes square, rectangle, circle, triangle, etc., and the shape of the first metal electrode layer 3 is circular; the optional range of the shape of the second metal electrode layer 4 includes a ring shape corresponding to the shape of the first metal electrode layer 3, and the shape of the second metal electrode layer 4 is a ring shape, and the center of the circle is the same as the center of the circle of the first metal electrode layer 3.
In the application example, the first metal electrode layer 3 and Cu-SnO 2 The film layer 2 forms schottky contact, the selective range of the first metal electrode layer 3 comprises high work function metals such as platinum, gold, nickel and the like, and the first metal electrode layer 3 is a platinum electrode layer;
in the application example, the second metal electrode layer 4 and Cu-SnO 2 The thin film layer 2 forms ohmic contact, the second metal electrode layer 4 can be selected from low work function metals such as titanium, aluminum, copper, indium, silver, tin and the like, and the second metal electrode layer 4 is selected from aluminum.
Unlike application example 1, in this embodiment, as shown in FIG. 7 (b), the first metal electrode layer 3 is located at Cu-SnO 2 The surface of the film layer 2 far away from the substrate is round in shape and 2mm in diameter; the second metal electrode layer 4 is positioned at Cu-SnO 2 The surface of the film layer 2, which is far from the substrate and is not covered by the first metal electrode layer, is annular in shape, and has an inner diameter of 2.2mm and an outer diameter of 5mm.
Cu-SnO in application examples of the present application 2 Schottky diode, cu-SnO 2 The film layer is monocrystalline, can form high-quality contact with the first electrode layer, has high stability, and is favorable for improving the Schottky barrier; the inner diameter spacing between the circumference of the circular first metal electrode layer and the circular second metal electrode layer is increased, which is beneficial to further improving Cu-SnO 2 Reverse breakdown voltage of the schottky diode reduces reverse leakage current.
As with application example 1, application example 2 of the present application also provides Cu-SnO 2 The preparation method of the Schottky diode comprises the following steps:
s1, providing Cu-SnO 2 A ceramic target;
s2, providing a substrate, utilizing Cu-SnO 2 Preparing Cu-SnO on the surface of the substrate by using a ceramic target material 2 A thin film layer;
S3、for Cu-SnO 2 Annealing the film, and finally annealing the annealed Cu-SnO 2 Film Process O 2 Plasma treatment to obtain Cu-SnO 2 A single crystal thin film;
s4, at the Cu-SnO 2 Preparing a first metal electrode layer on the surface of one side of the film layer, which is far away from the substrate;
s5 is Cu-SnO 2 The part of the film layer, which is far away from the side of the substrate and is not covered by the first metal electrode layer, is used for preparing a second metal electrode layer.
In this application embodiment, steps S1, S2, S3 are the same as embodiment 1.
The difference from application example 1 is that in application example 2 of the present application, the preparation method of the first metal electrode layer includes:
using a spin coater to mix Cu-SnO 2 Preparing a uniform photoresist film on the surface of the film layer far away from the substrate, copying the pattern on the mask onto the photoresist film by using the mask with circular patterns and the photoetching technology, and forming a Cu-SnO film on the surface of the film layer far away from the substrate 2 Preparing a first metal electrode layer on the surface of the film layer far away from the substrate and the surface of the photoresist film far away from the substrate, dissolving and removing the photoresist film by using acetone solution to obtain Cu-SnO 2 The surface of the thin film layer far from the substrate side is provided with a circular first metal electrode layer with a diameter of 2mm.
In an application embodiment of the present application, the preparation method of the second metal electrode layer includes:
using a spin coater to mix Cu-SnO 2 Preparing a uniform photoresist film on the surfaces of the film layer and the first metal electrode layer far away from the substrate, copying the pattern on the mask onto the photoresist film by using the mask with circular pattern and the photoetching technology, and forming a Cu-SnO film on the surface of the film layer and the first metal electrode layer far away from the substrate 2 Preparing a second metal electrode layer on the surface of the film layer far away from the substrate and the surface of the photoresist film far away from the substrate, dissolving and removing the photoresist film by using acetone solution to obtain Cu-SnO 2 And the annular second metal electrode layer of the surface part of the film layer, which is far away from the substrate and is not covered by the first metal electrode layer, has an inner diameter of 2.2mm and an outer diameter of 5mm.
In the application embodiment of the application, the first metal electrode layer and the second metal electrode layer can be prepared by chemical vapor deposition, physical vapor deposition, evaporation and other methods.
Cu-SnO prepared in the application example of the present application 2 The performance of the schottky diode was tested as shown in fig. 11, where the current-voltage curve shows Cu-SnO 2 The Schottky diode has good rectifying effect, and the leakage current is 8.8pA when the starting voltage is 3.28V and the rectifying ratio is 30.3,5V; as shown in fig. 12, the current density-voltage curve shows that the schottky barrier height of the diode is 0.94eV and the ideal factor is 12.24; as shown in FIG. 13, cu-SnO 2 The reverse breakdown voltage of the Schottky diode is larger than 50V, which indicates that increasing the circumference of the circular first metal electrode layer and the inner diameter distance of the annular second metal electrode layer obviously increases the reverse breakdown voltage of the Schottky diode; cu-SnO of the present example 2 The Schottky diode has better Schottky contact and high voltage resistance.
Test of Cu-SnO obtained in example 1 of the present application 2 As a result of XRD total spectrum of the single crystal thin film, as shown in FIG. 1, cu-SnO can be seen from FIG. 1 2 The single crystal film has only (100) crystal plane orientation, and is grown on a sapphire substrate by single crystal epitaxy.
Test of Cu-SnO obtained in example 1 of the present application 2 As a result of the rocking curve of the single crystal thin film, FIG. 2 shows that the rocking curve full width at half maximum (FWHM) is 0.162℃and Cu-SnO is shown in FIG. 2 2 The single crystal thin film has high crystallization quality.
Test of Cu-SnO obtained in example 1 of the present application 2 As a result of the transmission spectrum of the single crystal thin film, as shown in FIG. 3, the transmittance of the thin film in the near ultraviolet visible wavelength band reaches more than 90%, the absorption of light by the thin film in the wavelength range of 2000nm to 3000nm is weak, and the concentration of free carriers in the thin film is low, as shown in FIG. 3.
Test of Cu-SnO obtained in example 1 of the present application 2 Single crystal thin film layer (alpha h v) 2 As a result of the graph showing the relation between the energy of the incident photon and the energy of the incident photon, as shown in FIG. 4, it is apparent from FIG. 4 that the linear region of the curve is extended to obtain the intersection point with the abscissa, and Cu-SnO is known 2 The optical band gap of the film was 4.18eV.
Test of Cu-SnO obtained by applying example 1 of the present application 2 The current-voltage curve of the Schottky diode is shown in FIG. 8, and the result is shown in FIG. 8, in which Cu-SnO is known from FIG. 8 2 The Schottky diode has good rectifying effect, and the leakage current is 57pA when the starting voltage is 5.72V and the rectifying ratio is 2.4,5V.
Test of Cu-SnO obtained by applying example 1 of the present application 2 As shown in fig. 9, the current density-voltage curve of the schottky diode shows that the schottky barrier height of the diode is 0.91eV, the ideal factor is 11.28, indicating cu—sno from fig. 9 2 The schottky barrier height of the schottky diode is high.
Test of Cu-SnO obtained by applying example 1 of the present application 2 As shown in fig. 10, the current-reverse voltage graph of the schottky diode shows that the diode breaks down when the reverse bias voltage is 5V.
Test of Cu-SnO obtained by applying example 2 of the present application 2 The current-voltage curve of the Schottky diode is shown in FIG. 11, and the result is shown in FIG. 11, in which Cu-SnO is known from FIG. 11 2 The Schottky diode has a good rectifying effect, and the leakage current is 8.8pA when the starting voltage is 3.28V and the rectifying ratio is 30.3,5V.
Test of Cu-SnO obtained by applying example 2 of the present application 2 As shown in fig. 12, the current density-voltage curve of the schottky diode shows that the schottky barrier height of the diode is 0.94eV, the ideal factor is 12.24, indicating cu—sno from fig. 12 2 The schottky barrier height of the schottky diode is high.
Test of Cu-SnO obtained by applying example 2 of the present application 2 As shown in fig. 13, the reverse breakdown voltage of the schottky diode is greater than 50v, and the reverse breakdown voltage of cu-SnO is greater than 50v, as shown in fig. 13 2 The reverse breakdown voltage value of the schottky diode is raised by at least one order of magnitude.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, alternatives, and improvements that fall within the spirit and scope of the invention.

Claims (7)

1. Cu-SnO 2 The preparation method of the monocrystalline film is characterized in that: the method comprises the following steps:
preparation of Cu-SnO 2 A ceramic target;
providing a substrate, depositing Cu-SnO by pulse laser 2 Preparing Cu-SnO on the surface of the substrate by using a ceramic target material 2 A thin film layer; the temperature of the substrate is 700 ℃;
in the atmosphere of oxygen, to Cu-SnO 2 Annealing the film, and finally annealing the annealed Cu-SnO 2 Film Process O 2 Plasma treatment to obtain Cu-SnO 2 A single crystal thin film; wherein:
the pair of Cu-SnO 2 Film annealing is to anneal Cu-SnO in a vacuum tube furnace 2 The film is placed in an oxygen atmosphere at 600 ℃ for Cu-SnO 2 Annealing the film for 10-120 min;
the Cu-SnO 2 The preparation method of the ceramic target comprises the following steps:
SnO is prepared 2 Mixing the powder with CuO powder, ball milling, and drying to obtain mixed powder; wherein: the SnO 2 The molar ratio of the powder to the CuO powder is 99:1-90:10;
pressing the mixed powder into Cu-SnO 2 Ceramic green sheets;
in an oxygen atmosphere, in a vacuum tube furnace, cu-SnO is treated at a temperature of 700-1300 DEG C 2 Sintering the ceramic green sheet to obtain Cu-SnO 2 And (3) a target material.
2. The Cu-SnO of claim 1 2 Cu-SnO prepared by preparation method of monocrystalline film 2 A single crystal thin film.
3. The Cu-SnO prepared by the method of claim 1 2 Use of single crystal thin films in schottky diodes.
4.Cu-SnO 2 Schottky diode, its characterized in that: comprising the following steps:
a substrate;
Cu-SnO 2 a monocrystalline film layer located on the surface of the substrate;
a first metal electrode layer positioned on Cu-SnO 2 The monocrystalline film layer is far away from the substrate;
a second metal electrode layer with the same ring center as the first metal electrode layer and located at Cu-SnO 2 A portion of the monocrystalline film layer, which is far away from the substrate side and is not covered by the first metal electrode layer;
wherein: the Cu-SnO 2 A monocrystalline film layer produced by the method of claim 1;
the first metal electrode layer selectable range includes platinum, gold, or nickel; the second metal electrode layer can be selected from titanium, aluminum, copper, indium, silver or tin; the first metal electrode layer and Cu-SnO 2 Forming Schottky contact between the monocrystalline film layers; the second metal electrode layer and Cu-SnO 2 Ohmic contact is formed between the monocrystalline film layers.
5. The Cu-SnO of claim 4 2 Schottky diode, its characterized in that: the Cu-SnO 2 The thickness of the monocrystalline film layer is 10-3000 nm; the thickness of the first metal electrode layer is 30-300 nm, and the thickness of the second metal electrode layer is 30-100 nm.
6. The Cu-SnO of claim 4 2 Schottky diode, its characterized in that: the shape of the first metal electrode layer can be selected from square, rectangle, round and triangle; the shape of the second metal electrode layer can be selected from the range including a ring shape corresponding to the shape of the first metal electrode layer, and the inner diameter is larger than the diameter of the first metal electrode layer.
7. The Cu-SnO of any of claims 4 to 6 2 The preparation method of the Schottky diode is characterized by comprising the following steps of: comprising the following steps:
at the Cu-SnO 2 Single crystal thin filmPreparing a first metal electrode layer on the surface of one side of the layer far away from the substrate;
at the Cu-SnO 2 Preparing a second metal electrode layer on the part, which is far away from the substrate, of the monocrystalline film layer and is not covered by the first metal electrode layer; wherein:
the first metal electrode layer selectable range includes platinum, gold, or nickel; the second metal electrode layer can be selected from titanium, aluminum, copper, indium, silver or tin; the first metal electrode layer and Cu-SnO 2 Forming Schottky contact between the monocrystalline film layers; the second metal electrode layer and Cu-SnO 2 Ohmic contact is formed between the monocrystalline film layers.
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