CN114774891A - Sb2O3Thin film material and preparation of Sb based on sol-gel method2O3Method and application of thin film material - Google Patents
Sb2O3Thin film material and preparation of Sb based on sol-gel method2O3Method and application of thin film material Download PDFInfo
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- 239000010408 film Substances 0.000 title claims abstract description 66
- 239000000463 material Substances 0.000 title claims abstract description 30
- 239000010409 thin film Substances 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Inorganic materials O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 claims abstract description 39
- 238000000034 method Methods 0.000 claims abstract description 25
- 239000002243 precursor Substances 0.000 claims abstract description 24
- 238000003980 solgel method Methods 0.000 claims abstract description 13
- 239000000758 substrate Substances 0.000 claims abstract description 10
- 238000001704 evaporation Methods 0.000 claims abstract description 9
- 239000012298 atmosphere Substances 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 238000009987 spinning Methods 0.000 claims abstract description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 10
- 238000004528 spin coating Methods 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 7
- 229960000583 acetic acid Drugs 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 239000012362 glacial acetic acid Substances 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims 1
- 239000012776 electronic material Substances 0.000 abstract description 2
- 230000005669 field effect Effects 0.000 description 6
- 238000002441 X-ray diffraction Methods 0.000 description 5
- 239000004065 semiconductor Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 238000011031 large-scale manufacturing process Methods 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000003989 dielectric material Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 238000000691 measurement method Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 238000001308 synthesis method Methods 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 230000005685 electric field effect Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000002847 impedance measurement Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000002207 thermal evaporation Methods 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
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- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/1204—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material inorganic material, e.g. non-oxide and non-metallic such as sulfides, nitrides based compounds
- C23C18/1208—Oxides, e.g. ceramics
- C23C18/1216—Metal oxides
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Abstract
The present invention provides Sb2O3Thin film material and preparation of Sb based on sol-gel method2O3A method and application of a thin film material belong to the field of electronic materials and components. The preparation method is that Sb is mixed2O3The precursor solution is coated on the substrate in a spinning way to obtain a wet film; evaporating the prepared wet film at 80-120 deg.C for 10-15min, heat treating at 300-400 deg.C for 5-15min, taking out, and cooling to room temperature to obtain a layer of Sb which is not completely crystallized2O3A film; repeating the above steps for multiple times to obtain multiple layers of incompletely crystallized Sb2O3A film; crystallizing the film for 0.5-2h at the temperature of 450-600 ℃ in the air atmosphere to obtain completely crystallized Sb2O3Thin film, i.e. thin film with the advantages of high purity, good compactness, small average grain size, high electron mobility and the likeAnd (3) a film.
Description
Technical Field
The invention relates to the field of electronic materials and devices, in particular to Sb2O3Thin film material and preparation of Sb based on sol-gel method2O3A method of forming a thin film material.
Background
Two-dimensional (2D) semiconductors are one potential channel material for future Field Effect Transistors (FETs), with high mobility and gate controllability. The two-dimensional material has atomic-scale thickness and excellent photoelectric performance, and has wide application prospect in the field of next-generation photoelectronic devices. However, when the two-dimensional material is integrated with a conventional dielectric material, dangling bonds and disorder states on the surface of the dielectric material can seriously affect the properties of the two-dimensional material, so that the device performance is far inferior to the intrinsic performance of the two-dimensional material.
The structural characteristics of the surface of the inorganic molecular crystal without dangling bonds are utilized by predecessors, the surface of the wafer-level dielectric film prepared by the thermal evaporation deposition technology has no dangling bonds, has fewer carrier scattering sources and trap states, and a field effect transistor constructed by taking the wafer-level dielectric film as a dielectric layer and a two-dimensional semiconductor has higher mobility and working stability. Sb of coating by vaporization2O3Molecules can form an ultrathin compact film on the surface of a two-dimensional material, the film can be used as a top gate dielectric layer of a field effect transistor, the gate capacitance is greatly improved, excellent gate control performance is shown, the operating voltage and the power consumption of the transistor are also obviously reduced, and a foundation is laid for the application of the two-dimensional material to a low-power electronic device. But the thickness of the evaporation process is not easy to control, the evaporation process is not suitable for large-scale production, and the film layer is easy to fall off. In view of the above, the invention synthesizes Sb by using a sol-gel method2O3The film prepared by the method has the advantages of high purity, good compactness, small average grain size, high electron mobility and the like, and can be applied to low-power-consumption electronic devices.
Disclosure of Invention
The invention aims to: to is directed atThe above problems are solved by providing Sb2O3Thin film material and preparation of Sb based on sol-gel method2O3The invention discloses a method for preparing Sb on a ceramic substrate by a sol-gel synthesis method2O3The thin film material can be applied to low-power consumption electronic devices, and the process is simple and suitable for large-scale production.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
preparation of Sb based on sol-gel method2O3A method of forming a thin film material, the method comprising the steps of:
1) preparation of Sb2O3Precursor solution;
2) sb obtained in the step 1)2O3The precursor solution is coated on the substrate in a spinning way to obtain a wet film;
3) evaporating the wet film prepared by the spin coating in the step 2) to dryness at 80-120 ℃ for 10-15min, then carrying out heat treatment at 300-400 ℃ for 5-15min, taking out and cooling to room temperature to obtain a layer of Sb which is not completely crystallized2O3A film;
4) repeating the step 2) and the step 3) for multiple times to obtain multiple layers of incompletely crystallized Sb2O3A film;
5) subjecting the uncrystallized Sb obtained in step 4)2O3The film is crystallized for 0.5 to 2 hours in the air atmosphere at the temperature of 450-600 ℃ to obtain fully crystallized Sb2O3A film.
In the present invention, preferably, the Sb is2O3The precursor solution is prepared by mixing C6H9O6Sb or N3O9Dissolving Sb raw material in a mixed liquid with the volume ratio of glacial acetic acid to deionized water of 1:1 at the temperature of 100-120 ℃, mixing and stirring for 20-40min, and standing for 20-30h to obtain Sb2O3Precursor solution; the Sb2O3The concentration of the precursor solution is 0.3 mol/L.
In the invention, the spin coating in the step 2) is preferably performed for 30-40s at a rotation speed of 1500 r/min.
In the present invention, it is preferable thatStep 4) 15 layers of incompletely crystallized Sb were prepared2O3A film.
Sb prepared by the invention2O3The thin film may be applied to a top gate dielectric layer of a field transistor.
Due to the adoption of the technical scheme, the invention has the beneficial effects that:
in the invention, C is6H9O6Sb、N3O9Preparing a precursor from Sb, and preparing Sb on a ceramic substrate by a sol-gel synthesis method2O3The film material has the advantages of high purity, good compactness and small average grain size. Due to Sb2O3The molecular crystal film has no dangling bonds, has few charge scattering centers and charge traps, can realize higher electron mobility, and can be used as a top gate dielectric layer of a field transistor. Compared with the evaporation method, the method of the invention is convenient to control the thickness of the film, can be suitable for large-scale production, and has large adhesive force between the film layer and the substrate and is not easy to fall off.
Drawings
FIG. 1 is Sb2O3XRD pattern of the film;
FIG. 2 shows Sb2O3Scanning electron micrographs of the films;
FIG. 3 is Sb2O3Electron mobility versus temperature plot for thin films;
FIG. 4 shows Sb2O3A plot of film dielectric constant versus frequency;
FIG. 5 shows Sb in the present invention2O3The thin film is applied to a field effect transistor.
Detailed Description
The present invention will be described in further detail with reference to specific examples, but the embodiments of the present invention are not limited to the scope of the examples. These examples are intended to illustrate the invention only and are not intended to limit the scope of the invention. In addition, various modifications may occur to those skilled in the art upon reading the present disclosure, and such equivalent variations are within the scope of the present invention as defined in the appended claims.
First, preparation examples
Example 1
Preparation of Sb based on sol-gel method2O3A method of forming a thin film material, the method comprising the steps of:
1) preparation of Sb2O3Precursor solution of C6H9O6Dissolving Sb raw material in mixed liquid with the volume ratio of glacial acetic acid to deionized water of 1:1 at 100 ℃, mixing and stirring for 40min, and standing for 20h to obtain Sb2O3Precursor solution; the Sb is2O3The concentration of the precursor solution is 0.3 mol/L;
2) sb obtained in the step 1)2O3Spin-coating the precursor solution on the substrate at a rotation speed of 1500r/min for 30s to obtain a wet film;
3) evaporating the wet film prepared by spin coating in the step 2) at 90 ℃ for 15min, then carrying out heat treatment at 400 ℃ for 18min, taking out and cooling to room temperature to obtain a layer of incompletely crystallized Sb2O3A film;
4) repeating the step 2) and the step 3) for a plurality of times to obtain 15 layers of incompletely crystallized Sb2O3A film;
5) subjecting the uncrystallized Sb obtained in the step 4)2O3Crystallizing the film at 500 ℃ in air atmosphere for 60min to obtain completely crystallized Sb2O3A film.
Example 2
Preparation of Sb based on sol-gel method2O3A method of forming a thin film material, the method comprising the steps of:
1) preparation of Sb2O3Precursor solution of N3O9Dissolving Sb raw material in a mixed liquid with the volume ratio of glacial acetic acid to deionized water of 1:1 at 110 ℃, mixing and stirring for 30min, and standing for 25h to obtain Sb2O3Precursor solution; the Sb is2O3The concentration of the precursor solution is 0.3 mol/L;
2) sb obtained in the step 1)2O3The precursor solution rotates at 1500r/minSpin-coating for 35s on the substrate to obtain a wet film;
3) evaporating the wet film prepared by the spin coating in the step 2) to dryness at 95 ℃ for 12min, then carrying out heat treatment at 450 ℃ for 15min, taking out and cooling to room temperature to obtain a layer of Sb which is not completely crystallized2O3A film;
4) repeating the step 2) and the step 3) for a plurality of times to obtain 12 layers of incompletely crystallized Sb2O3A film;
5) subjecting the uncrystallized Sb obtained in step 4)2O3Crystallizing the film at 520 ℃ in air atmosphere for 55min to obtain completely crystallized Sb2O3A film.
Example 3
Preparation of Sb based on sol-gel method2O3A method of forming a thin film material, the method comprising the steps of:
1) preparation of Sb2O3Precursor solution of C6H9O6Dissolving Sb raw material in a mixed liquid with a volume ratio of glacial acetic acid to deionized water of 1:1 at 120 ℃, mixing and stirring for 20min, and standing for 30h to obtain Sb2O3Precursor solution; the Sb2O3The concentration of the precursor solution is 0.3 mol/L;
2) sb obtained in the step 1)2O3Spin-coating the precursor solution on the substrate at a rotation speed of 1500r/min for 40s to obtain a wet film;
3) evaporating the wet film prepared by the spin coating in the step 2) to dryness at 100 ℃ for 10min, then carrying out heat treatment at 500 ℃ for 12min, taking out and cooling to room temperature to obtain a layer of incompletely crystallized Sb2O3A film;
4) repeating the step 2) and the step 3) for multiple times to obtain 12 layers of incompletely crystallized Sb2O3A film;
5) subjecting the uncrystallized Sb obtained in the step 4)2O3Crystallizing the film at 550 ℃ in air atmosphere for 50min to obtain completely crystallized Sb2O3A film.
Secondly, the performance and the application of the product
1. X-ray diffraction test
Sb of examples 1 to 3 by X-ray diffraction2O3Carrying out phase analysis on the film to obtain cubic phase Sb2O3A film. In the obtained XRD pattern, all peak positions are in good agreement with corresponding PDF cards, and the XRD pattern of the film is shown in figure 1, which shows that the sol-gel method can successfully prepare Sb2O3A film.
2. Scanning electron microscope test
The secondary electron image of the film was taken with a scanning electron microscope to observe the surface topography. Sb from FIG. 22O3As can be seen from the SEM image of the thin film, Sb2O3The film is uniform and compact, can well cover the substrate, and has no holes, pinholes or cracks.
3. Four-point measurement technique
The four-point measurement technology, also called four-point test method, kelvin measurement method, is an impedance measurement method in electronic circuits, and is mainly used for accurately measuring the resistance value of a resistor. Referring to ohm's law R ═ U/I, the resistance of the resistor can be measured by measuring the voltage U across the resistor and the current I flowing through the resistor.
Fig. 3 is a graph showing the relationship between the measured electron mobility and temperature. The result shows that the electron mobility of the film is high in the temperature range of 10K-290K.
4. Dielectric constant test
Plating electrodes on the surface of the film, and testing the dielectric property of the film by using a dielectric spectrometer to obtain the dielectric constant of the material. And obtaining the variation relation of the dielectric constant with the frequency through the dielectric spectrogram. From FIG. 4, it can be seen that the dielectric constant of the film is high.
5. Application of product
Sb prepared by the invention2O3The thin film may be used for a top gate dielectric layer of a field effect transistor, see fig. 5. A field effect transistor is a semiconductor device that controls the current of an output loop by using the electric field effect of a control input loop, and conducts electricity only by the majority carriers in the semiconductor. Due to Sb2O3The thin film has good electron mobility, so that the gate capacitance is expected to be greatly improved,the method has excellent grid control performance, and lays a foundation for the application of the two-dimensional material to low-power-consumption electronic devices.
The above description is for the purpose of illustrating the preferred embodiments of the present invention, but the present invention is not limited thereto, and all changes and modifications that can be made within the spirit of the present invention should be included in the scope of the present invention.
Claims (6)
1. Preparation of Sb based on sol-gel method2O3A method of forming a film material, said method comprising the steps of:
1) preparation of Sb2O3Precursor solution;
2) sb obtained in the step 1)2O3The precursor solution is coated on the substrate in a spinning way to obtain a wet film;
3) evaporating the wet film prepared by the spin coating in the step 2) to dryness at 80-120 ℃ for 10-15min, then carrying out heat treatment at 300-400 ℃ for 5-15min, taking out and cooling to room temperature to obtain a layer of incompletely crystallized Sb2O3A film;
4) repeating the step 2) and the step 3) for a plurality of times to obtain a plurality of layers of incompletely crystallized Sb2O3A film;
5) subjecting the uncrystallized Sb obtained in step 4)2O3The film is crystallized for 0.5 to 2 hours at the temperature of 450-600 ℃ in the air atmosphere to obtain the completely crystallized Sb2O3A film.
2. The preparation of Sb according to claim 1 based on a sol-gel process2O3Method for producing a thin film material, characterized in that said Sb is2O3The precursor solution is prepared by mixing C6H9O6Sb or N3O9Dissolving Sb raw material in a mixed liquid with the volume ratio of glacial acetic acid to deionized water of 1:1 at the temperature of 100-120 ℃, mixing and stirring for 20-40min, and standing for 20-30h to obtain Sb2O3Precursor solution; the Sb is2O3The concentration of the precursor solution is 0.3 mol/L.
3. The method for preparing Sb according to claim 1 based on a sol-gel process2O3The method for preparing the thin film material is characterized in that the spin coating in the step 2) is performed for 30-40s at the rotating speed of 1500 r/min.
4. The preparation of Sb according to claim 1 based on a sol-gel process2O3The method for preparing the thin film material is characterized in that 15 layers of incompletely crystallized Sb are prepared in the step 4)2O3A film.
5. Sb prepared by the method according to any one of claims 1 to 42O3A film material.
6. Sb prepared by the method according to any one of claims 1 to 42O3The application of the film material is characterized in that: the application refers to Sb obtained by preparation2O3The thin film serves as a top gate dielectric layer for the field transistor.
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