CN114892276A - Spinel sulfide thin film material and preparation method thereof - Google Patents
Spinel sulfide thin film material and preparation method thereof Download PDFInfo
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- CN114892276A CN114892276A CN202210349053.9A CN202210349053A CN114892276A CN 114892276 A CN114892276 A CN 114892276A CN 202210349053 A CN202210349053 A CN 202210349053A CN 114892276 A CN114892276 A CN 114892276A
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/46—Sulfur-, selenium- or tellurium-containing compounds
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- C—CHEMISTRY; METALLURGY
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- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
- C30B23/02—Epitaxial-layer growth
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Abstract
The invention discloses a preparation method of a spinel sulfide single crystal epitaxial film, which comprises the following steps: (1) mixing CoS powder and Ni 3 S 2 Grinding, tabletting and vacuum tube sealing high-temperature calcining the powder and the S powder which are used as target raw materials; (2) cleaning the YSZ substrate with acetone, alcohol and deionized water for 5 min; (3) putting the fired target material and the cleaned YSZ substrate into a pulse laser deposition system (4) together to grow the single crystal NiCO by regulating the growth temperature and the laser energy density 2 S 4 A film. The process used in the invention prepares NiCO for the first time 2 S 4 The single crystal film provides good conditions for exploring the physical properties of the material such as electric transport, magnetism and the like.
Description
Technical Field
The invention belongs to the field of pulse laser deposition technology and spinel film preparation, and particularly relates to NiCo 2 S 4 Spinel sulfide thin film materials and a preparation method thereof.
Background
Spinel-type oxide thin film NiCo 2 O 4 Has been known by peopleExtensive study, in contrast to NiCo 2 O 4 ，NiCo 2 S 4 With smaller forbidden band width, S 2- (184pm) ion radius ratio O 2- (140pm) is much larger, electrons are more localized, the electronegativity of sulfur is lower than that of oxygen in metal oxide, when the sulfur atom replaces the oxygen atom in the crystal, a flexible crystal structure is formed, the structure is not damaged due to the extension of crystal faces, but the electron transfer rate is greatly improved, and previous researches show that NiCo 2 S 4 Having 100 times of NiCo 2 O 4 The electrical conductivity of (1). The single crystal epitaxial film has unique advantages compared with the bulk: better physical properties, easy application to devices, etc. The growth quality of the spinel type sulfide thin film prepared by the method is poor, so that a method for simply and efficiently preparing the high-quality spinel type sulfide epitaxial thin film is found, and the method has a remarkable meaning for the research, development and application of the whole spinel type sulfide material.
Disclosure of Invention
In view of the fact that no method for preparing high-quality spinel sulfide film is found at present, the technical problem to be solved by the invention is to provide NiCo 2 S 4 Spinel sulfide film material and preparation method thereof, and NiCo prepared by using spinel sulfide film material 2 S 4 The epitaxial thin film material is a single crystal thin film, has excellent electrical properties and good stability, and is used for researching NiCo 2 S 4 Provide samples for a range of good performance.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of spinel type sulfide thin film material comprises the following steps:
(1) with CoS powder, Ni 3 S 2 Grinding, tabletting and high-temperature calcining the powder and the S powder which are taken as materials to obtain NiCo 2 S 4 A target material;
(2) ultrasonically cleaning the YSZ substrate by using acetone, alcohol and deionized water for 5min respectively;
(3) putting the fired target material and the cleaned YSZ substrate into a pulsed laser deposition system;
(4) growing single crystal epitaxial NiCo by regulating growth temperature and pulse energy density 2 S 4 A film.
Further, in the step (1), 1.19g of CoS powder, Ni 3 S 2 0.53g of powder and 0.35g of S powder, grinding for 30min by using an agate mortar, tabletting by using a target press after grinding, wherein the pressure is 20Mpa, the tabletting time is 10min, transferring the target material after tabletting and a ceramic gasket into a quartz tube together, sealing the tube by using a vacuum tube sealing machine, transferring the target material after vacuum sealing into a tube furnace for high-temperature calcination, and obtaining the sintered NiCo after calcination 2 S 4 A target material.
Further, the degree of vacuum in the vacuum tube sealing machine was 4.5X 10 -4 Pa。
Further, the conditions for transferring the vacuum-sealed target material into a tube furnace for high-temperature calcination are as follows: heating from room temperature to 670 ℃, heating rate of 5 ℃/min, and keeping the temperature for 12 h.
Further, NiCo sintered in the step (1) 2 S 4 The target material needs to be polished by fine sand paper, and is adhered to a target holder by conductive carbon after being polished.
Further, in the step (2), the YSZ substrate is respectively subjected to ultrasonic cleaning for 5min by acetone, alcohol and deionized water, and after the cleaning is finished, the YSZ substrate needs to be dried by a nitrogen gun and is adhered to a substrate table by conductive silver paste.
Further, the target holder with the target and the substrate table with the YSZ are placed into a sputtering chamber of the pulsed laser deposition system together in the step (3), and the distance between the target and the YSZ substrate is controlled to be 55 mm.
Further, the degree of vacuum of the pulse laser deposition system in the step (4) is 4.5 × 10 -4 Pa, temperature of 500 deg.C, laser beam frequency of 9Hz, and laser energy density of 1.6J/cm 2 The number of deposition pulses was 15000pulses-30000 pulses.
Further, pre-sputtering is required for 10min before coating in the step (4) to ensure that no other impurities are attached to the surface of the target.
Compared with the prior art, the invention has the following beneficial effects:
(1) the preparation condition process explored by the invention prepares NiCo for the first time 2 S 4 The single crystal epitaxial film provides an excellent film sample for exploring the physical performance of the material.
(2) The material prepared by the invention has excellent optical performance, and provides a good foundation for the application of the material in the field of photoelectric devices.
(3) The epitaxial preparation method provided by the invention is novel, and provides a new idea for the field of spinel sulfide film preparation.
Drawings
FIG. 1 is a flow chart of a process for preparing a spinel-based sulfide thin film material of the present invention;
FIG. 2 is a NiCo product of examples 1, 2 and 3 of the present invention 2 S 4 Calibrated Raman plots of the thin film material;
FIG. 3 is a NiCo product of example 1 of the invention 2 S 4 A plot of the RSM measured from the calibrated YSZ (002) orientation of the film material;
FIG. 4 is a NiCo product of example 1 of the invention 2 S 4 A Phi-Scan plot of the calibrated YSZ (202) measurement of the thin film material;
FIG. 5 is a NiCo product of example 1 of the invention 2 S 4 Light transmittance map of thin film material.
Detailed Description
In an embodiment of the present invention, as shown in fig. 1, the method for preparing the spinel sulfide thin film material includes the following steps:
(1) weighing CoS powder 1.19g, Ni 3 S 2 0.53g of powder and 0.35g of S powder, grinding for 30min in a vacuum glove box by using an agate mortar, tabletting by using a tabletting machine after grinding, wherein the tabletting pressure is 20Mpa, the time is 10min, putting the pressed target material and a ceramic gasket into a quartz tube after tabletting, and sealing the tube in vacuum by using a vacuum tube sealing machine, wherein the vacuum degree of the sealed tube is controlled to be 4.5 multiplied by 10 -4 pa, after the sealing of the tube, putting the quartz tube into a tube furnace forSintering the target material, wherein the sintering temperature is 670 ℃, the heat preservation time is 12h, the heating rate is 5 ℃/min, and NiCo can be obtained after sintering 2 S 4 The sintered target material is firstly polished to be smooth by using fine sand paper, and then the target material is adhered to a target material support by using conductive carbon adhesive;
(2) ultrasonically cleaning a YSZ substrate with acetone, alcohol and deionized water respectively for 5min, blow-drying the YSZ substrate with a nitrogen gun after cleaning, adhering the YSZ substrate to a substrate table with conductive silver paste after blow-drying, and quickly drying the silver paste with a heating table;
(3) putting the target material and the substrate into a pulse laser deposition system together, and controlling the distance between the target material and the substrate to be 55 mm;
(4) coating in a pulsed laser deposition system with vacuum degree controlled at 4.5 × 10 -4 Pa, temperature of 500 deg.C, laser frequency of 9Hz, and energy density of 1.6J/cm 2 And the laser pulse number is 6000-30000 pulses, and the epitaxial single crystal thin film material of the spinel sulfide can be obtained.
The following describes the implementation of the present invention in detail by means of 3 examples.
Example 1
As shown in fig. 1, a method for preparing a spinel sulfide thin film material includes the following steps:
(1) weighing CoS powder 1.19g, Ni 3 S 2 0.53g of powder and 0.35g of S powder, grinding for 30min in a vacuum glove box by using an agate mortar, tabletting by using a tabletting machine after grinding, wherein the tabletting pressure is 20Mpa, the time is 10min, putting the pressed target material and a ceramic gasket into a quartz tube after tabletting, and sealing the tube in vacuum by using a vacuum tube sealing machine, wherein the vacuum degree of the sealed tube is controlled to be 4.5 multiplied by 10 -4 pa, after the tube sealing is finished, putting the quartz tube into a tube furnace for target sintering, wherein the sintering temperature is 670 ℃, the heat preservation time is 12h, the heating rate is 5 ℃/min, and NiCo can be obtained after sintering is finished 2 S 4 The sintered target material is firstly polished to be smooth by using fine sand paper, and then the target material is adhered to a target material support by using conductive carbon adhesive;
(2) ultrasonically cleaning a YSZ substrate with acetone, alcohol and deionized water respectively for 5min, blow-drying the YSZ substrate with a nitrogen gun after cleaning, adhering the YSZ substrate to a substrate table with conductive silver paste after blow-drying, and quickly drying the silver paste with a heating table;
(3) putting the target material and the substrate into a pulse laser deposition system together, and controlling the distance between the target material and the substrate to be 55 mm;
(4) coating in a pulsed laser deposition system with vacuum degree controlled at 4.5 × 10 -4 pa at 500 deg.C, laser frequency of 9Hz, and energy density of 1.6J/cm 2 And the number of laser pulses is 18000pulses (the thickness is 60nm), and the epitaxial monocrystal thin film material of the spinel sulfide can be obtained.
Example 2
As shown in fig. 1, a method for preparing a spinel sulfide thin film material includes the following steps:
(1) weighing 1.19g of CoS powder, 0.53g of Ni3S2 powder and 0.35g of S powder, grinding for 30min in a vacuum glove box by using an agate mortar, tabletting by using a tabletting machine after grinding, wherein the tabletting pressure is 20Mpa, the tabletting time is 10min, putting the pressed target material and the ceramic gasket into a quartz tube after tabletting, and carrying out vacuum tube sealing by using a vacuum tube sealing machine, wherein the vacuum degree of the tube sealing is controlled to be 4.5 multiplied by 10 -4 pa, after the tube sealing is finished, putting the quartz tube into a tube furnace for target sintering, wherein the sintering temperature is 670 ℃, the heat preservation time is 12h, the heating rate is 5 ℃/min, and NiCo can be obtained after sintering is finished 2 S 4 The sintered target material is firstly polished to be smooth by using fine sand paper, and then the target material is adhered to a target material support by using conductive carbon adhesive;
(2) ultrasonically cleaning a YSZ substrate with acetone, alcohol and deionized water respectively for 5min, blow-drying the YSZ substrate with a nitrogen gun after cleaning, adhering the YSZ substrate to a substrate table with conductive silver paste after blow-drying, and quickly drying the silver paste with a heating table;
(3) putting the target material and the substrate into a pulse laser deposition system together, and controlling the distance between the target material and the substrate to be 55 mm;
(4) in a pulsed laserCoating film in the deposition system, controlling the vacuum degree at 4.5 × 10 -4 Pa, temperature of 500 deg.C, laser frequency of 9Hz, and energy density of 1.6J/cm 2 The number of laser pulses was 30000pulses (thickness: 100nm), and the epitaxial single crystal thin film material of spinel sulfide was obtained.
Example 3
As shown in fig. 1, a method for preparing a spinel sulfide thin film material includes the following steps:
(1) weighing CoS powder 1.19g, Ni 3 S 2 0.53g of powder and 0.35g of S powder, grinding for 30min in a vacuum glove box by using an agate mortar, tabletting by using a tabletting machine after grinding, wherein the tabletting pressure is 20Mpa, the time is 10min, putting the pressed target material and a ceramic gasket into a quartz tube after tabletting, and sealing the tube in vacuum by using a vacuum tube sealing machine, wherein the vacuum degree of the sealed tube is controlled to be 4.5 multiplied by 10 -4 pa, after the tube sealing is finished, putting the quartz tube into a tube furnace for target sintering, wherein the sintering temperature is 670 ℃, the heat preservation time is 12h, the heating rate is 5 ℃/min, and NiCo can be obtained after sintering is finished 2 S 4 The sintered target material is firstly polished to be smooth by using fine sand paper, and then the target material is adhered to a target material support by using conductive carbon adhesive;
(2) ultrasonically cleaning a YSZ substrate with acetone, alcohol and deionized water respectively for 5min, blow-drying the YSZ substrate with a nitrogen gun after cleaning, adhering the YSZ substrate to a substrate table with conductive silver paste after blow-drying, and quickly drying the silver paste with a heating table;
(3) putting the target material and the substrate into a pulse laser deposition system together, and controlling the distance between the target material and the substrate to be 55 mm;
(4) coating in a pulsed laser deposition system with vacuum degree controlled at 4.5 × 10 -4 Pa, temperature of 500 deg.C, laser frequency of 9Hz, and energy density of 1.6J/cm 2 The number of laser pulses was 6000pulses (thickness: 20nm), and the epitaxial single crystal thin film material of spinel sulfide was obtained.
FIG. 2 is a NiCo product of examples 1, 2 and 3 of the present invention 2 S 4 Raman spectra of thin film materials, FIG. 3 is a graph of the preparation of example 1 of the present inventionPreparation of NiCo 2 S 4 Calibration of the film material YSZ (002) orientation was measured as a RSM plot, from which it can be seen that the film has good epitaxial relationship with the substrate. FIG. 4 is a NiCo product of inventive example 1 2 S 4 The Phi-Scan graph measured by the alignment YSZ (202) of the film material shows that the film has 4 peaks in the range of 0-360 degrees, which shows that the film has four-fold symmetry and shows good epitaxial relationship between the film and the substrate. FIG. 5 is a NiCo product of inventive example 1 2 S 4 Optical transmission of thin film materials. As can be seen from the data in FIG. 5, the transmittance of the film in the range of 400-800nm is about 40%, while the transmittance of the film in the ultraviolet region and the infrared region is very low, indicating that NiCO has a low transmittance 2 S 4 Has certain window characteristics and potential utilization value in the aspect of photoelectric devices.
The foregoing detailed description of the preferred embodiments of the invention has been presented. It should be understood that numerous modifications and variations could be devised by those skilled in the art in light of the present teachings without departing from the inventive concepts. Therefore, the technical solutions that can be obtained by a person skilled in the art through logical analysis, reasoning or limited experiments based on the prior art according to the concepts of the present invention should be within the scope of protection determined by the claims.
Claims (10)
1. A preparation method of spinel sulfide thin film material is characterized by comprising the following steps:
(1) with CoS powder, Ni 3 S 2 Grinding, tabletting and high-temperature calcining the powder and the S powder which are taken as materials to obtain NiCo 2 S 4 A target material;
(2) ultrasonically cleaning the YSZ substrate by using acetone, alcohol and deionized water for 5min respectively;
(3) putting the fired target material and the cleaned YSZ substrate into a pulsed laser deposition system;
(4) growing single crystal epitaxial NiCo by regulating growth temperature and pulse energy density 2 S 4 A film.
2. The method for preparing spinel-type sulfide thin film material according to claim 1, wherein in the step (1), 1.19g of CoS powder and Ni are weighed 3 S 2 0.53g of powder and 0.35g of S powder, grinding for 30min by using an agate mortar, tabletting by using a target press after grinding, wherein the pressure is 20Mpa, the tabletting time is 10min, transferring the target material after tabletting and a ceramic gasket into a quartz tube together, sealing the tube by using a vacuum tube sealing machine, transferring the target material after vacuum sealing into a tube furnace for high-temperature calcination, and obtaining the sintered NiCo after calcination 2 S 4 A target material.
3. The method of claim 2, wherein the degree of vacuum in the vacuum tube sealing machine is 4.5 x 10 -4 Pa。
4. The method for preparing the spinel-type sulfide thin film material according to claim 2, wherein the conditions for transferring the vacuum-sealed target material into the tube furnace for high-temperature calcination are as follows: heating from room temperature to 670 ℃, heating rate is 5 ℃/min, and keeping the temperature for 12 h.
5. The method for preparing spinel sulfide thin film material of claim 1, wherein the NiCo sintered in step (1) 2 S 4 The target material needs to be polished by fine sand paper, and is adhered to a target holder by conductive carbon after being polished.
6. The method for preparing the spinel sulfide thin film material according to claim 1, wherein the YSZ substrate in step (2) is ultrasonically cleaned with acetone, alcohol and deionized water for 5min, and then dried by using a nitrogen gun and adhered to a substrate table with conductive silver paste.
7. The method of claim 1, wherein the step (3) comprises placing the target holder with the target and the substrate table with the YSZ into a sputtering chamber of a pulsed laser deposition system, and the distance between the target and the YSZ substrate is controlled to be 55 mm.
8. The method for preparing spinel-type sulfide thin film material according to claim 1, wherein the degree of vacuum of the pulsed laser deposition system in the step (4) is 4.5 x 10 -4 Pa, temperature of 500 deg.C, laser beam frequency of 9Hz, and laser energy density of 1.6J/cm 2 The number of deposition pulses was 15000pulses-30000 pulses.
9. The method for preparing the spinel-type sulfide thin film material according to claim 1, wherein pre-sputtering is required for 10min before the film coating in the step (4) to ensure that no other impurities are attached to the surface of the target.
10. A spinel sulphide thin film material produced by a process according to any one of claims 1 to 9.
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Cited By (1)
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| CN114645321A (en) * | 2022-03-24 | 2022-06-21 | 电子科技大学 | Co9S8Method for preparing single crystal transition metal sulfide film |
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