CN110724934B - Powder evaporation device and using method and application thereof - Google Patents
Powder evaporation device and using method and application thereof Download PDFInfo
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- CN110724934B CN110724934B CN201810786067.0A CN201810786067A CN110724934B CN 110724934 B CN110724934 B CN 110724934B CN 201810786067 A CN201810786067 A CN 201810786067A CN 110724934 B CN110724934 B CN 110724934B
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/448—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials
- C23C16/4485—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials by evaporation without using carrier gas in contact with the source material
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Abstract
The invention relates to a powder evaporation device, which comprises a base, wherein a heating table is arranged on the base, a main cavity body is arranged on the heating table, a container is arranged in the main cavity body, powder materials are contained in the container, a rotary powder flattening device is arranged above the container, the powder flattening device comprises a rotating shaft which is lifted and rotated and a scraper arranged at the tail end of the rotating shaft, the scraper descends into the powder materials to be evaporated along with the rotating shaft and stirs the powder materials, and also descends onto the surface of the powder materials to be evaporated along with the rotating shaft and scrapes the surface of the powder materials; an inflation pipeline and an air pumping pipeline are arranged on the main cavity, and a waste gas filtering device and a vacuum pump are externally connected to the air pumping pipeline. The invention also relates to a method for using the device and application thereof. The invention has the characteristics of sealing, controllable vacuum degree, powder paving device and the like, and particles are uniformly dispersed during evaporation, so that the invention can be used for preparing large-area, high-crystallinity, uniform and compact semiconductor films.
Description
Technical Field
The invention relates to the technical field of semiconductor film preparation, in particular to a powder evaporation device and a using method and application thereof.
Background
Solar energy is used as a renewable energy source, has the characteristics of rich resources, no pollution, no geographical condition limitation on application and the like, and is the basis of future energy source structures. The solar photovoltaic technology is one of the important fields of solar energy utilization, so that how to prepare a cleaner and environment-friendly high-efficiency battery by using a new material and a new technology attracts attention, and particularly, a perovskite solar battery has rich sources and low price of a perovskite light absorption layer material, and is rapidly developed in recent years.
At present, the preparation method of the perovskite light absorption layer in the perovskite solar cell includes a one-step spin coating method, a two-step spin coating method, a continuous deposition method, a co-evaporation method, a gas phase auxiliary solution method and the like. In the existing technologies, such as a thermal spraying method, a thermal evaporation method, a CVD method, and the like, evaporation sources are mostly arranged in a non-vacuum environment, and are greatly influenced by water and oxygen in the environment, and reactant vapors mostly flow to the surface of a substrate along with a carrier gas in a unidirectional manner to be deposited, diffused, and reacted, so that the reaction rate is difficult to control, and reaction unevenness of each part of the substrate is easy to cause, and industrial preparation of large-area perovskite solar cells is difficult to realize. Especially, the quality of the finally prepared perovskite semiconductor film is determined by factors such as the evaporation uniformity and evaporation rate of precursor powder, and the non-uniform diffusion of the surface type evaporation source gas molecules can reduce the yield and stability of the product in the actual production link.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a powder evaporation device and a using method and application thereof, the device has the characteristics of being planar, closed, controllable in vacuum degree, provided with an evaporation source automatic powder paving device and the like, particles are uniformly dispersed during evaporation, a uniform and stable reaction environment is provided, and therefore, the device can be used for preparing large-area, high-crystallinity, uniform and compact semiconductor films and can be embedded into a large production line for continuous production.
The invention is realized in such a way, and provides a powder evaporation device, which comprises a base, wherein a heating table is arranged on the base, an openable and closed main cavity body is arranged on the heating table, a container is arranged in the main cavity body, powder materials to be evaporated are contained in the container, a powder flattening device is arranged above the container and is controlled by a flattening control unit, the powder flattening device comprises a rotating shaft and a scraper, the rotating shaft is lifted and rotated, the scraper is arranged at the tail end of the rotating shaft, and the scraper descends along with the rotating shaft into the powder materials to be evaporated and stirs the powder materials and also descends along with the rotating shaft onto the surfaces of the powder materials to be evaporated and scrapes the surfaces of the powder materials; be provided with gas charging line and exhaust line on the main cavity exhaust line is external to have exhaust gas filtering device and vacuum pump on the exhaust line, the vacuum pump passes through exhaust line and extracts the interior waste gas of main cavity, waste gas filters through exhaust gas filtering device.
The invention is realized in such a way, and also provides a use method of the powder evaporation device, which comprises the following steps:
the first step, opening the main chamber, injecting an appropriate quantity of powdered material to be evaporated into the container.
And secondly, closing the main cavity, vacuumizing the main cavity through a vacuum pump, and heating the heating table.
And thirdly, adjusting the height of the scraper through the paving control unit, controlling the scraper to rotate around the rotating shaft, stirring the powder material when the scraper is tightly attached to the bottom of the container, and re-spreading the powder material and leveling the surface of the powder material when the scraper is at a certain height away from the bottom of the container.
And fourthly, controlling the temperature and the vacuum degree of the main cavity to continuously heat and evaporate the powder material in the container.
The present invention has been achieved in this way, and provides a surface source device for producing a perovskite semiconductor thin film having a large area, in which the above-described powder evaporation apparatus is used for producing a perovskite semiconductor thin film, or the perovskite semiconductor thin film is produced by the use of the above-described powder evaporation apparatus.
Compared with the prior art, the powder evaporation device and the use method and application thereof can provide a closed evaporation source device with controllable air pressure and temperature, and the device and the method can realize the paving, evaporation and preservation of powder materials (such as perovskite precursor powder), keep the powder materials in a dry, loose and uniform state, and maintain the powder materials to evaporate in a constant vacuum environment, thereby obviously improving the uniformity of the powder materials during evaporation, providing a foundation for the preparation of semiconductor thin films (such as perovskite semiconductor thin films) and having important significance in the preparation of large-area semiconductor thin films. The device and the method can be used for the immersion reaction and the storage and pretreatment of evaporation source powder, and have important significance for the immersion preparation of large-area high-quality perovskite thin films.
Drawings
FIG. 1 is a schematic plan view of a powder evaporator according to a preferred embodiment of the present invention.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects to be solved by the present invention more clearly apparent, the present invention is further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Referring to fig. 1, a preferred embodiment of the powder evaporation device, its application method and application of the present invention includes a base 1. A heating table 2 is arranged on the base 1, the heating table 2 being designed to be uniformly hot and temperature-controlled. The shape and size of the heating table 2 can be changed according to actual requirements. The heating table 2 is controlled by the heating table control unit 15, and the temperature, the heating rate and the heating time of the heating table 2 can be set, so that the temperature of the heating table 2 is uniform and can be controlled by a program.
An openable and closable main chamber 3 is provided on the heating table 2, a container 4 is provided in the main chamber 3, and a powder material 5 to be evaporated is contained in the container 4. The main cavity 3 is provided with a cover capable of opening and closing, when the cover of the main cavity 3 is opened, the powder material 5 in the container 4 can be added or taken, and when the cover of the main cavity 3 is closed, the inside of the main cavity 3 is airtight.
Above the container 4 a powder spreading device is arranged. The powder levelling means is controlled by a levelling control unit 14. The powder paving device comprises a rotating shaft 6 which is lifted and rotated and a scraper 7 arranged at the tail end of the rotating shaft 6. The paving control unit 14 can set the rotating speed when the scraper 7 is driven to rotate by the rotating shaft 6, can set the height of the rotating shaft 6 and can set the distance from the bottom of the scraper 7 to the bottom of the container 4. The scraper 7 can be lowered with the rotating shaft 6 into the powder material 5 to be evaporated and agitate the powder material 5, and can be lowered with the rotating shaft 6 onto the surface of the powder material 5 to be evaporated and scrape the surface of the powder material 5 flat.
6 one end settings of pivot of powder paving device are on support frame 8, support frame 8 is fixed on base 1, the end of pivot 6 extends to in the main cavity body 3, scraper 7 sets up in the main cavity body 3 and is located container 4 directly over. The shape of the container 4 can be square, round and the like, the shape of the scraper 7 can be conical, flat, zigzag and the like, and the size of the scraper 7 needs to be matched with that of the container 4.
An inflation pipeline 9 and an air suction pipeline 10 are arranged on the main cavity 3. An exhaust gas filtering device 11 and a vacuum pump 12 are externally connected to the pumping pipeline 10. The vacuum pump 12 pumps the exhaust gas in the main chamber 3 through the suction line 10, and the exhaust gas is filtered by the exhaust gas filtering device 11. The inflation pipeline 9 is connected with inflation equipment, and the inflation pipeline is kept closed when inflation is not needed. The vacuum pump 12 and the inflation apparatus are controlled by a vacuum control unit 16 so that the air pressure in the main chamber 3 is maintained within a suitable range.
Thickness measuring devices 13 are respectively arranged on two sides of the scraper 7, the thickness of the powder material 5 in the container 4 is detected through the thickness measuring devices 13, and the thickness change of the powder material 5 is fed back in real time, so that the thickness of the powder material 5 can be better controlled. The powder material 5 has an average thickness of 2 to 10mm in the container 4. The rotating shaft 6, the scraper 7, the support frame 8 and the thickness measuring device 13 can be installed or disassembled according to actual requirements, and the main cavity 3 can still be kept airtight after the disassembly.
The container 4 is a flat-bottom container, and after the powder material is flattened by the powder flattening device, the thickness difference of the powder material 5 to be evaporated in the container 4 is not more than 0.4 mm. The container 4 is round, square and the like, and the material of the container 4 can be glass, quartz, ceramic, stainless steel, graphite and the like, so that the container has the characteristics of corrosion resistance and 100-400 ℃ high temperature resistance.
The scraper 7 can be in the shape of a cone, a flat shape, a sawtooth shape and the like, the scraper 7 is made of glass, quartz, metal, ceramic, polytetrafluoroethylene and the like, and the scraper has the characteristics of corrosion resistance and 100-400 ℃ high temperature resistance.
The invention also discloses a using method of the powder evaporating device, which comprises the following steps:
first, the main chamber 3 is opened and the appropriate quantity of powdered material 5 to be evaporated is injected into the container 4.
And a second step of closing the main cavity 3, vacuumizing the main cavity 3 through the vacuum pump 12, and heating the heating table 2 through the heating table control unit 15.
Thirdly, adjusting the height of the scraper 7 through the paving control unit 14, controlling the scraper 7 to rotate around the rotating shaft 6, and stirring the powder material 5 when the scraper 7 is tightly attached to the bottom of the container 4; when the scraper 7 is at a certain height from the bottom of the container 4, the re-spreading of the powder material 5 and the scraping of the surface thereof are achieved, so that the powder material 5 is loosely and uniformly spread in the container 4 and is thus more sufficiently and uniformly heated.
And fourthly, controlling the temperature and the vacuum degree of the main cavity to continuously heat and evaporate the powder material in the container.
The invention also discloses a surface source device for preparing the perovskite semiconductor thin film with large area, which uses the powder evaporation device or the using method of the powder evaporation device to prepare the perovskite semiconductor thin film.
The powder material 5 to be evaporated is perovskite precursor powder AX, wherein A is at least one of an amine group, an amidino group or an alkali group, and X is iodine (I), bromine (Br), chlorine (Cl), and thiocyanogen (NCS)-) Cyanide (CN)-) Cyanoxy (NCO)-) At least one anion. Common materials of perovskite precursor powder AX are iodomethylamine MAI, iodoformamidine FAI and the like. The method can be used for immersion preparation of the organic metal halide perovskite thin film, and can also be used for pretreatment of the evaporation source powder, namely perovskite precursor powder AX, and preservation of the evaporation source powder AX. When the method is used for pretreatment of the evaporation source powder AX, repeated stirring and re-spreading are carried out on the evaporation source powder AX under the conditions of vacuumizing and heating, so that volatile impurities in the evaporation source powder AX are removed, and drying and uniformity of the powder are realized. When the vacuum control unit is used for storing the evaporation source powder AX, the vacuum control unit is used for maintaining the dryness in the cavity and keeping the cavity at a certain vacuum degree.
The heating temperature of the heating table 2 is controlled within the temperature range of 20-400 ℃. The vacuum degree of the main cavity 3 is controlled at 10-5Pa~105Pressure range of Pa. The heating and evaporation duration of the powder material 5 is 5 minutes to 4 hours.
The area source device related by the invention is not limited to the field of perovskite solar cells, and the device can also be used for evaporating or sublimating oxide or halide by a gas phase method.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (7)
1. A powder evaporation device comprises a base, wherein a heating table is arranged on the base, and the powder evaporation device is characterized in that an openable and closed main cavity body is arranged on the heating table, a container is arranged in the main cavity body, powder materials to be evaporated are contained in the container, a rotary powder flattening device is arranged above the container and is controlled by a flattening control unit, the powder flattening device comprises a rotating shaft and a scraper, the rotating shaft is lifted and rotated, the scraper is arranged at the tail end of the rotating shaft, the scraper descends along with the rotating shaft into the powder materials to be evaporated and stirs the powder materials, and also descends along with the rotating shaft onto the surfaces of the powder materials to be evaporated and scrapes the surfaces of the powder materials; an inflation pipeline and an air extraction pipeline are arranged on the main cavity, a waste gas filtering device and a vacuum pump are externally connected to the air extraction pipeline, the vacuum pump extracts waste gas in the main cavity through the air extraction pipeline, and the waste gas is filtered through the waste gas filtering device; the pivot one end setting of powder paving device is on the support frame, the support frame is fixed on the base, in the end of pivot extends to the main cavity, the scraper setting is internal and be located the container in the main cavity directly over the scraper both sides are equipped with thickness measurement device respectively, the container is flat container, treat the powder material process of evaporation the powder paving device is strickleed the back, and the thickness difference of powder material in the container is no longer than 0.4mm, and the average thickness of powder material in the container is at 2~10 mm.
2. A method of using the powder vaporizing apparatus of claim 1, comprising the steps of:
the first step, opening the main cavity and injecting a proper amount of powder material to be evaporated into the container;
closing the main cavity, vacuumizing the main cavity through a vacuum pump, and heating the heating table;
thirdly, adjusting the height of the scraper through the paving control unit, controlling the scraper to rotate around a rotating shaft, stirring the powder material when the scraper is tightly attached to the bottom of the container, and re-spreading the powder material and leveling the surface of the powder material when the scraper is at a certain height away from the bottom of the container;
and fourthly, controlling the temperature and the vacuum degree of the main cavity to continuously heat and evaporate the powder material in the container.
3. A surface source apparatus for producing a perovskite semiconductor thin film having a large area, characterized in that the powder evaporation apparatus according to claim 1 is used for producing a perovskite semiconductor thin film, or the perovskite semiconductor thin film is produced by the method of using the powder evaporation apparatus according to claim 2.
4. The surface source apparatus for preparing large-area perovskite semiconductor thin film as claimed in claim 3, wherein the powder material to be evaporated is perovskite precursor powder AX, wherein A is at least one of amine group, amidino group or alkali group, and X is at least one anion of iodine, bromine, chlorine, thiocyanato, cyanide group, and oxocyanide group.
5. The surface source device for preparing a large-area perovskite semiconductor thin film as claimed in claim 3, wherein the heating temperature of the heating table is controlled within a temperature range of 20 ℃ to 400 ℃.
6. The surface source apparatus for producing a large area perovskite semiconductor thin film as claimed in claim 3, wherein the degree of vacuum of the main chamber is controlled to 10-5Pa~105Pressure range of Pa.
7. The surface source device for producing a large-area perovskite semiconductor thin film as claimed in claim 3, wherein the duration of the heating evaporation of the powder material is 5 minutes to 4 hours.
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| CN113828775A (en) * | 2020-06-24 | 2021-12-24 | 天津大学 | Powder laying device for laser additive manufacturing of multilayer materials |
| CN112467032B (en) * | 2020-10-27 | 2022-12-06 | 南昌大学 | Method for preparing high-quality organic-inorganic perovskite film by using waste raw materials |
| CN113073008A (en) * | 2021-04-13 | 2021-07-06 | 漳州职业技术学院 | Extraction device for essential oil in passion fruit peel and using method |
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