CN114031080B - Silicon phosphide transistor synthesis and target production method thereof - Google Patents
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Abstract
The application relates to the technical field of silicon phosphide crystal dense-transistor synthesis and target production thereof, and discloses a silicon phosphide crystal dense-transistor synthesis and target production method thereof, which comprises the steps of accurately weighing silicon powder with purity of 99.999% and red phosphorus with purity of 99.999%, loading the silicon powder into a quartz tube, sealing the quartz tube, heating the quartz tube in a synthesis furnace to 800-1200 ℃, and preserving heat for 6-16 hours. Synthesizing to obtain single-phase silicon phosphide crystal with purity of 99.995%. Ball milling the product to powder of 500-800 meshes, loading the powder into a graphite mold, hot-pressing and sintering the powder in a vacuum hot-pressing furnace under the conditions of mechanical pressure of 10-25 MPa, temperature of 1000-1300 ℃ and argon atmosphere of 0.01MPa for 5-10 hours, cooling, taking out a silicon phosphide target blank, and carrying out mechanical processing and ultrasonic cleaning to obtain the silicon phosphide target material, wherein the relative density of the target material is more than 95%, the purity is more than 99.995%, and the single phase and grain size are less than 50 mu m.
Description
Technical Field
The application relates to the technical field of silicon phosphide transistor synthesis and target production thereof, in particular to a method for synthesizing a silicon phosphide transistor and producing a target thereof.
Background
Silicon phosphide is a IV-V group compound, silicon phosphide crystal is a novel two-dimensional material, the structure of the silicon phosphide crystal is similar to that of two-dimensional materials such as graphite, molybdenum disulfide and the like with a layered structure, covalent bonds are formed in the layers, and atoms are connected by strong forces; the layers are van der waals forces and are connected by weak intermolecular forces. In recent years, two-dimensional materials become research hotspots of material science, but at present, more two-dimensional material materials have obvious defects, so that the application of the two-dimensional material materials in the microelectronics field and other fields, such as zero band gap and easy agglomeration of graphene, are limited; the molybdenum disulfide has low carrier mobility at room temperature and is easy to deliquesce in a humid environment. In the past few years, scientists have urgent hoped to find new two-dimensional semiconductor materials, silicon phosphide is taken as a P-type direct band gap semiconductor material, and has been paid attention to and widely studied because of excellent optical performance and novel electron transport characteristics, and has potential great application prospects in the fields of photon technology, optical catalysis, steady flow molecular devices, lubricants and the like.
Disclosure of Invention
The application aims to provide a method for synthesizing a silicon phosphide close tube and producing a target thereof, and the produced silicon phosphide (SiP) target is used for preparing the silicon phosphide two-dimensional material or film by a physical vapor deposition method.
The application provides a method for synthesizing a silicon phosphide closed tube and producing a target material thereof, which adopts the following technical scheme:
the method for synthesizing the silicon phosphide transistor and producing the target thereof specifically comprises the following steps: silicon powder with the purity of 99.999 percent and red phosphorus with the purity of 99.999 percent are accurately weighed and then are filled into a quartz tube, the filling amount of each tube is 200-350 g, the molar ratio of silicon to red phosphorus is 1:1, and the raw materials are arranged at one end of the quartz tube. And vacuumizing the quartz tube to ensure that the air pressure in the quartz tube is 0.01 Torr, and sealing the quartz tube. Heating the quartz tube in a synthesis furnace to 800-1200 ℃ and preserving heat for 6-16 hours. Synthesizing to obtain single-phase silicon phosphide crystal with purity of 99.995%. Ball milling the product to powder of 500-800 meshes, loading the powder into a graphite mold, hot-pressing and sintering the powder in a vacuum hot-pressing furnace under the conditions of mechanical pressure of 10-25 MPa, temperature of 1000-1300 ℃ and argon atmosphere of 0.01MPa for 5-10 hours, cooling, taking out a silicon phosphide target blank, and carrying out mechanical processing and ultrasonic cleaning to obtain the silicon phosphide target material, wherein the relative density of the target material is more than 95%, the purity is more than 99.995%, and the single phase and grain size are less than 50 mu m.
By adopting the technical scheme, high-purity phosphorus and silicon are filled into a quartz tube and synthesized in a tubular double-temperature-zone synthesis furnace.
Preferably, the purity of the silicon powder is 99.999 percent, and the purity of red phosphorus is 99.999 percent.
Preferably, the diameter of the quartz tube is 35-50 mm, the length is 450mm, the wall thickness is 2.5-3.5 mm, and the softening point is 1400 ℃. Before use, the mixture is soaked in aqua regia for 12 hours, washed by ultrapure water and finally dried by infrared rays.
Preferably, the raw material is at one end of the quartz tube. And vacuumizing the quartz tube to ensure that the air pressure in the quartz tube is 0.01 Torr, and sealing the quartz tube.
Preferably, the quartz tube is vacuumized, so that the air pressure in the quartz tube is 0.01 Torr, and the quartz tube is sealed. Heating the quartz tube in a synthesis furnace to 800-1200 ℃ and preserving heat for 6-16 hours.
Preferably, the synthesis results in single phase silicon phosphide crystals having a purity of 99.995%.
Through the technical scheme, the synthesized product is ball milled to prepare powder, the particle size of the powder is reduced, and the sintering activity of the powder is improved.
Preferably, the ball mill is a planetary ball mill, and the ratio of big ball to middle ball to small ball is 1:1:1, wherein the diameter of the large sphere is 8mm, the diameter of the middle sphere is 5.2mm, and the diameter of the small sphere is 3.8mm; ball-to-material ratio 2.8:1, a step of; ball mill revolution is 200r/min; ball milling time is 2-2.5h.
Preferably, the particle size of the powder after ball milling is 500-800 meshes.
By adopting the technical scheme, the silicon phosphide powder is filled into a graphite mold, and is subjected to hot press sintering molding in a vacuum hot press furnace to prepare the silicon phosphide target blank.
Preferably, the hot press sintering atmosphere is an argon atmosphere.
Preferably, the hot press sintering condition is that the hot press sintering is carried out for 5 to 10 hours under the conditions of mechanical pressure of 10 to 25MPa, temperature of 1000 to 1300 ℃ and argon atmosphere of 0.01 MPa.
By adopting the technical scheme, the target blank cooled to room temperature in the vacuum hot-pressing furnace is taken out, and the silicon phosphide target material is obtained through machining, cleaning, drying and packaging.
Preferably, the cleaning is ultrasonic cleaning.
Preferably, the relative density of the target is more than 95%, the purity is more than 99.995%, and the single phase and grain size is less than 50 μm.
In summary, the application has the following beneficial effects:
1. the application adopts a dense pipe to synthesize the silicon phosphide crystal, the purity of the raw material is 99.999 percent, the single-pipe loading quantity is 200-350 g, and the silicon phosphide crystal with single-phase purity of 99.995 percent is prepared. Ensures the safety of the close tube synthesis, improves the synthesis efficiency and ensures that the purity of the silicon phosphide crystal is more than 99.995.
2. When the silicon phosphide powder is molded and sintered, the vacuum hot-pressing sintering method is adopted to prepare the silicon phosphide target material, and the silicon phosphide powder can be sintered and molded under the condition that the melting point is far lower, so that the production cost is greatly reduced.
3. According to the application, the silicon phosphide powder is placed in the ball mill for ball milling, so that the particle size of the silicon phosphide powder is further reduced, and the sintering activity of the silicon phosphide powder is improved, so that the compactness of the silicon phosphide powder after sintering and forming is improved, the internal porosity of the target after forming is greatly reduced, and the film forming performance of the silicon phosphide is improved.
4. According to the application, through researching and optimizing the silicon phosphide synthesis and vacuum hot-pressing sintering process, the purity of the prepared silicon phosphide target material reaches more than 99.99%, the density is more than 95%, and a high-performance film-making material source is provided for downstream factories and researchers.
Detailed Description
The present application will be described in further detail with reference to examples.
Examples
Embodiment 1, the method for synthesizing the silicon phosphide close tube and producing the target material thereof specifically comprises the following steps:
s1, accurately weighing silicon powder with the purity of 99.999% and red phosphorus with the purity of 99.999%, loading the silicon powder and the red phosphorus into a quartz tube, wherein the loading amount of each tube is 200g, the molar ratio of silicon to red phosphorus is 1:1, and the raw materials are arranged at one end of the quartz tube. The quartz tube has a diameter of 45mm, a length of 450mm, a wall thickness of 3.5mm and a softening point of 1400 ℃. Before use, the mixture is soaked in aqua regia for 12 hours, washed by ultrapure water and finally dried by infrared rays.
And S2, vacuumizing the quartz tube to ensure that the air pressure in the quartz tube is 0.01 Torr, and sealing the quartz tube by oxyhydrogen flame. Heating quartz tubes in a synthesis furnace to 800-1200 ℃ at the raw material end, and preserving heat for 6-16 hours. Synthesizing to obtain single-phase silicon phosphide crystal with purity of 99.995%.
S3, ball milling the product, wherein the ball mill is a planetary ball mill, and the ball milling ratio of big ball, middle ball and small ball is 1:1:1, wherein the diameter of the large sphere is 8mm, the diameter of the middle sphere is 5.2mm, and the diameter of the small sphere is 3.8mm; ball-to-material ratio 2.8:1, a step of; ball mill revolution is 200r/min; ball milling time is 2-2.5h. Grinding to 500-800 mesh powder.
S4, loading the silicon phosphide powder into a graphite mold, hot-pressing and sintering the graphite mold in a vacuum hot-pressing furnace under the conditions of mechanical pressure of 10-25 MPa, temperature of 1000-1300 ℃ and argon atmosphere of 0.01MPa for 5-10 hours, cooling, taking out a silicon phosphide target blank, and carrying out mechanical processing and ultrasonic cleaning to obtain the silicon phosphide target material, wherein the relative density of the target material is more than 95%, the purity is more than 99.995%, the single phase and the grain size is less than 50 mu m.
The present embodiment is only for explanation of the present application and is not to be construed as limiting the present application, and modifications to the present embodiment, which may not creatively contribute to the present application as required by those skilled in the art after reading the present specification, are all protected by patent laws within the scope of claims of the present application.
Claims (4)
1. The method for producing the silicon phosphide crystal target material is characterized by comprising the following steps of:
firstly, silicon powder with the purity of 99.999% and red phosphorus with the purity of 99.999% are accurately weighed and then are filled into a quartz tube, the filling amount of each tube is 200-350 g, the mole ratio of silicon to red phosphorus is 1:1, raw materials are arranged at one end of the quartz tube, the diameter of the quartz tube is 35-50 mm, the length of the quartz tube is 450mm, the wall thickness of the quartz tube is 2.5-3.5 mm, the softening point of the quartz tube is 1400 ℃, aqua regia is used for soaking for 12 hours before use, ultrapure water is used for cleaning, and finally infrared rays are used for drying;
step two, vacuumizing the quartz tube to ensure that the air pressure in the quartz tube is 0.01 Torr, and sealing the quartz tube;
heating the quartz tube in a synthesis furnace to 800-1200 ℃, and preserving heat for 6-16 hours to synthesize a single-phase silicon phosphide crystal with the purity of 99.995%;
ball milling the product to powder of 500-800 meshes, loading the powder into a graphite mold, carrying out hot-pressing sintering for 5-10 hours in a vacuum hot-pressing furnace under the conditions of mechanical pressure of 10-25 MPa, temperature of 1000-1300 ℃ and argon atmosphere of 0.01MPa, cooling, taking out a silicon phosphide target blank, and carrying out mechanical processing and ultrasonic cleaning to obtain the silicon phosphide target material, wherein the ball mill is a planetary ball mill, and the ball milling ratio of big ball to middle ball is 1:1:1, wherein the diameter of the large sphere is 8mm, the diameter of the middle sphere is 5.2mm, and the diameter of the small sphere is 3.8mm; ball-to-material ratio 2.8:1, a step of; ball mill revolution is 200r/min; ball milling time is 2-2.5h.
2. The method for producing the silicon phosphide crystalline target material according to claim 1, wherein the method comprises the steps of: the argon is high-purity argon.
3. The method for producing the silicon phosphide crystalline target material according to claim 1, wherein the method comprises the steps of: the relative density of the target material is more than 95%, the purity is more than 99.995%, and the single phase and the grain size are less than 50 mu m.
4. The method for producing the silicon phosphide crystalline target material according to claim 1, wherein the method comprises the steps of: and the silicon phosphide target material is obtained through machining, ultrasonic cleaning, drying and packaging.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005029410A (en) * | 2003-07-10 | 2005-02-03 | Shin Etsu Chem Co Ltd | Method for manufacturing finely powdered silicon or silicon compound |
| CN104496473A (en) * | 2014-12-30 | 2015-04-08 | 山东昊轩电子陶瓷材料有限公司 | Production method of high-density conductive niobium oxide target |
| CN111330603A (en) * | 2020-03-25 | 2020-06-26 | 深圳先进技术研究院 | Novel efficient photocatalytic material and application thereof |
| CN113371714A (en) * | 2021-05-10 | 2021-09-10 | 如皋市化合物半导体产业研究所 | Preparation method of silicon-phosphorus alloy |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005029410A (en) * | 2003-07-10 | 2005-02-03 | Shin Etsu Chem Co Ltd | Method for manufacturing finely powdered silicon or silicon compound |
| CN104496473A (en) * | 2014-12-30 | 2015-04-08 | 山东昊轩电子陶瓷材料有限公司 | Production method of high-density conductive niobium oxide target |
| CN111330603A (en) * | 2020-03-25 | 2020-06-26 | 深圳先进技术研究院 | Novel efficient photocatalytic material and application thereof |
| CN113371714A (en) * | 2021-05-10 | 2021-09-10 | 如皋市化合物半导体产业研究所 | Preparation method of silicon-phosphorus alloy |
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