CN113526476A - High-pressure high-temperature method for preparing high-temperature semiconductor material Boron Phosphide (BP) - Google Patents
High-pressure high-temperature method for preparing high-temperature semiconductor material Boron Phosphide (BP) Download PDFInfo
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Abstract
The invention discloses a preparation method of a high-temperature semiconductor material boron phosphide material. Mainly relates to a boron phosphide material with high-temperature semiconductor material, belonging to the field of semiconductors. Elemental phosphorus, crystal boron and nickel metal are mixed according to a certain proportion, and are ground, mixed, wrapped, packaged and pre-pressed to synthesize the boron phosphide material under the conditions of 5.0Pa and 1000-3200 ℃. The invention prepares the Boron Phosphide (BP) material with high-temperature semiconductor material by utilizing a high-temperature high-pressure synthesis method for the first time, and the Boron Phosphide (BP) material has the characteristics of large grain size, high crystallinity, high density and stable structure. The material has the advantages of simple preparation process, high synthesis efficiency and great application potential, and can be used as materials of high-temperature semiconductor devices, light-emitting diodes, laser diodes and the like.
Description
Technical Field
The invention relates to a high-temperature semiconductor material Boron Phosphide (BP) material, in particular to a high-temperature semiconductor material Boron Phosphide (BP) material and a preparation method thereof, belonging to the field of semiconductor materials.
Background
BP has high melting point (2840K), high hardness (32 GPa), high thermal conductivity and high chemical stability. The high-temperature semiconductor material is an important high-temperature semiconductor material, is a third generation high-temperature semiconductor material following semiconductor materials such as gallium arsenide and indium phosphide, has wider forbidden bandwidth, higher breakdown electric field, higher thermal conductivity, higher electron saturation velocity and higher radiation resistance, and can realize high voltage, high temperature, high frequency and high radiation resistance. But because its decomposition temperature is lower than its melting point temperature, it is necessary to be in the vicinity of the melting point, which is more likely to cause decomposition, in order to obtain a large single crystal; under high pressure, the phosphorus-boron system only has one boron phosphide phase, so that the high-temperature high-pressure synthesis method becomes a good synthesis method. The conventional method for preparing the high-temperature semiconductor material Boron Phosphide (BP) material comprises the following steps:
chemical vapor deposition (T.L. CHU et al. Journal of Applied Physics 1970), which is a technique of applying gaseous substances to produce chemical and transport reactions, etc., on solids and produce solid deposits. Although the method synthesizes large single crystals, the method is easy to decompose, reduces the performance of samples, and has long synthesis time and high cost.
Self-propagating high temperature synthesis (Vladimir a et al. journal of super materials.2013), which is a technique to form new materials using a strong exothermic reaction between powder elements. The method is difficult to obtain a pure high-temperature semiconductor material Boron Phosphide (BP) material, and the synthesis reaction process and the material performance are difficult to control due to the over-high reaction speed.
Metathesis (Luyang Chen et al Chemistry Letters 2003), a technique for the preparation of compounds that react with each other. The displacement reaction can produce pure boron phosphide powder without extraneous contamination. But large single crystal material is not grown.
The conventional methods are difficult to prepare large boron phosphide single-crystal materials, and the preparation of high-temperature semiconductor material Boron Phosphide (BP) material single crystals is always a great challenge. Boron Phosphide (BP) materials, a high-temperature semiconductor material, have a wide range of applications due to their excellent physicochemical properties. In order to obtain a high-temperature semiconductor material Boron Phosphide (BP) material, a domestic hinge type cubic press is utilized to directly synthesize the material under the conditions of high temperature and high pressure, and a single crystal material with excellent performance and application value is prepared. The invention has the advantages of simple preparation process, controllable cost, contribution to industrial production, high purity, and great application potential, and can be used for high-temperature semiconductor devices, light-emitting diodes and laser diodes.
Disclosure of Invention
The invention aims to overcome the defects of the traditional normal pressure preparation method and provide a synthesis method of boron phosphide and a preparation method thereof. So as to solve the problems of low purity of the sample prepared by the traditional preparation method, difficult growth of crystal grains and the like. The invention adopts phosphorus, boron and nickel as initial raw materials, the raw materials are mixed according to the molar ratio of 5:2:3, and boron phosphide single crystal is directly synthesized under the conditions of 5.0 GPa, 1400 ℃ and the heat preservation time of 120 minutes. The invention adopts phosphorus and boron as initial raw materials, and the boron and the phosphorus are mixed according to the molar ratio of 1:1, and the boron phosphide single crystal is directly synthesized under the conditions of 5.0 GPa, 1000-3200 ℃ and the heat preservation time of 10-120 minutes. The high-temperature semiconductor material Boron Phosphide (BP) material synthesized by the invention has the remarkable characteristics of high purity, large grain size and the like. The high-temperature semiconductor material provided by the invention has a forbidden band width of 2.5 eV.
The invention provides a method for synthesizing a high-temperature semiconductor material Boron Phosphide (BP) material, which comprises the following steps:
the first step is as follows: selecting crystal boron, metallic nickel and elemental phosphorus as initial raw materials, and mixing the raw materials according to a certain proportion;
the second step is that: uniformly grinding the mixed phosphorus-boron-nickel mixed powder;
the third step: prepressing the phosphorus-boron-nickel mixed powder into a cylinder;
the fourth step: putting the pre-pressed cylinder into a high-pressure synthesis assembly, and putting the assembled high-pressure synthesis assembly into a synthesis cavity for high-temperature high-pressure synthesis;
the fifth step: and (4) after the synthesis is finished, cooling and releasing pressure, and removing nickel by acid washing to obtain the high-temperature semiconductor material Boron Phosphide (BP) material.
In the first step of the method, the particle sizes of phosphorus, boron and nickel are all 5-200 mu m. And directly sintering the mixed powder together at high temperature and high pressure to form the phosphorus-boron-nickel bulk material. In the first step of the method, phosphorus, boron and nickel are mixed according to the mass ratio of 5:2: 3.
In the fifth step of the method, aqua regia or concentrated hydrochloric acid and concentrated sulfuric acid are used for acid washing.
The prepressed packaging cylinder in the fourth step of the method is placed in a sodium chloride salt pipe in a pyrophyllite synthesis block, the upper end and the lower end of the salt pipe are sealed by salt sheets to form salt columns, then the salt columns are placed in a graphite pipe, graphite sheets are sequentially assembled at the upper end and the lower end of the graphite pipe to form graphite columns, the graphite columns are placed in a dolomite pipe, and a dolomite sheet with the graphite columns in the middle, a molybdenum sheet and a conductive steel ring are sequentially assembled at the two ends of the dolomite pipe. After the assembly in the fifth step of the method is completed, the synthetic block is placed in a synthetic cavity of a large press, the pressure is preferably 5.0 GPa under the high-temperature and high-pressure conditions, the temperature is about 1400 ℃, and the heat preservation and pressure maintaining are carried out for 120 minutes. The equipment suitable for the high-temperature high-pressure synthesis process in the fifth step of the method can be a two-side top press, a four-side top press, a six-side top press and equipment capable of generating high-temperature high-pressure conditions.
In the sixth step of the method, the acid for washing away the high-melting-point metal is aqua regia.
Secondly, the second method for synthesizing the high-temperature semiconductor material Boron Phosphide (BP) material provided by the invention comprises the following steps:
the first step is as follows: selecting crystal boron and phosphorus as initial raw materials and mixing the raw materials according to a certain proportion;
the second step is that: uniformly grinding the mixed phosphorus and boron powder;
the third step: prepressing the phosphorus-boron-nickel mixed powder into a cylinder;
the fourth step: putting the pre-pressed cylinder into a high-pressure synthesis assembly, and putting the assembled high-pressure synthesis assembly into a synthesis cavity for high-temperature high-pressure synthesis;
the fifth step: and after the synthesis is finished, cooling and relieving the pressure to obtain the high-temperature semiconductor material Boron Phosphide (BP) material.
In the first step of the method, the particle sizes of phosphorus and boron are both 5-200 mu m. And directly sintering the mixed powder together at high temperature and high pressure to form the phosphorus-boron-nickel bulk material. In the first step of the method, phosphorus and boron are mixed according to the mass ratio of 1:1, mixing.
The prepressed packaging cylinder in the fourth step of the method is placed in a sodium chloride salt pipe in a pyrophyllite synthesis block, the upper end and the lower end of the salt pipe are sealed by salt sheets to form salt columns, then the salt columns are placed in a graphite pipe, graphite sheets are sequentially assembled at the upper end and the lower end of the graphite pipe to form graphite columns, the graphite columns are placed in a dolomite pipe, and a dolomite sheet with the graphite columns in the middle, a molybdenum sheet and a conductive steel ring are sequentially assembled at the two ends of the dolomite pipe. After the assembly in the fifth step, the synthetic block is placed in a synthetic cavity of a large press, the pressure is preferably 5.0 GPa under the high-temperature and high-pressure conditions, the temperature is about 1000 ℃ and 3200 ℃, and the heat preservation and pressure maintaining are carried out for 10-120 minutes. The equipment suitable for the high-temperature high-pressure synthesis process in the fifth step of the method can be a two-side top press, a four-side top press, a six-side top press and equipment capable of generating high-temperature high-pressure conditions.
Advantageous effects
(1) The invention provides a method for directly synthesizing a high-temperature semiconductor material Boron Phosphide (BP) material under the conditions of high temperature and high pressure by taking crystal boron, metallic nickel and simple substance phosphorus as initial raw materials. Has the characteristics of low cost, environmental protection, simple synthesis process, good product performance, high yield and the like.
(2) The high-temperature semiconductor material Boron Phosphide (BP) material obtained by the method provided by the invention has the remarkable characteristics of high purity, large grain size and the like.
Drawings
FIG. 1 is a photograph of a high temperature semiconductor material Boron Phosphide (BP) material prepared by the present invention.
FIG. 2 shows the X-ray diffraction pattern of Boron Phosphide (BP) material as a high-temperature semiconductor material prepared by the present invention (example II).
FIG. 3 is a scanning electron microscope image of a Boron Phosphide (BP) material as a high-temperature semiconductor material prepared by the present invention (example II).
Fig. 4 shows a laser raman spectrum of a Boron Phosphide (BP) material as a high-temperature semiconductor material prepared by the present invention (example two).
FIG. 5 is a single crystal x-ray diffraction pattern of a high temperature semiconductor material Boron Phosphide (BP) material prepared in accordance with the present invention (example two).
Detailed Description
The first embodiment is as follows: taking phosphorus, boron and nickel powder with a molar ratio of 5:2:3 as initial raw materials, grinding the selected raw materials, then putting the raw materials into a high-melting-point wrapping material for packaging, prepressing under the pressure of 600 MPa to obtain a cylindrical wrapping body, then putting the cylindrical wrapping body into a sodium chloride salt tube in a pyrophyllite synthesis block, sealing the upper end and the lower end of the salt tube with salt sheets to form salt columns, then putting the salt columns into a graphite tube, sequentially assembling graphite sheets at the upper end and the lower end of the graphite tube to form graphite columns, then putting the graphite columns into a dolomite tube, and sub-assembling dolomite sheets, molybdenum sheets and a conductive steel ring with the graphite columns in the middle at the two ends of the dolomite tube. And (3) placing the assembled synthesized block into a synthesis cavity of a large press, keeping the temperature and pressure at 1400 ℃ and about 5.0 GPa, keeping the temperature and pressure for 60 minutes, cooling and relieving the pressure, taking out the material, soaking the material in aqua regia, and removing the metallic nickel to obtain the high-temperature semiconductor material Boron Phosphide (BP) material.
Example two: taking phosphorus, boron and nickel powder with a molar ratio of 5:2:3 as initial raw materials, grinding the selected raw materials, then putting the raw materials into a high-melting-point wrapping material for packaging, prepressing under the pressure of 600 MPa to obtain a cylindrical wrapping body, then putting the cylindrical wrapping body into a sodium chloride salt tube in a pyrophyllite synthesis block, sealing the upper end and the lower end of the salt tube with salt sheets to form salt columns, then putting the salt columns into a graphite tube, sequentially assembling graphite sheets at the upper end and the lower end of the graphite tube to form graphite columns, then putting the graphite columns into a dolomite tube, and sub-assembling dolomite sheets, molybdenum sheets and a conductive steel ring with the graphite columns in the middle at the two ends of the dolomite tube. And (3) placing the assembled synthesized block into a synthesis cavity of a large press, keeping the temperature and pressure at 1600 ℃ and about 5.0 GPa, keeping the temperature and pressure for 60 minutes, cooling and relieving the pressure, taking out the material, soaking the material in aqua regia, and removing the metallic nickel to obtain the high-temperature semiconductor material Boron Phosphide (BP) material.
Example three: taking phosphorus, boron and nickel powder with a molar ratio of 5:2:3 as initial raw materials, grinding the selected raw materials, then putting the raw materials into a high-melting-point wrapping material for packaging, prepressing under the pressure of 600 MPa to obtain a cylindrical wrapping body, then putting the cylindrical wrapping body into a sodium chloride salt tube in a pyrophyllite synthesis block, sealing the upper end and the lower end of the salt tube with salt sheets to form salt columns, then putting the salt columns into a graphite tube, sequentially assembling graphite sheets at the upper end and the lower end of the graphite tube to form graphite columns, then putting the graphite columns into a dolomite tube, and sub-assembling dolomite sheets, molybdenum sheets and a conductive steel ring with the graphite columns in the middle at the two ends of the dolomite tube. And (3) placing the assembled synthetic block into a synthetic cavity of a large press, keeping the temperature and pressure at 1000 ℃ and about 5.0 GPa, keeping the temperature and pressure for 60 minutes, cooling and relieving the pressure, taking out the material, soaking the material in aqua regia, and removing metallic nickel to obtain the high-temperature semiconductor material Boron Phosphide (BP) material.
Example four: taking phosphorus, boron and nickel powder with a molar ratio of 5:2:3 as initial raw materials, grinding the selected raw materials, then putting the raw materials into a high-melting-point wrapping material for packaging, prepressing under the pressure of 600 MPa to obtain a cylindrical wrapping body, then putting the cylindrical wrapping body into a sodium chloride salt tube in a pyrophyllite synthesis block, sealing the upper end and the lower end of the salt tube with salt sheets to form salt columns, then putting the salt columns into a graphite tube, sequentially assembling graphite sheets at the upper end and the lower end of the graphite tube to form graphite columns, then putting the graphite columns into a dolomite tube, and sub-assembling dolomite sheets, molybdenum sheets and a conductive steel ring with the graphite columns in the middle at the two ends of the dolomite tube. And (3) placing the assembled synthesized block into a synthesis cavity of a large press, keeping the temperature and the pressure at 1200 ℃ and about 5.0 GPa, keeping the temperature and the pressure for 60 minutes, cooling and relieving the pressure, taking out the material, soaking the material in aqua regia, and removing the metallic nickel to obtain the high-temperature semiconductor material Boron Phosphide (BP) material.
Example five: taking phosphorus-boron-nickel powder with a molar ratio of 5:2:3 as an initial raw material, grinding the selected raw material, then putting the raw material into a high-melting-point wrapping material for packaging, prepressing under the pressure of 600 MPa to obtain a cylindrical wrapping body, then putting the cylindrical wrapping body into a sodium chloride salt tube in a pyrophyllite synthesis block, sealing the upper end and the lower end of the salt tube with salt sheets to form salt columns, then putting the salt columns into a graphite tube, sequentially assembling graphite sheets at the upper end and the lower end of the graphite tube to form ink columns, then putting the graphite columns into a dolomite tube, and sub-assembling dolomite sheets, molybdenum sheets and a conductive steel ring with the graphite columns in the middle at the two ends of the dolomite tube. And (3) placing the assembled synthetic block into a synthetic cavity of a large press, keeping the temperature and pressure at 1400 ℃ and about 5.0 GPa, keeping the temperature and pressure for 120 minutes, cooling and relieving the pressure, taking out the material, soaking the material in aqua regia, and removing metallic nickel to obtain the high-temperature semiconductor material Boron Phosphide (BP) material.
Example six: taking phosphorus and boron powder with a molar ratio of 1:1 as initial raw materials, grinding the selected raw materials, prepressing under the pressure of 600 MPa to obtain a cylindrical inclusion, then putting the cylindrical inclusion into a sodium chloride salt tube in a pyrophyllite synthesis block, sealing the upper end and the lower end of the salt tube with salt sheets to form salt columns, then putting the salt columns into a graphite tube, sequentially assembling graphite sheets at the upper end and the lower end of the graphite tube to form graphite columns, then putting the graphite columns into a dolomite tube, and assembling dolomite sheets with the graphite columns in the middle, molybdenum sheets and conductive steel rings at the two ends of the dolomite tube in sequence. And (3) placing the assembled synthesized block into a synthesis cavity of a large press, keeping the temperature and the pressure at 1000 ℃ and about 5.0 GPa, keeping the temperature and the pressure for 60 minutes, cooling and relieving the pressure, taking out the material, and then obtaining the high-temperature semiconductor material Boron Phosphide (BP) material.
Example seven: taking phosphorus and boron powder with a molar ratio of 1:1 as initial raw materials, grinding the selected raw materials, prepressing under the pressure of 600 MPa to obtain a cylindrical inclusion, then putting the cylindrical inclusion into a sodium chloride salt tube in a pyrophyllite synthesis block, sealing the upper end and the lower end of the salt tube with salt sheets to form salt columns, then putting the salt columns into a graphite tube, sequentially assembling graphite sheets at the upper end and the lower end of the graphite tube to form graphite columns, then putting the graphite columns into a dolomite tube, and assembling dolomite sheets with the graphite columns in the middle, molybdenum sheets and conductive steel rings at the two ends of the dolomite tube in sequence. And (3) placing the assembled synthesized block into a synthesis cavity of a large press, keeping the temperature and the pressure at 1200 ℃ and about 5.0 GPa, keeping the temperature and the pressure for 60 minutes, cooling and relieving the pressure, taking out the material, and then obtaining the high-temperature semiconductor material Boron Phosphide (BP) material.
Example eight: taking phosphorus and boron powder with a molar ratio of 1:1 as initial raw materials, grinding the selected raw materials, prepressing under the pressure of 600 MPa to obtain a cylindrical inclusion, then putting the cylindrical inclusion into a sodium chloride salt tube in a pyrophyllite synthesis block, sealing the upper end and the lower end of the salt tube with salt sheets to form salt columns, then putting the salt columns into a graphite tube, sequentially assembling graphite sheets at the upper end and the lower end of the graphite tube to form graphite columns, then putting the graphite columns into a dolomite tube, and assembling dolomite sheets with the graphite columns in the middle, molybdenum sheets and conductive steel rings at the two ends of the dolomite tube in sequence. And (3) placing the assembled synthesized block into a synthesis cavity of a large press, keeping the temperature and pressure at 1400 ℃ and about 5.0 GPa, keeping the temperature and pressure for 60 minutes, cooling and relieving the pressure, taking out the material, and then obtaining the high-temperature semiconductor material Boron Phosphide (BP) material.
Example nine: taking phosphorus and boron powder with a molar ratio of 1:1 as initial raw materials, grinding the selected raw materials, prepressing under the pressure of 600 MPa to obtain a cylindrical inclusion, then putting the cylindrical inclusion into a sodium chloride salt tube in a pyrophyllite synthesis block, sealing the upper end and the lower end of the salt tube with salt sheets to form salt columns, then putting the salt columns into a graphite tube, sequentially assembling graphite sheets at the upper end and the lower end of the graphite tube to form graphite columns, then putting the graphite columns into a dolomite tube, and assembling dolomite sheets with the graphite columns in the middle, molybdenum sheets and conductive steel rings at the two ends of the dolomite tube in sequence. And (3) placing the assembled synthesized block into a synthesis cavity of a large press, keeping the temperature and the pressure at 1600 ℃ and about 5.0 GPa, keeping the temperature and the pressure for 60 minutes, cooling and relieving the pressure, taking out the material, and then obtaining the high-temperature semiconductor material Boron Phosphide (BP) material.
Example ten: taking phosphorus and boron powder with a molar ratio of 1:1 as initial raw materials, grinding the selected raw materials, prepressing under the pressure of 600 MPa to obtain a cylindrical inclusion, then putting the cylindrical inclusion into a sodium chloride salt tube in a pyrophyllite synthesis block, sealing the upper end and the lower end of the salt tube with salt sheets to form salt columns, then putting the salt columns into a graphite tube, sequentially assembling graphite sheets at the upper end and the lower end of the graphite tube to form graphite columns, then putting the graphite columns into a dolomite tube, and assembling dolomite sheets with the graphite columns in the middle, molybdenum sheets and conductive steel rings at the two ends of the dolomite tube in sequence. And (3) placing the assembled synthesized block into a synthesis cavity of a large press, keeping the temperature and pressure at 1800 ℃ and 5.0 GPa for 60 minutes, cooling and relieving the pressure, taking out the material, and thus obtaining the high-temperature semiconductor material Boron Phosphide (BP) material.
Example eleven: taking phosphorus and boron powder with a molar ratio of 1:1 as initial raw materials, grinding the selected raw materials, prepressing under the pressure of 600 MPa to obtain a cylindrical inclusion, then putting the cylindrical inclusion into a sodium chloride salt tube in a pyrophyllite synthesis block, sealing the upper end and the lower end of a hexagonal boron nitride tube by using hexagonal boron nitride sheets to form a hexagonal boron nitride column, then putting the salt column into a graphite tube, sequentially assembling graphite sheets at the upper end and the lower end of the graphite tube to form a graphite column, then putting the graphite column into a zirconium dioxide tube, and sub-assembling zirconium dioxide sheets, molybdenum sheets and conductive steel rings with the graphite column in the middle at the two ends of the zirconium dioxide tube. And (3) placing the assembled synthesized block into a synthesis cavity of a large press, keeping the temperature and the pressure at 2000 ℃ and about 5.0 GPa for 30 minutes, cooling and relieving the pressure, taking out the material, and then obtaining the high-temperature semiconductor material Boron Phosphide (BP) material.
Example twelve: taking phosphorus and boron powder with a molar ratio of 1:1 as initial raw materials, grinding the selected raw materials, prepressing under the pressure of 600 MPa to obtain a cylindrical inclusion, then putting the cylindrical inclusion into a sodium chloride salt tube in a pyrophyllite synthesis block, sealing the upper end and the lower end of a hexagonal boron nitride tube by using hexagonal boron nitride sheets to form a hexagonal boron nitride column, then putting the salt column into a graphite tube, sequentially assembling graphite sheets at the upper end and the lower end of the graphite tube to form a graphite column, then putting the graphite column into a zirconium dioxide tube, and sub-assembling zirconium dioxide sheets, molybdenum sheets and conductive steel rings with the graphite column in the middle at the two ends of the zirconium dioxide tube. And (3) placing the assembled synthesized block into a synthesis cavity of a large press, keeping the temperature and pressure at 3200 ℃ and 5.0 GPa or so for 10 minutes, cooling and relieving the pressure, taking out the material, and then obtaining the high-temperature semiconductor material Boron Phosphide (BP) material.
The upper and lower interval values of the process parameters (such as mass fraction, synthesis temperature, pressure, time and the like) listed in the invention can realize the invention, and an example is not listed again. The above description is only for the preferred embodiment of the present invention, and the technical solutions of the present invention are not limited to the above description, and those skilled in the art can make various changes, substitutions and alterations without departing from the spirit and scope of the present invention, and thus the equivalent technical solutions also belong to the scope of the present invention.
Claims (11)
1. A high-pressure high-temperature synthesis method of high-temperature semiconductor material Boron Phosphide (BP) is characterized by comprising the following steps: the boron phosphide semiconductor material is synthesized by a high-pressure high-temperature method, and the prepared material has high purity, high crystallinity and stable performance at high temperature.
2. The first method for preparing Boron Phosphide (BP) as a high-temperature semiconductor material according to claim 1, wherein: the method mainly comprises the following steps:
(1) selecting crystal boron, metallic nickel and elemental phosphorus as initial raw materials;
(2) fully and uniformly mixing the raw materials mixed in the step (1) in a mortar;
(3) putting the powder in the step (2) into a cylinder by prepressing;
(4) putting the cylinder pre-pressed in the step (3) into a high-pressure synthesis assembly;
(5) placing the assembled high-pressure synthesis assembly in a synthesis cavity for high-temperature high-pressure synthesis under the synthesis conditions of 5 GPa and 1400 ℃ and the heat preservation time of 30-120 minutes;
(6) and (3) after the synthesis is finished, reducing the temperature and relieving the pressure, taking out the synthesized block, and then carrying out acid washing to remove nickel elements to obtain the high-temperature semiconductor material Boron Phosphide (BP) material as claimed in claim 1.
3. The second method for preparing Boron Phosphide (BP) as a high-temperature semiconductor material according to claim 1, wherein: the method mainly comprises the following steps:
(7) selecting crystal boron and simple substance phosphorus as initial raw materials;
(8) fully and uniformly mixing the raw materials mixed in the step (7) in a mortar;
(9) putting the powder in the step (8) into a cylinder by prepressing;
(10) putting the cylinder pre-pressed in the step (9) into a high-pressure synthesis assembly;
(11) placing the assembled high-pressure synthesis assembly in a synthesis cavity for high-temperature high-pressure synthesis, wherein the synthesis condition is 5 GPa, 1000 ℃ and 3200 ℃, and the heat preservation time is 30-120 minutes;
(12) and (3) after the synthesis is finished, reducing the temperature and relieving the pressure, and taking out the synthesized block to obtain the high-temperature semiconductor material Boron Phosphide (BP) material in claim 1.
4. The high temperature semiconductor BP material of claim 1, wherein: the prepared high-temperature semiconductor material Boron Phosphide (BP) material is a cubic structure BP, and the form of the material is powder or granular crystal and the like.
5. The method of preparing a high temperature semiconductor material Boron Phosphide (BP) material according to claim 2, wherein: the acid in the step (6) is aqua regia, concentrated hydrochloric acid or concentrated sulfuric acid.
6. A high temperature semiconductor material Boron Phosphide (BP) material according to claim 1, wherein: the preparation of the high-temperature semiconductor material Boron Phosphide (BP) material adopts a high-temperature high-pressure synthesis method.
7. The method of preparing a high temperature semiconductor material Boron Phosphide (BP) material according to claim 2: mixing phosphorus, boron and nickel in the step (1) according to a molar ratio of 5:2: 3; and (7) mixing phosphorus and boron according to a molar ratio of 1: 1.
8. The high temperature semiconductor BP material of claim 1, wherein: the prepared high-temperature semiconductor material Boron Phosphide (BP) material is a cubic structure BP, and the form of the material is powder or granular single crystal and the like.
9. A high temperature semiconductor material Boron Phosphide (BP) material according to claim 1, wherein: the preparation of the high-temperature semiconductor material Boron Phosphide (BP) material adopts a high-temperature high-pressure synthesis method.
10. The method of preparing a high temperature semiconductor material Boron Phosphide (BP) material according to claim 2, wherein: the grinding time in the steps (2) and (8) is 2 h.
11. The method of preparing a high temperature semiconductor material Boron Phosphide (BP) material according to claim 2, wherein: the pressing machines in the steps (5) and (11) are a cubic press, a two-side press, a four-side press and equipment capable of generating high-temperature and high-pressure conditions.
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| JPH029713A (en) * | 1988-06-27 | 1990-01-12 | Daido Steel Co Ltd | Production of boron phosphide |
| CN1460296A (en) * | 2001-05-28 | 2003-12-03 | 昭和电工株式会社 | Semiconductor device, semiconductor layer and production method thereof |
| CN102530974A (en) * | 2012-02-28 | 2012-07-04 | 吉林大学 | High-temperature high-pressure preparation method of molybdenum boride |
| CN108975918A (en) * | 2018-08-13 | 2018-12-11 | 四川大学 | A kind of high tenacity high-temperature structural material MoSi2-Mo5Si3The preparation of composite ceramics |
| CN109734451A (en) * | 2019-01-31 | 2019-05-10 | 四川大学 | A kind of high entropy ceramics of transition metal diboride and preparation method thereof |
| CN110284195A (en) * | 2019-07-18 | 2019-09-27 | 南方科技大学 | Boron phosphide single crystal and preparation method and application thereof |
| CN110499529A (en) * | 2019-08-28 | 2019-11-26 | 四川大学 | A kind of high temperature and pressure preparation of routine superconductor material tungsten phosphide (WP) |
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| JPH029713A (en) * | 1988-06-27 | 1990-01-12 | Daido Steel Co Ltd | Production of boron phosphide |
| CN1460296A (en) * | 2001-05-28 | 2003-12-03 | 昭和电工株式会社 | Semiconductor device, semiconductor layer and production method thereof |
| CN102530974A (en) * | 2012-02-28 | 2012-07-04 | 吉林大学 | High-temperature high-pressure preparation method of molybdenum boride |
| CN108975918A (en) * | 2018-08-13 | 2018-12-11 | 四川大学 | A kind of high tenacity high-temperature structural material MoSi2-Mo5Si3The preparation of composite ceramics |
| CN109734451A (en) * | 2019-01-31 | 2019-05-10 | 四川大学 | A kind of high entropy ceramics of transition metal diboride and preparation method thereof |
| CN110284195A (en) * | 2019-07-18 | 2019-09-27 | 南方科技大学 | Boron phosphide single crystal and preparation method and application thereof |
| CN110499529A (en) * | 2019-08-28 | 2019-11-26 | 四川大学 | A kind of high temperature and pressure preparation of routine superconductor material tungsten phosphide (WP) |
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