CN112802957B - Preparation device and preparation method of porous silicon and magnesium silicide composite material - Google Patents

Preparation device and preparation method of porous silicon and magnesium silicide composite material Download PDF

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CN112802957B
CN112802957B CN202110133071.9A CN202110133071A CN112802957B CN 112802957 B CN112802957 B CN 112802957B CN 202110133071 A CN202110133071 A CN 202110133071A CN 112802957 B CN112802957 B CN 112802957B
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quartz
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tube
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porous silicon
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CN112802957A (en
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汪舰
王童
王兰杰
胡保付
徐坚
刘丙国
杜保立
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Henan University of Technology
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    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
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    • H10N10/00—Thermoelectric devices comprising a junction of dissimilar materials, i.e. devices exhibiting Seebeck or Peltier effects
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    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
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    • H10N10/00—Thermoelectric devices comprising a junction of dissimilar materials, i.e. devices exhibiting Seebeck or Peltier effects
    • H10N10/80—Constructional details
    • H10N10/85—Thermoelectric active materials
    • H10N10/851—Thermoelectric active materials comprising inorganic compositions
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N10/00—Thermoelectric devices comprising a junction of dissimilar materials, i.e. devices exhibiting Seebeck or Peltier effects
    • H10N10/80—Constructional details
    • H10N10/85—Thermoelectric active materials
    • H10N10/851—Thermoelectric active materials comprising inorganic compositions
    • H10N10/855—Thermoelectric active materials comprising inorganic compositions comprising compounds containing boron, carbon, oxygen or nitrogen
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    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract

The invention relates to a preparation device and a preparation method of a porous silicon and magnesium silicide composite material, which comprises the following steps: the preparation device comprises a quartz test tube, a quartz bracket, a quartz plug, a heat insulation sleeve, a lifter, a vertical tube furnace and a high-temperature resistance wire; the tube wall of the quartz test tube is provided with a convex point towards the inner direction of the tube; the quartz bracket comprises a cylindrical quartz substrate and two quartz wires; the quartz plug is used for vacuum sealing the quartz test tube; the quartz bracket is positioned between the convex point of the wall of the quartz test tube and the quartz plug and can move back and forth; the heat insulation sleeve comprises a cylindrical sleeve and a high-temperature-resistant resistance wire grid; the heat insulation sleeve is connected with the lifter through a high-temperature resistance wire. The method prepares the magnesium silicide by repeatedly depositing magnesium and magnesium-silicon on the porous silicon and reacting the magnesium and the magnesium-silicon by a two-step method, has simple operation and low cost, and can prepare the high-quality porous silicon and magnesium silicide composite material.

Description

Preparation device and preparation method of porous silicon and magnesium silicide composite material
Technical Field
The invention relates to the field of thermoelectric material manufacturing, in particular to a preparation device and a preparation method of a porous silicon and magnesium silicide composite material.
Background
With the large consumption of fossil fuels, the emerging energy and environmental crisis has begun to affect people's lives more and more. People need a green, recyclable, low-carbon sustainable development approach. Thermoelectric materials are functional materials that enable direct interconversion between thermal and electrical energy. The industrial waste heat, the automobile exhaust and other waste heat can be converted into electric energy for recycling, and the energy crisis can be effectively relieved. The thermoelectric properties of thermoelectric materials are generally defined by a dimensionless figure of merit zT = (S) 2 σ) T/κ, where S, σ, κ, and T are Seebeck coefficient, electrical conductivity, thermal conductivity, and absolute temperature, respectively.
Both porous silicon and magnesium silicide are very potential thermoelectric materials and have been extensively studied. The porous silicon has a special porous structure, greatly reduces the thermal conductivity of bulk silicon, but has little influence on the electrical conductivity of the bulk silicon. The magnesium silicide-based thermoelectric material is a medium-temperature thermoelectric material which is rich in raw material, green and environment-friendly and has a good development prospect, has good electrical conductivity, and has high thermal conductivity. The porous silicon is used as a framework to prepare the porous silicon and magnesium silicide composite material, so that the thermal conductivity of the magnesium silicide based thermoelectric material is effectively reduced, and the thermoelectric performance of the material is influenced. However, the magnesium material required for the preparation of magnesium silicide is a very active metal, chemically reacts with many substances at high temperatures, and is very susceptible to oxidation. Therefore, the material has high requirements on the use conditions. Currently, magnetron sputtering, electron beam assisted deposition, and the like are used to prepare magnesium silicide on a single crystal silicon wafer. The instruments used in these methods are expensive and not suitable for widespread use. In addition, since magnesium is very easily oxidized, magnesium oxide impurities are more or less introduced during the reaction of depositing magnesium or silicon magnesium using the above method.
Therefore, the device and the method for preparing the magnesium silicide with high quality and no magnesium oxide impurity are developed, have important significance for preparing the porous silicon and magnesium silicide composite material, and provide a new method for preparing the magnesium silicide.
Disclosure of Invention
In view of the above problems, an object of the present invention is to provide an apparatus and a method for preparing a porous silicon and magnesium silicide composite material. The preparation device and the preparation method are easy to establish temperature gradient, so that magnesium is easier to attach and react on the surface of the porous silicon hole; the preparation device and the preparation method enable magnesium to react with porous silicon in a completely closed environment, so that no magnesium oxide impurity is generated in a prepared magnesium silicide sample, and no other impurities are introduced; the preparation device of the porous silicon and magnesium silicide composite material is simple to operate and low in cost, and can prepare the high-quality porous silicon and magnesium silicide composite material.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, a device for preparing a porous silicon and magnesium silicide composite material is characterized in that: the device comprises a quartz test tube, a quartz bracket, a quartz plug, a heat insulation sleeve, a lifter, a vertical tube furnace and a high-temperature resistance wire; a convex point towards the inner direction of the tube is arranged on the tube wall of the quartz test tube at a position 1.5-3 cm away from the bottom of the quartz test tube; the quartz support comprises a cylindrical quartz substrate and two quartz wires, and two ends of each quartz wire are bonded on one end face of the quartz substrate; the quartz plug is 8-15cm away from the bottom of the quartz test tube and is used for sealing the quartz test tube in vacuum; the quartz bracket is positioned between the convex point of the quartz test tube wall and the quartz plug and can move back and forth; the heat insulation sleeve comprises a cylindrical sleeve and a high-temperature resistance wire grid, the cylindrical sleeve is 1.5-3 cm high, the inner diameter of the cylindrical sleeve is larger than the outer diameter of a quartz test tube, the outer diameter of the cylindrical sleeve is smaller than the inner diameter of a furnace tube of the vertical tube furnace, and the high-temperature resistance wire grid is fixed at one end of the cylindrical sleeve and used for preventing the quartz test tube from passing through; the heat insulation sleeve is connected with the elevator through a high-temperature resistance wire; the lifter is positioned right above the furnace mouth of the vertical tube furnace; the vertical tube furnace is used for establishing a temperature gradient for the quartz test tube.
The cylindrical sleeve of the heat insulation sleeve is composed of refractory heat insulation materials such as alumina microspheres and ceramic fibers.
In a second aspect, the present invention provides a method for preparing a porous silicon and magnesium silicide composite material, comprising the steps of:
1) Removing an oxide layer on the surface of the magnesium grains by cutting, and then putting the magnesium grains at the bottom of a quartz test tube;
2) Preparing porous silicon by corroding one surface of a silicon wafer by a known electrochemical anodic corrosion method;
3) Fixing the prepared porous silicon wafer on a quartz bracket, enabling the non-corroded surface to be in contact with a cylindrical quartz substrate in the quartz bracket, and then placing the porous silicon surface facing the bottom of a quartz test tube into the quartz test tube;
4) After replacing the gas in the quartz tube with argon, heating the quartz tube at a position 8-15cm away from the bottom of the quartz tube under the vacuum-pumping condition to enable a convex point to appear at the position in the tube in the direction of the tube;
5) Placing the quartz plug into the quartz test tube in the step 4), enabling the plug to be in contact with the convex point manufactured in the step 4), replacing gas in the quartz test tube with argon, heating the outer wall of the quartz test tube under a vacuum condition, and enabling the quartz plug to be bonded with the quartz test tube so as to seal the quartz test tube;
6) The quartz tube is shaken to enable the quartz support to move to one side of the quartz plug, the magnesium grains are located at the bottom of the quartz tube, then the quartz tube is horizontally placed into a horizontal tube furnace, the magnesium grains are heated to 650-700 ℃ by utilizing the temperature gradient in the tube furnace, the porous silicon is at a relatively low temperature and is kept for 5-10 min, and then the quartz tube is quickly pushed out to be rapidly cooled, so that the residual oxide layer on the surface of the magnesium grains is cracked;
7) Vertically placing a quartz test tube, positioning a quartz plug above the quartz test tube, positioning magnesium granules below the quartz test tube, then placing the bottom of the quartz test tube into a heat insulation sleeve, and vertically placing the quartz test tube and the heat insulation sleeve into a vertical tubular furnace by using a lifter;
8) Heating magnesium particles to 500-600 ℃ by using the temperature gradient of the vertical tube furnace and the heat insulation effect of the heat insulation sleeve, heating the porous silicon wafer to 300-350 ℃, and keeping the temperature for 1-4 min, wherein the generated magnesium vapor can be condensed on the surface of the porous silicon wafer;
9) Moving the heat insulating sleeve and the quartz test tube downwards in the vertical tube furnace by a lifter to enable the porous silicon wafer to be at 500-600 ℃, the magnesium grains to be at 250-350 ℃, and keeping for 10-30 min to enable magnesium on the surface of the porous silicon wafer to react with the porous silicon to generate magnesium silicide;
10 Repeating the processes of step 8) and step 9) to prepare more magnesium silicide.
The magnesium particles are commercially available magnesium particles.
Due to the adoption of the technical scheme, the invention has the following advantages: 1. the device provided by the invention has the advantages that the main body material is completely quartz, although magnesium reacts with silicon dioxide, the main body is not greatly influenced, and impurities cannot be introduced into the porous silicon and magnesium silicide composite material; 2. the invention can easily adjust the distance between the magnesium and the porous silicon, thereby easily controlling the temperature difference between the magnesium and the porous silicon and further controlling the deposition and reaction rate of the magnesium on the porous silicon; 3. the magnesium particles in the invention firstly react with residual trace oxygen in the device to remove oxygen so as to prepare high-quality magnesium silicide; 4. the device prepares the magnesium silicide by two steps of repeated deposition of magnesium and magnesium-silicon reaction, so the reaction process has good controllability.
Drawings
FIG. 1 is a schematic structural diagram of an apparatus for preparing a porous silicon and magnesium silicide composite material according to the present invention;
FIG. 2 is a schematic view showing the construction of a quartz cuvette and its internal apparatus in the apparatus of the present invention;
FIG. 3 is a front view of the quartz holder of the present invention;
FIG. 4 is a top view of an insulating sleeve according to the present invention;
figure 5 is an XRD pattern of example 2 of the invention.
Detailed Description
The present invention will be described in detail below with reference to the drawings and examples.
A preparation device of porous silicon and magnesium silicide composite material is shown in figures 1-4 and comprises a quartz test tube 1, a quartz bracket 2, a quartz plug 3, a heat insulation sleeve 4, a lifter 5, a vertical tube furnace 6 and a high temperature resistance wire 7, wherein:
a convex point 11 towards the inner direction of the tube is arranged on the tube wall of the quartz test tube 1 at a distance of 1.5-3 cm from the bottom of the quartz test tube 1. The quartz holder 2 includes a cylindrical quartz substrate 21 and two quartz wires 22, and both ends of the quartz wires 22 are bonded to one end surface of the quartz substrate 21. The quartz plug 3 is 8-15cm away from the tube bottom of the quartz test tube 1 and is used for sealing the quartz test tube 1 in vacuum; the quartz bracket 2 is positioned between the convex point 11 of the tube wall of the quartz test tube 1 and the quartz plug 3 and can move back and forth; the heat insulation sleeve 4 comprises a cylindrical sleeve 41 and a high-temperature resistance wire grid 42, the cylindrical sleeve 41 is 1.5-3 cm high, the inner diameter of the cylindrical sleeve is larger than the outer diameter of the quartz test tube 1, the outer diameter of the cylindrical sleeve is smaller than the inner diameter of a furnace tube of the vertical tube furnace 6, and the high-temperature resistance wire grid 42 is fixed at one end of the heat insulation sleeve 41 and used for preventing the quartz test tube 1 from passing through; the heat insulation sleeve 4 is connected with the lifter 5 through a high temperature resistance wire 7; the lifter 5 is positioned right above the furnace mouth of the vertical tube furnace 6; the vertical tube furnace 6 is used to establish a temperature gradient for the quartz test tube 1.
When the quartz test tube 1 is heated in the vertical tube furnace 6, the bottom of the quartz test tube 1 is vertically placed in the heat insulation sleeve 4, and due to gravity factors, the quartz support 2 automatically moves downwards until the quartz support is clamped by the convex points 11, so that the porous silicon wafer 8 and the magnesium grains 9 on the quartz support 2 keep a distance of 1.5-3 cm. The quartz holder 2 can fix the porous silicon wafer without introducing impurities. The heat insulating sleeve 4 causes a large temperature difference between the porous silicon wafer 8 and the magnesium grains 9, and therefore the cylindrical sleeve 41 of the heat insulating sleeve 4 is made of a refractory heat insulating material such as alumina microspheres, ceramic fibers, or the like.
Compared with the prior art, the preparation device provided by the invention is simple to operate and low in cost, and can be used for preparing the high-quality porous silicon and magnesium silicide composite material.
Example 1
A preparation method of a porous silicon and magnesium silicide composite material comprises the following steps:
1) Removing an oxide layer on the surface of the magnesium grains 9 by cutting, and then putting the magnesium grains 9 into the bottom of the quartz test tube 1;
2) Corroding one surface of the silicon wafer by a known electrochemical anodic corrosion method to prepare a porous silicon wafer 8, wherein the porous silicon wafer 8 comprises a porous silicon layer 81 and a silicon substrate 82;
3) Fixing the prepared porous silicon wafer 8 on a quartz bracket 2, enabling a silicon substrate 82 to be in contact with a cylindrical quartz substrate 21 in the quartz bracket 2, and then putting a porous silicon layer 81 facing the bottom of a quartz test tube 1 into the quartz test tube 1;
4) After the gas in the quartz test tube 1 is replaced by argon, heating the position 8cm away from the tube bottom of the quartz test tube 1 under the vacuum condition to ensure that a convex point 12 towards the inner direction of the tube appears at the position;
5) Putting the quartz plug 3 into the quartz tube, enabling the quartz plug 3 to be in contact with the convex points 12 in the step 4), replacing gas in the quartz tube 1 with argon, heating the outer wall of the quartz tube 1 under a vacuum condition, and enabling the quartz plug 3 to be bonded with the tube wall of the quartz tube 1 so as to seal the quartz tube 1;
6) The quartz support 2 is moved to one side of the quartz plug 3 by shaking the quartz test tube 1, the magnesium grains 7 are positioned at the bottom of the quartz test tube 1, then the quartz test tube 1 is horizontally placed into a horizontal tube furnace, the temperature gradient in the tube furnace is utilized to heat the magnesium grains 7 to 650 ℃, the porous silicon wafer 8 is at a relatively low temperature and is kept for 10min, and then the quartz test tube 1 is quickly pushed out to be quickly cooled, so that the residual oxide layer on the surface of the magnesium grains 7 is cracked;
7) Vertically placing a quartz test tube 1, positioning a quartz plug 3 above a magnesium particle 7, automatically moving a quartz support 2 downwards until the quartz support is clamped by a convex point 11, then placing the bottom of the quartz test tube 1 into a heat insulation sleeve 4, and vertically placing the quartz test tube 1 and the heat insulation sleeve 4 into a vertical tube furnace 6 by using a lifter 5;
8) Heating the magnesium particles 7 to 500 ℃ and the porous silicon wafer 8 to 300 ℃ by utilizing the temperature gradient of the vertical tubular furnace 6 and the heat insulation effect of the heat insulation sleeve 4, and keeping the temperature for 4min to condense magnesium vapor on the surface of the porous silicon wafer 8;
9) The heat insulation sleeve 4 and the quartz test tube 1 are moved downwards in the vertical tube furnace 6 through the lifter 5, the porous silicon wafer 8 is kept at 500 ℃, the magnesium grains 7 are kept at 250 ℃ for 30min, and magnesium on the surface of the porous silicon wafer 8 reacts with the porous silicon layer 81 to generate magnesium silicide;
10 ) the heat insulating sleeve 4 and the quartz test tube 1 are naturally cooled, and then the processes of the step 8) and the step 9) are repeated to prepare more magnesium silicide.
Example 2
A preparation method of a porous silicon and magnesium silicide composite material comprises the following steps:
1) Removing an oxide layer on the surface of the magnesium grains 9 by cutting, and then putting the magnesium grains 9 into the bottom of the quartz test tube 1;
2) Corroding one surface of the silicon wafer by a known electrochemical anodic corrosion method to prepare a porous silicon wafer 8, wherein the porous silicon wafer 8 comprises a porous silicon layer 81 and a silicon substrate 82;
3) Fixing the prepared porous silicon wafer 8 on a quartz bracket 2, enabling a silicon substrate 82 to be in contact with a cylindrical quartz substrate 21 in the quartz bracket 2, and then placing a porous silicon layer 81 facing the bottom of a quartz test tube 1 into the quartz test tube 1;
4) After the gas in the quartz test tube 1 is replaced by argon, heating the position 11cm away from the tube bottom of the quartz test tube 1 under the vacuum condition to enable a convex point 12 towards the inner direction of the tube to appear at the position;
5) Putting the quartz plug 3 into the quartz tube, enabling the quartz plug 3 to be in contact with the convex points 12 in the step 4), replacing gas in the quartz tube 1 with argon, heating the outer wall of the quartz tube 1 under a vacuum condition, and enabling the quartz plug 3 to be bonded with the tube wall of the quartz tube 1 so as to seal the quartz tube 1;
6) The quartz support 2 is moved to one side of the quartz plug 3 by shaking the quartz test tube 1, the magnesium grains 7 are positioned at the bottom of the quartz test tube 1, then the quartz test tube 1 is horizontally placed into a horizontal tube furnace, the magnesium grains 7 are heated to 675 ℃ by utilizing the temperature gradient in the tube furnace, the porous silicon wafer 8 is at a relatively low temperature and is kept for 8min, and then the quartz test tube 1 is quickly pushed out to be rapidly cooled, so that the residual oxide layer on the surface of the magnesium grains 7 is cracked;
7) Vertically placing a quartz test tube 1, positioning a quartz plug 3 above a magnesium particle 7, automatically moving a quartz support 2 downwards until the quartz support is clamped by a convex point 11, then placing the bottom of the quartz test tube 1 into a heat insulation sleeve 4, and vertically placing the quartz test tube 1 and the heat insulation sleeve 4 into a vertical tube furnace 6 by using a lifter 5;
8) Heating magnesium particles 7 to 550 ℃ and a porous silicon wafer 8 to 325 ℃ by utilizing the temperature gradient of the vertical tubular furnace 6 and the heat insulation effect of the heat insulation sleeve 4, and keeping the temperature for 3min to condense magnesium vapor on the surface of the porous silicon wafer 8;
9) The heat insulation sleeve 4 and the quartz test tube 1 are moved downwards in the vertical tube furnace 6 through the lifter 5, so that the porous silicon wafer 8 is at 550 ℃, the magnesium grains 7 are at 300 ℃, and the temperature is kept for 20min, so that magnesium on the surface of the porous silicon wafer 8 reacts with the porous silicon layer 81 to generate magnesium silicide;
10 ) the heat insulating sleeve 4 and the quartz test tube 1 are naturally cooled, and then the processes of the step 8) and the step 9) are repeated to prepare more magnesium silicide.
The XRD test result of the porous silicon and magnesium silicide composite material is shown in fig. 5, which indicates that magnesium silicide is prepared.
Example 3
A preparation method of a porous silicon and magnesium silicide composite material comprises the following steps:
1) Removing an oxide layer on the surface of the magnesium grains 9 by cutting, and then putting the magnesium grains 9 into the bottom of the quartz test tube 1;
2) Corroding one surface of the silicon wafer by a known electrochemical anodic corrosion method to prepare a porous silicon wafer 8, wherein the porous silicon wafer 8 comprises a porous silicon layer 81 and a silicon substrate 82;
3) Fixing the prepared porous silicon wafer 8 on a quartz bracket 2, enabling a silicon substrate 82 to be in contact with a cylindrical quartz substrate 21 in the quartz bracket 2, and then placing a porous silicon layer 81 facing the bottom of a quartz test tube 1 into the quartz test tube 1;
4) After the gas in the quartz test tube 1 is replaced by argon, heating the position 15cm away from the tube bottom of the quartz test tube 1 under the vacuum condition to ensure that a convex point 12 towards the inner direction of the tube appears at the position;
5) Putting the quartz plug 3 into the quartz tube, enabling the quartz plug 3 to be in contact with the convex points 12 in the step 4), replacing gas in the quartz tube 1 with argon, heating the outer wall of the quartz tube 1 under a vacuum condition, and enabling the quartz plug 3 to be bonded with the tube wall of the quartz tube 1 so as to seal the quartz tube 1;
6) The quartz support 2 is moved to one side of the quartz plug 3 by shaking the quartz test tube 1, the magnesium grains 7 are positioned at the bottom of the quartz test tube 1, then the quartz test tube 1 is horizontally placed into a horizontal tube furnace, the magnesium grains 7 are heated to 700 ℃ by utilizing the temperature gradient in the tube furnace, the porous silicon wafer 8 is at a relatively low temperature and is kept for 5min, and then the quartz test tube 1 is quickly pushed out to be rapidly cooled, so that the residual oxide layer on the surface of the magnesium grains 7 is cracked;
7) Vertically placing a quartz test tube 1, positioning a quartz plug 3 above a magnesium particle 7, automatically moving a quartz support 2 downwards until the quartz support is clamped by a convex point 11, then placing the bottom of the quartz test tube 1 into a heat insulation sleeve 4, and vertically placing the quartz test tube 1 and the heat insulation sleeve 4 into a vertical tube furnace 6 by using a lifter 5;
8) Heating magnesium particles 7 to 600 ℃ and heating the porous silicon wafer 8 to 350 ℃ by utilizing the temperature gradient of the vertical tubular furnace 6 and the heat insulation effect of the heat insulation sleeve 4, and keeping the temperature for 1min to condense magnesium vapor on the surface of the porous silicon wafer 8;
9) The heat insulation sleeve 4 and the quartz test tube 1 are moved downwards in the vertical tube furnace 6 through the lifter 5, so that the porous silicon wafer 8 is at 600 ℃, the magnesium particles 7 are at 350 ℃, and the temperature is kept for 10min, so that magnesium on the surface of the porous silicon wafer 8 reacts with the porous silicon layer 81 to generate magnesium silicide;
10 ) the heat insulating sleeve 4 and the quartz test tube 1 are naturally cooled, and then the processes of the step 8) and the step 9) are repeated to prepare more magnesium silicide.

Claims (1)

1. A preparation method of a porous silicon and magnesium silicide composite material is characterized by comprising the following steps:
1) Removing an oxide layer on the surface of the magnesium grains by cutting, and then putting the magnesium grains at the bottom of a quartz test tube;
2) Preparing porous silicon by corroding one surface of a silicon wafer by an electrochemical anodic corrosion method;
3) Fixing the prepared porous silicon wafer on a quartz bracket, enabling the non-corroded surface to be in contact with a cylindrical quartz substrate in the quartz bracket, and then placing the porous silicon surface facing the bottom of a quartz test tube into the quartz test tube;
4) After replacing the gas in the quartz tube with argon, heating the position 8-15cm away from the bottom of the quartz tube under the vacuum condition to enable a convex point to appear in the position towards the inner direction of the tube;
5) Placing a quartz plug into the quartz test tube in the step 4), enabling the plug to be in contact with the convex points manufactured in the step 4), replacing gas in the quartz test tube with argon, heating the outer wall of the quartz test tube under a vacuum condition, and enabling the quartz plug to be bonded with the quartz test tube to seal the quartz test tube;
6) The quartz tube is shaken to enable the quartz support to move to one side of the quartz plug, the magnesium grains are located at the bottom of the quartz tube, then the quartz tube is horizontally placed into a horizontal tube furnace, the temperature gradient in the tube furnace is utilized to enable the magnesium grains to be heated to 650-700 ℃, the temperature is kept for 5-10 min, then the quartz tube is rapidly pushed out to be rapidly cooled, and the residual oxide layer on the surface of the magnesium grains is broken;
7) Vertically placing a quartz test tube, positioning a quartz plug above the quartz test tube, positioning magnesium granules below the quartz test tube, then placing the bottom of the quartz test tube into a heat insulation sleeve, and vertically placing the quartz test tube and the heat insulation sleeve into a vertical tubular furnace by using a lifter;
8) Heating magnesium particles to 500-600 ℃ by utilizing the temperature gradient of a vertical tubular furnace and the heat insulation effect of a heat insulation sleeve, heating a porous silicon wafer to 300-350 ℃, and keeping the temperature for 1-4 min to generate magnesium vapor which is condensed on the surface of the porous silicon wafer;
9) Moving the heat insulating sleeve and the quartz test tube downwards in the vertical tube furnace by a lifter to enable the porous silicon wafer to be at 500-600 ℃, the magnesium grains to be at 250-350 ℃, and keeping for 10-30 min to enable magnesium on the surface of the porous silicon wafer to react with the porous silicon to generate magnesium silicide;
10 Repeating the processes of step 8) and step 9) to prepare more magnesium silicide;
the preparation device adopted in the preparation process comprises a quartz test tube, a quartz bracket, a quartz plug, a heat insulation sleeve, a lifter, a vertical tube furnace and a high-temperature resistance wire;
a convex point towards the inner direction of the tube is arranged on the tube wall of the quartz test tube at a position 1.5-3 cm away from the bottom of the quartz test tube; the quartz support comprises a cylindrical quartz substrate and two quartz wires, and two ends of each quartz wire are bonded on one end face of the quartz substrate; the quartz plug is 8-15cm away from the bottom of the quartz test tube and is used for sealing the quartz test tube in vacuum; the quartz bracket is positioned between the convex point of the quartz test tube wall and the quartz plug and can move back and forth; the heat insulation sleeve comprises a cylindrical sleeve and a high-temperature resistance wire grid, the cylindrical sleeve is 1.5-3 cm high, the inner diameter of the cylindrical sleeve is larger than the outer diameter of the quartz test tube, the outer diameter of the cylindrical sleeve is smaller than the inner diameter of the furnace tube of the vertical tube furnace, and the high-temperature resistance wire grid is fixed at one end of the cylindrical sleeve and used for preventing the quartz test tube from passing through; the heat insulation sleeve is connected with the lifter through a high-temperature resistance wire; the lifter is positioned right above the furnace mouth of the vertical tube furnace; the vertical tube furnace is used for establishing a temperature gradient for a quartz test tube, and the cylindrical sleeve of the heat insulation sleeve is composed of refractory heat insulation materials made of alumina microspheres or ceramic fibers.
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