CN112520693A - Device and process for heat treatment of waste silicon wafers - Google Patents
Device and process for heat treatment of waste silicon wafers Download PDFInfo
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- CN112520693A CN112520693A CN202011393360.4A CN202011393360A CN112520693A CN 112520693 A CN112520693 A CN 112520693A CN 202011393360 A CN202011393360 A CN 202011393360A CN 112520693 A CN112520693 A CN 112520693A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
- C01B3/06—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of inorganic compounds containing electro-positively bound hydrogen, e.g. water, acids, bases, ammonia, with inorganic reducing agents
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
- C01B3/06—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of inorganic compounds containing electro-positively bound hydrogen, e.g. water, acids, bases, ammonia, with inorganic reducing agents
- C01B3/08—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of inorganic compounds containing electro-positively bound hydrogen, e.g. water, acids, bases, ammonia, with inorganic reducing agents with metals
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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
- 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
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Abstract
The invention discloses a device and a process for heat treatment of waste silicon chips; the heat treatment device comprises a device main body, a heater, a cover body and a stainless steel condenser pipe; the device main body is a semi-closed hollow cylinder, stainless steel condenser pipes are fully distributed at the top end and two sides of the hollow cylinder, and heat insulation sheets cover the surfaces of the stainless steel condenser pipes; a heater is arranged right below the hollow cylinder; a cover body is arranged in front of the hollow cylinder, stainless steel condenser pipes are arranged on two sides of the cover body, and a stainless steel exhaust pipe is arranged in front of the cover body; the heat treatment process using the device is to take a waste silicon slice as a raw material, laminate the waste silicon slice with a reduction alloy slice, put the reduction alloy slice into the device and carry out heat treatment; then mixing with low-boiling point metal salt, heating, annealing, and repeating circularly to obtain the silicon-based hydrogen production material; the heat treatment device has simple structure and convenient use, and the silicon-based hydrogen production material prepared by the device has high chemical activity; therefore, the device and the process for heat treatment of the waste silicon wafer have good application prospects in the field of hydrogen production.
Description
Technical Field
The invention belongs to the field of hydrogen production, and particularly relates to a device and a process for heat treatment of waste silicon wafers.
Background
In recent years, a solar cell taking silicon as a main component has come to the end of life, and how to treat waste silicon wafers is a problem that governments face environmental pollution and need to solve urgently. Silicon is known to be a promising hydrogen production material; reaction with alkali can yield appreciable hydrogen. Many documents report the technology of preparing hydrogen by reacting silicon with sodium hydroxide and calcium hydroxide; and the specific surface area of the silicon is increased by doping, electrochemical corrosion and other technologies, so that the chemical reaction activity of the silicon is improved. However, the strong alkaline solution is corrosive, has high requirements on equipment materials, and can bring harm to users.
Disclosure of Invention
Aiming at the defects of the prior technical scheme, the invention aims to provide a device and a process for heat treatment of waste silicon wafers, overcome the defects of the prior preparation technology and improve the chemical activity of silicon materials.
In order to achieve the purpose, the technical scheme of the invention is as follows: an apparatus for heat treatment of waste silicon wafers comprises an apparatus main body, a heater, a cover body and a stainless steel condenser pipe; the method is characterized in that: the device main body is a semi-closed hollow cylinder, stainless steel condenser pipes are fully distributed at the top end and two sides of the hollow cylinder, and heat insulation sheets cover the surfaces of the stainless steel condenser pipes; a heater is arranged right below the hollow cylinder; a cover body is arranged in front of the hollow cylinder, stainless steel condenser pipes are arranged on two sides of the cover body, a stainless steel exhaust pipe is arranged in front of the cover body, and the stainless steel exhaust pipe is connected with an air pump;
a process for heat treatment of waste silicon wafers; stacking waste silicon wafers serving as raw materials with reduced alloy sheets, briquetting and carrying out heat treatment; then mixing with low-boiling point metal salt, heating and annealing to obtain the silicon-based hydrogen production material; the mass ratio of the silicon chip to the reduction alloy sheet is 0.2-2; the reduction alloy sheet is ternary, quaternary or above alloy mainly containing aluminum, and comprises high-reduction metal and low-melting-point metal; 75-90 wt% of aluminum, 5-20 wt% of high reducing metal and 5-10 wt% of low melting point metal; the high reducing metal is one or more of lithium, sodium, calcium and potassium, and the low melting point metal is one or more of bismuth, tin, indium, gallium and lead; the low boiling point metal salt is one of aluminum chloride, stannous chloride and stannic chloride, and the low boiling point metal salt accounts for 0.1-10 wt% of the total mass of the silicon chip and the reduction alloy chip surface; a process for heat-treating a waste silicon wafer, comprising:
1) weighing a certain mass of waste silicon sheets and reduction alloy sheets, laminating and briquetting;
2) putting the product obtained in the step 1) into a heat treatment device, fixing a cover body, vacuumizing, opening stainless steel condenser pipes at two sides of the cover body for condensing water, starting a heater, heating the main body of the heat treatment device to 500-;
3) closing the heater, and naturally cooling the main body of the heat treatment device in the step 2) to 250-500 ℃; then opening a stainless steel condenser pipe condensate on the surface of the hollow cylinder, and rapidly annealing to normal temperature; standing for 1-3 h;
4) crushing the product of the step 3) and mixing with a low-boiling point metal salt; then putting the cover body into a heat treatment device, fixing the cover body, vacuumizing, opening stainless steel condensation pipes on two sides of the cover body, and heating the heat treatment device body to 250-500 ℃;
5) turning off the heater, opening the stainless steel condenser pipe condensate water on the surface of the hollow cylinder, and rapidly annealing the main body of the heat treatment device in the step 4) to normal temperature; standing for 1-3 h; closing the stainless steel condenser pipe condensate water on the surface of the hollow cylinder, starting the heater, and heating the heat treatment device main body to 250-500 ℃; then the heater is closed, the stainless steel condenser pipe condensate water on the surface of the hollow cylinder is opened, and the main body of the heat treatment device is rapidly annealed to normal temperature; the heating and annealing cycle is repeated for 2-5 times; obtaining the silicon-based hydrogen production material.
The patent relates to a device and a process for heat treatment of waste silicon wafers; the chemical reaction activity of the silicon is improved through silicon alloying, salt doping and heat treatment processes; designing a heat treatment device, and preparing silicon alloy, salt doping and silicon alloy disordering through heating and annealing; the reaction of the 4-element or even 5-element reduction alloy and silicon is beneficial to reducing the formation temperature of the silicon alloy; then, adopting low-boiling-point metal salt to realize that the salt is fully doped into the surface of the alloy; compared with the prior art, the method for treating the waste silicon wafer for preparing hydrogen by hydrolysis provided by the invention has the following advantages:
1) the preparation process is simple, the working procedures are controllable, and industrial production can be realized;
2) the heat treatment device is designed to be multifunctional and is used for alloy preparation and annealing; the design of the heat treatment device is simplified, and the heat treatment device does not need to be moved in the heating and condensing process;
3) the waste silicon wafer is recycled, which is beneficial to reducing environmental pollution; the silicon-based hydrogen production material has high chemical activity, mild hydrolysis condition and large hydrogen production;
4) the reduction alloy is adopted to react with silicon, which is beneficial to forming silicon alloy at a reduced temperature; the low boiling point metal salt is adopted, so that the salt is favorably fully doped on the surface of the silicon alloy; the annealing process is adopted, and the silicon alloy is disordered and amorphized, so that the specific surface area and the chemical activity of the silicon alloy are improved;
5) the silicon-based hydrogen production material has the advantages that the alloy components are uniformly distributed and amorphized, and a micro-corrosion area of a high-concentration metal salt solution is easily formed in the hydrolysis process of the structure, so that the chemical reaction activity of the silicon alloy is greatly improved; the silicon-based hydrogen production material has good application prospect in the field of hydrogen production.
Description of the drawings:
FIG. 1 is a schematic view showing the construction of an apparatus for heat-treating a waste silicon wafer.
In the figure, the position of the upper end of the main shaft,
1. a heater; 2. a stainless steel exhaust tube; 3. a cover body; 4. a stainless steel condenser tube; 5. a device main body; 6. a heat insulating sheet.
Detailed Description
In order to further understand the contents, features and effects of the present invention, the following embodiments are described in detail as follows:
example 1
An apparatus for heat treatment of waste silicon wafers comprises an apparatus main body, a heater, a cover body and a stainless steel condenser pipe; the method is characterized in that: the device main body is a semi-closed hollow cylinder, stainless steel condenser pipes are fully distributed at the top end and two sides of the hollow cylinder, and heat insulation sheets cover the surfaces of the stainless steel condenser pipes; a heater is arranged right below the hollow cylinder; a cover body is arranged in front of the hollow cylinder, stainless steel condenser pipes are arranged on two sides of the cover body, a stainless steel exhaust pipe is arranged in front of the cover body, and the stainless steel exhaust pipe is connected with an air pump;
a process for heat treating a waste silicon wafer, comprising:
1) weighing a certain mass of waste silicon sheets and reduction alloy sheets, laminating and briquetting;
2) putting the product obtained in the step 1) into a heat treatment device, fixing a cover body, vacuumizing, opening stainless steel condenser pipes at two sides of the cover body to condense water, starting a heater, heating the main body of the heat treatment device to 600 ℃, and standing for 5 hours;
3) turning off the heater, and naturally cooling the main body of the heat treatment device in the step 2) to 300 ℃; then opening a stainless steel condenser pipe condensate on the surface of the hollow cylinder, and rapidly annealing to normal temperature; standing for 2 h;
4) crushing the product of the step 3) and mixing with a low-boiling point metal salt; then putting the cover body into a heat treatment device, fixing the cover body, vacuumizing, opening stainless steel condenser pipes at two sides of the cover body to condense water, and heating a main body of the heat treatment device to 300 ℃;
5) turning off the heater, opening the stainless steel condenser pipe condensate water on the surface of the hollow cylinder, and rapidly annealing the main body of the heat treatment device in the step 4) to normal temperature; standing for 2 h; closing the stainless steel condenser pipe condensate water on the surface of the hollow cylinder, starting a heater, and heating the heat treatment device main body to 300 ℃; then the heater is closed, the stainless steel condenser pipe condensate water on the surface of the hollow cylinder is opened, and the main body of the heat treatment device is rapidly annealed to normal temperature; the heating and annealing cycle is repeated for 2 times; obtaining the silicon-based hydrogen production material.
The composition design of the waste silicon wafer comprises the following steps:
1) silicon wafer, 27.6 g; reduced alloy sheet, 24g (aluminum, 20 g; lithium, 1.6 g; tin, 1 g; bismuth, 0.4 g); 1g of stannous chloride;
hydrolysis experiments show that the silicon-based hydrogen production material prepared by the waste silicon slice heat treatment device and the process has good hydrolysis performance in 50-degree hot water.
Example 2
A process for heat treating a waste silicon wafer, comprising:
1) weighing a certain mass of waste silicon sheets and reduction alloy sheets, laminating and briquetting;
2) putting the product obtained in the step 1) into a heat treatment device, fixing a cover body, vacuumizing, opening stainless steel condenser pipes at two sides of the cover body to condense water, starting a heater, heating the main body of the heat treatment device to 500 ℃, and standing for 10 hours;
3) turning off the heater, and naturally cooling the main body of the heat treatment device in the step 2) to 400 ℃; then opening a stainless steel condenser pipe condensate on the surface of the hollow cylinder, and rapidly annealing to normal temperature; standing for 3 h;
4) crushing the product of the step 3) and mixing with a low-boiling point metal salt; then putting the cover body into a heat treatment device, fixing the cover body, vacuumizing, opening stainless steel condenser pipes on two sides of the cover body to condense water, and heating a main body of the heat treatment device to 400 ℃;
5) turning off the heater, opening the stainless steel condenser pipe condensate water on the surface of the hollow cylinder, and rapidly annealing the main body of the heat treatment device in the step 4) to normal temperature; standing for 3 h; closing the stainless steel condenser pipe condensate water on the surface of the hollow cylinder, starting a heater, and heating the heat treatment device main body to 400 ℃; then the heater is closed, the stainless steel condenser pipe condensate water on the surface of the hollow cylinder is opened, and the main body of the heat treatment device is rapidly annealed to normal temperature; the heating and annealing cycle is repeated for 3 times; obtaining the silicon-based hydrogen production material.
The composition design of the waste silicon wafer comprises the following steps:
2) 20g of silicon wafer; 30g of reduced alloy sheet (aluminum, 26 g; lithium, 1.5 g; sodium, 0.3 g; indium, 0.8 g; gallium, 1.4 g); 1g of aluminum chloride;
3) 15g of silicon wafer; 20g of reduced alloy flakes (aluminum, 16 g; lithium, 1.6 g; calcium, 0.4 g; indium, 0.6 g; bismuth, 1.4 g); 1g of tin chloride;
hydrolysis experiments show that the silicon-based hydrogen production material prepared by the waste silicon slice heat treatment device and the process has good hydrolysis performance in 50-degree hot water.
Example 3
The procedure was as in example 1
The composition design of the waste silicon wafer comprises the following steps:
4) 20g of silicon wafer; reduced alloy flakes, 20g (aluminum, 15 g; lithium, 2 g; lead, 2 g; tin, 1 g); 1g of aluminum chloride;
5) 15g of silicon wafer; 10g of reduced alloy sheet (aluminum, 8 g; lithium, 0.8 g; calcium, 0.4 g; tin, 0.8 g; B); 1g of stannous chloride;
hydrolysis experiments show that the silicon-based hydrogen production material has good hydrolysis performance in hot water of 50 ℃.
The above-described embodiments of the patent are intended to be illustrative, but not limiting, of the scope of the patent, which is included for the purpose of better understanding the patent by those skilled in the art; any equivalent alterations or modifications made according to the spirit of the disclosure of this patent are intended to be included in the scope of this patent.
Claims (2)
1. An apparatus for heat treatment of waste silicon wafers comprises an apparatus main body, a heater, a cover body and a stainless steel condenser pipe; the method is characterized in that: the device main body is a semi-closed hollow cylinder, stainless steel condenser pipes are fully distributed at the top end and two sides of the hollow cylinder, and heat insulation sheets cover the surfaces of the stainless steel condenser pipes; a heater is arranged right below the hollow cylinder; the front of the hollow cylinder is provided with a cover body, two sides of the cover body are provided with stainless steel condenser pipes, and the front of the cover body is provided with a stainless steel exhaust pipe which is connected with an air pump.
2. A process for heat treatment of waste silicon wafers; stacking waste silicon wafers serving as raw materials with reduced alloy sheets, briquetting and carrying out heat treatment; then mixing with low-boiling point metal salt, heating and annealing to obtain the silicon-based hydrogen production material; the mass ratio of the silicon chip to the reduction alloy sheet is 0.2-2; the reduction alloy sheet is ternary, quaternary or above alloy mainly containing aluminum, and comprises high-reduction metal and low-melting-point metal; 75-90 wt% of aluminum, 5-20 wt% of high reducing metal and 5-10 wt% of low melting point metal; the high reducing metal is one or more of lithium, sodium, calcium and potassium, and the low melting point metal is one or more of bismuth, tin, indium, gallium and lead; the low boiling point metal salt is one of aluminum chloride, stannous chloride and stannic chloride, and the low boiling point metal salt accounts for 0.1-10 wt% of the total mass of the silicon chip and the reduction alloy chip surface; a process for heat-treating a waste silicon wafer, comprising:
1) weighing a certain mass of waste silicon sheets and reduction alloy sheets, laminating and briquetting;
2) putting the product obtained in the step 1) into a heat treatment device, fixing a cover body, vacuumizing, opening stainless steel condenser pipes at two sides of the cover body for condensing water, starting a heater, heating the main body of the heat treatment device to 500-;
3) closing the heater, and naturally cooling the main body of the heat treatment device in the step 2) to 250-500 ℃; then opening a stainless steel condenser pipe condensate on the surface of the hollow cylinder, and rapidly annealing to normal temperature; standing for 1-3 h;
4) crushing the product of the step 3) and mixing with a low-boiling point metal salt; then putting the cover body into a heat treatment device, fixing the cover body, vacuumizing, opening stainless steel condensation pipes on two sides of the cover body, and heating the heat treatment device body to 250-500 ℃;
5) turning off the heater, opening the stainless steel condenser pipe condensate water on the surface of the hollow cylinder, and rapidly annealing the main body of the heat treatment device in the step 4) to normal temperature; standing for 1-3 h; closing the stainless steel condenser pipe condensate water on the surface of the hollow cylinder, starting the heater, and heating the heat treatment device main body to 250-500 ℃; then the heater is closed, the stainless steel condenser pipe condensate water on the surface of the hollow cylinder is opened, and the main body of the heat treatment device is rapidly annealed to normal temperature; the heating and annealing cycle is repeated for 2-5 times; obtaining the silicon-based hydrogen production material.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2011070849A1 (en) * | 2009-12-10 | 2011-06-16 | セントラル硝子株式会社 | Alloy for hydrogen generation and method for producing same |
| CN102408096A (en) * | 2011-07-26 | 2012-04-11 | 辽宁师范大学 | Aluminum-based composite hydrogen manufacturing material and preparation method thereof |
| CN202667613U (en) * | 2012-05-03 | 2013-01-16 | 中国计量学院 | Ternary-system aluminum lithium alloy manufacturing device for hydrogen generation |
| CN107195895A (en) * | 2017-01-06 | 2017-09-22 | 中国计量大学 | A kind of silica-base material preparation method using alloy as reducing agent |
| CN107188123A (en) * | 2017-01-06 | 2017-09-22 | 中国计量大学 | A kind of preparation method of silicon/alkali metal hydrogen manufacturing material |
| CN111424314A (en) * | 2020-04-30 | 2020-07-17 | 包头美科硅能源有限公司 | Gallium-silicon alloy manufacturing furnace for gallium-doped monocrystalline silicon and manufacturing method thereof |
-
2020
- 2020-12-02 CN CN202011393360.4A patent/CN112520693B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2011070849A1 (en) * | 2009-12-10 | 2011-06-16 | セントラル硝子株式会社 | Alloy for hydrogen generation and method for producing same |
| CN102408096A (en) * | 2011-07-26 | 2012-04-11 | 辽宁师范大学 | Aluminum-based composite hydrogen manufacturing material and preparation method thereof |
| CN202667613U (en) * | 2012-05-03 | 2013-01-16 | 中国计量学院 | Ternary-system aluminum lithium alloy manufacturing device for hydrogen generation |
| CN107195895A (en) * | 2017-01-06 | 2017-09-22 | 中国计量大学 | A kind of silica-base material preparation method using alloy as reducing agent |
| CN107188123A (en) * | 2017-01-06 | 2017-09-22 | 中国计量大学 | A kind of preparation method of silicon/alkali metal hydrogen manufacturing material |
| CN111424314A (en) * | 2020-04-30 | 2020-07-17 | 包头美科硅能源有限公司 | Gallium-silicon alloy manufacturing furnace for gallium-doped monocrystalline silicon and manufacturing method thereof |
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