CN112030224A - Method for manufacturing arsenic rod for molecular beam epitaxy - Google Patents
Method for manufacturing arsenic rod for molecular beam epitaxy Download PDFInfo
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- CN112030224A CN112030224A CN202010915130.3A CN202010915130A CN112030224A CN 112030224 A CN112030224 A CN 112030224A CN 202010915130 A CN202010915130 A CN 202010915130A CN 112030224 A CN112030224 A CN 112030224A
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
- C30B23/02—Epitaxial-layer growth
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
- C30B25/02—Epitaxial-layer growth
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Abstract
The invention discloses a method for manufacturing an arsenic rod for molecular beam epitaxy, which specifically comprises the following steps of 1: basic processing of the relevant equipment, step 2: basic operation of the quartz tube, step 3: primary processing of arsenic particles, step 4: high-order processing of arsenic particles, step 5: and (3) secondary melting of arsenic particles, step 6: the invention discloses basic molding of arsenic particles, and relates to the technical field of arsenic rods. This molecular beam epitaxy uses arsenic stick's manufacturing method for arsenic granule can be through the preliminary melting of high-order processing, then the rethread secondary melts, make arsenic granule thoroughly melt in high temperature high-pressure furnace, so that the follow-up can be the shaping smoothly, avoided arsenic granule because the incomplete shaping effect that leads to of melting is not good, indirect qualification rate and the product quality that has improved the later stage product, raw materials arsenic granule can directly get into the helium gas guarantor environment, the effectual oxidation of avoiding arsenic granule, impurity generation in the arsenic stick manufacturing process has been avoided.
Description
Technical Field
The invention relates to the technical field of arsenic rods, in particular to a method for manufacturing an arsenic rod for molecular beam epitaxy.
Background
Arsenic is a nonmetallic element, which is located in the 4 th cycle and the VA group in the periodic table of chemical elements, has the atomic number of 33 and the symbol of As, and exists As three allotropes of ash arsenic, black arsenic and yellow arsenic. Arsenic is widely present in nature, and hundreds of arsenic minerals are found. Arsenic and its compounds are used in pesticides, herbicides, insecticides, and many alloys. Arsenic trioxide, a compound of arsenic trioxide, is called arsenic trioxide, and is a substance with strong toxicity. As an alloy additive, arsenic is used to produce lead-made shot, printing alloy, brass (for condenser), accumulator grid plate, antiwear alloy, high-strength structural steel, corrosion-resistant steel, etc. Dezincification is prevented when brass contains arsenic by weight. High-purity arsenic is a raw material for producing compound semiconductors, such as gallium arsenide and indium arsenide, and is also a doping element for semiconductor materials, such as germanium and silicon, and these materials are widely used as diodes, light emitting diodes, infrared emitters, lasers, and the like.
With the development of the related electronic industry, the related requirements of arsenic rods are higher and higher, but free arsenic elements are quite active, and the arsenic elements are very easy to generate oxidation reaction with air at normal room temperature and in an air state to form related compounds, so that the production of related arsenic elemental rods is seriously influenced.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides a method for manufacturing an arsenic rod for molecular beam epitaxy, which solves the problems that the related requirements of the arsenic rod are higher and higher along with the development of related electronic industries, but free arsenic element is quite active, the arsenic element is very easy to generate oxidation reaction with air under normal room temperature and air state to form related compounds, the quality of high-purity arsenic is seriously influenced, and meanwhile, the arsenic rod is more convenient to use generally in molecular epitaxy.
(II) technical scheme
In order to achieve the purpose, the invention is realized by the following technical scheme: a method for manufacturing an arsenic rod for molecular beam epitaxy specifically comprises the following steps:
step 1: basic processing of the related devices: cleaning the inside and outside of a quartz tube by using distilled water, wiping the quartz tube dry after cleaning, quickly cleaning the quartz tube by using hydrofluoric acid, completely cleaning silicon dioxide powder on the surface of the quartz tube, then cleaning the quartz tube when soaking the quartz tube by using the distilled water, completely cleaning the inner surface and the outer surface of the quartz tube, and completely rotating and drying the quartz tube after completely cleaning;
step 2: basic operation of the quartz tube: putting the quartz tube into a helium protective environment, loading arsenic particles into the quartz tube, vacuumizing the quartz tube by using a vacuum machine, and then sealing the quartz tube;
and step 3: primary processing of arsenic particles: placing the quartz tube loaded with the arsenic particles in a sealed high-temperature high-pressure furnace, raising the temperature in the furnace to 700-;
and 4, step 4: high-order processing of arsenic particles: adding sufficient helium into the high-temperature high-pressure furnace, fully heating the quartz tube when the high-temperature high-pressure furnace is filled with high-pressure inert gas, basically melting the arsenic particles when the temperature is heated to 800-;
and 5: secondary melting of arsenic particles: observing the state of the arsenic particles in the high-temperature and high-pressure furnace through the isolation window, starting heating operation for the second time when the temperature is reduced to 600-650 ℃, increasing the temperature of the high-temperature and high-pressure furnace to 920 ℃, completely melting the arsenic particles, and then continuously preserving the heat for 20 minutes;
step 6: basic shaping of arsenic particles: stopping heating, automatically cooling the molten arsenic particles in the quartz tube, and then when the temperature is reduced to room temperature, remolding the arsenic particles into a rod shape to be loaded in a sealing way.
Preferably, in the step 1, the concentration of the hydrofluoric acid is 4%.
Preferably, in the step 1, the inside of the quartz tube is dried synchronously.
Preferably, in the step 2, a clamping device is used for loading the arsenic particles into the quartz tube.
Preferably, in the step 2, the vacuum is pumped to 10-2MPa。
Preferably, in the step 1, an infrared lamp drying oven quartz tube is used for drying.
Preferably, in the step 3, an infrared thermometer is adopted to assist in measuring the temperature of the oven cavity.
Preferably, in the step 5, the high-temperature high-pressure furnace is completely sealed when in operation.
(III) advantageous effects
The invention provides a method for manufacturing an arsenic rod for molecular beam epitaxy. Compared with the prior art, the method has the following beneficial effects:
(1) the method for manufacturing the arsenic rod for molecular beam epitaxy comprises the following steps of: high-order processing of arsenic particles: adding sufficient helium into the high-temperature high-pressure furnace, fully heating the quartz tube when the high-temperature high-pressure furnace is filled with high-pressure inert gas, basically melting the arsenic particles when the temperature is heated to 800-; and 5: secondary melting of arsenic particles: the arsenic particle state of the high-temperature high-pressure furnace inside is observed through the isolation window, when the temperature is reduced to 600-650 ℃, the heating operation is started for the second time, the temperature of the high-temperature high-pressure furnace is increased to 920 ℃ for the second time, the arsenic particles are completely melted, then the heat is continuously preserved for 20 minutes, through the combined setting of the step 4 and the step 5, the arsenic particles can be preliminarily melted through high-order processing, then the secondary melting is carried out, the arsenic particles are completely melted in the high-temperature high-pressure furnace, the subsequent smooth forming is carried out, the poor forming effect caused by incomplete melting of the arsenic particles is avoided, and the qualification rate and the product quality of products in the later period are indirectly improved.
(2) The method for manufacturing the arsenic rod for molecular beam epitaxy comprises the following steps of: basic operation of the quartz tube: putting the quartz tube into a helium protective environment, loading arsenic particles into the quartz tube, vacuumizing the quartz tube by using a vacuum machine, and then sealing the quartz tube; and step 3: primary processing of arsenic particles: the method comprises the steps of placing a quartz tube loaded with arsenic particles in a sealed high-temperature high-pressure furnace, raising the temperature in the furnace to 700-.
(3) The method for manufacturing the arsenic rod for molecular beam epitaxy comprises the following steps of 1: basic processing of the related devices: clean with the inside and outside use distilled water of quartz capsule, clean the back that finishes, dry it, adopt hydrofluoric acid to wash the quartz capsule fast, clean the silica powder on quartz capsule surface comprehensively, then use distilled water to wash when soaking the quartz capsule, after the comprehensive washing, clean the back with the inside and outside surface of quartz capsule, rotate the stoving comprehensively, step 6: basic shaping of arsenic particles: stopping heating, the melting arsenic granule in the quartz capsule is cooling by oneself, then when the temperature reduces to the room temperature, the arsenic granule remolds into the bar-like sealed loading, through step 1 and step 6's joint setting, through the relevant processing to the quartz capsule of participation work, can effectually get rid of the impurity in the relevant manufacture process, has avoided the influence of impurity to the final product to relevant processing step is very simple and convenient, and the processing logic is very clear.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the attached tables in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to table 1, the embodiment of the present invention provides three technical solutions: a method for manufacturing an arsenic rod for molecular beam epitaxy specifically comprises the following embodiments:
example 1
Step 1: basic processing of the related devices: cleaning the inside and outside of a quartz tube by using distilled water, wiping the quartz tube dry after cleaning, quickly cleaning the quartz tube by using hydrofluoric acid, completely cleaning silicon dioxide powder on the surface of the quartz tube, then cleaning the quartz tube when soaking the quartz tube by using the distilled water, completely cleaning the inner surface and the outer surface of the quartz tube, and completely rotating and drying the quartz tube after completely cleaning;
step 2: basic operation of the quartz tube: putting the quartz tube into a helium protective environment, loading arsenic particles into the quartz tube, vacuumizing the quartz tube by using a vacuum machine, and then sealing the quartz tube;
and step 3: primary processing of arsenic particles: placing the quartz tube loaded with the arsenic particles in a sealed high-temperature high-pressure furnace, raising the temperature in the furnace to 700 ℃, primarily sublimating the arsenic particles, then keeping the temperature for 5 minutes, stopping the furnace, when the temperature is reduced by 220 ℃, starting the high-temperature high-pressure furnace again, raising the temperature to 750 ℃ again, keeping the temperature for 15 minutes, and completely removing oxide films in the arsenic particles;
and 4, step 4: high-order processing of arsenic particles: adding sufficient helium into the high-temperature high-pressure furnace, fully heating the quartz tube when the high-temperature high-pressure furnace is filled with high-pressure inert gas, basically melting arsenic particles when the temperature is heated to 800 ℃, suspending heating, and automatically cooling the quartz tube;
and 5: secondary melting of arsenic particles: observing the state of arsenic particles in the high-temperature and high-pressure furnace through the isolation window, starting heating operation for the second time when the temperature is reduced to 600 ℃, increasing the temperature of the high-temperature and high-pressure furnace to 920 ℃ for the second time, completely melting the arsenic particles, and then continuously preserving the heat for 20 minutes;
step 6: basic shaping of arsenic particles: stopping heating, automatically cooling the molten arsenic particles in the quartz tube, and then when the temperature is reduced to room temperature, remolding the arsenic particles into a rod shape to be loaded in a sealing way.
Example 2
Step 1: basic processing of the related devices: cleaning the inside and outside of a quartz tube by using distilled water, wiping the quartz tube dry after cleaning, quickly cleaning the quartz tube by using hydrofluoric acid, completely cleaning silicon dioxide powder on the surface of the quartz tube, then cleaning the quartz tube when soaking the quartz tube by using the distilled water, completely cleaning the inner surface and the outer surface of the quartz tube, and completely rotating and drying the quartz tube after completely cleaning;
step 2: basic operation of the quartz tube: putting the quartz tube into a helium protective environment, loading arsenic particles into the quartz tube, vacuumizing the quartz tube by using a vacuum machine, and then sealing the quartz tube;
and step 3: primary processing of arsenic particles: placing the quartz tube loaded with the arsenic particles in a sealed high-temperature high-pressure furnace, raising the temperature in the furnace to 725 ℃, primarily sublimating the arsenic particles, then keeping the temperature for 5 minutes, stopping the furnace, when the temperature is reduced by 220 ℃, starting the high-temperature high-pressure furnace again, raising the temperature to 750 ℃ again, keeping the temperature for 22.5 minutes, and completely removing an oxidation film in the arsenic particles;
and 4, step 4: high-order processing of arsenic particles: adding sufficient helium into the high-temperature high-pressure furnace, fully heating the quartz tube when the high-temperature high-pressure furnace is filled with high-pressure inert gas, basically melting arsenic particles when the temperature is 825 ℃, suspending heating, and automatically cooling the quartz tube;
and 5: secondary melting of arsenic particles: observing the state of arsenic particles in the high-temperature and high-pressure furnace through the isolation window, starting heating operation for the second time when the temperature is reduced to 625 ℃, increasing the temperature of the high-temperature and high-pressure furnace to 920 ℃ for the second time, completely melting the arsenic particles, and then continuously preserving the heat for 20 minutes;
step 6: basic shaping of arsenic particles: stopping heating, automatically cooling the molten arsenic particles in the quartz tube, and then when the temperature is reduced to room temperature, remolding the arsenic particles into a rod shape to be loaded in a sealing way.
Example 3
Step 1: basic processing of the related devices: cleaning the inside and outside of a quartz tube by using distilled water, wiping the quartz tube dry after cleaning, quickly cleaning the quartz tube by using hydrofluoric acid, completely cleaning silicon dioxide powder on the surface of the quartz tube, then cleaning the quartz tube when soaking the quartz tube by using the distilled water, completely cleaning the inner surface and the outer surface of the quartz tube, and completely rotating and drying the quartz tube after completely cleaning;
step 2: basic operation of the quartz tube: putting the quartz tube into a helium protective environment, loading arsenic particles into the quartz tube, vacuumizing the quartz tube by using a vacuum machine, and then sealing the quartz tube;
and step 3: primary processing of arsenic particles: placing the quartz tube loaded with the arsenic particles in a sealed high-temperature high-pressure furnace, raising the temperature in the furnace to 750 ℃, primarily sublimating the arsenic particles, then keeping the temperature for 5 minutes, stopping the furnace, when the temperature is reduced by 220 ℃, starting the high-temperature high-pressure furnace again, raising the temperature to 750 ℃ again, keeping the temperature for 30 minutes, and completely removing oxide films in the arsenic particles;
and 4, step 4: high-order processing of arsenic particles: adding sufficient helium into the high-temperature high-pressure furnace, fully heating the quartz tube when the high-temperature high-pressure furnace is filled with high-pressure inert gas, basically melting arsenic particles when the temperature is heated to 850 ℃, suspending heating, and automatically cooling the quartz tube;
and 5: secondary melting of arsenic particles: observing the state of arsenic particles in the high-temperature and high-pressure furnace through the isolation window, starting heating operation for the second time when the temperature is reduced to 650 ℃, increasing the temperature of the high-temperature and high-pressure furnace to 920 ℃ for the second time, completely melting the arsenic particles, and then continuously preserving the heat for 20 minutes;
step 6: basic shaping of arsenic particles: stopping heating, automatically cooling the molten arsenic particles in the quartz tube, and then when the temperature is reduced to room temperature, remolding the arsenic particles into a rod shape to be loaded in a sealing way.
And those not described in detail in this specification are well within the skill of those in the art.
Comparative experiment
According to claim 1, the existing manufacturer can produce three arsenic rods, after the three arsenic rods are cleaned, the three arsenic rods are compared with the common arsenic rods in terms of storage life and manufacturing time, as shown in table 1, through laboratory tests, the shortest storage life is 1.8 years, the storage life is 0.2 years longer than that of the comparative example, the longest manufacturing time in the example is 5.3 years, and the storage life is 1.5 years shorter than that of the comparative example.
Table 1: comparative example comparison table of service life and production time
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (8)
1. A method for manufacturing an arsenic rod for molecular beam epitaxy is characterized by comprising the following steps: the method specifically comprises the following steps:
step 1: basic processing of the related devices: cleaning the inside and the outside of a quartz tube by using high-purity water, wiping the quartz tube to be dry after cleaning, quickly cleaning the quartz tube by using hydrofluoric acid, completely cleaning silicon dioxide powder on the surface of the quartz tube, then cleaning the quartz tube when soaking by using the high-purity water, and completely rotating and drying after completely cleaning the inner surface and the outer surface of the quartz tube;
step 2: basic operation of the quartz tube: putting the quartz tube into a helium protective environment, loading arsenic particles into the quartz tube, vacuumizing the quartz tube by using a vacuum machine, and then sealing the quartz tube;
and step 3: primary processing of arsenic particles: placing the quartz tube loaded with the arsenic particles in a sealed high-temperature high-pressure furnace, raising the temperature in the furnace to 700-;
and 4, step 4: high-order processing of arsenic particles: adding sufficient helium into the high-temperature high-pressure furnace, fully heating the quartz tube when the high-temperature high-pressure furnace is filled with high-pressure inert gas, basically melting the arsenic particles when the temperature is heated to 800-;
and 5: secondary melting of arsenic particles: observing the state of the arsenic particles in the high-temperature and high-pressure furnace through the isolation window, starting heating operation for the second time when the temperature is reduced to 600-650 ℃, increasing the temperature of the high-temperature and high-pressure furnace to 920 ℃, completely melting the arsenic particles, and then continuously preserving the heat for 20 minutes;
step 6: basic shaping of arsenic particles: stopping heating, automatically cooling the molten arsenic particles in the quartz tube, and then when the temperature is reduced to room temperature, remolding the arsenic particles into a rod shape to be loaded in a sealing way.
2. The method of claim 1, wherein the method comprises: in the step 1, the concentration of hydrofluoric acid is 4%.
3. The method of claim 1, wherein the method comprises: in the step 1, the inside of the quartz tube is dried synchronously.
4. The method of claim 1, wherein the method comprises: in step 2, a clamping device is required to load arsenic particles into the quartz tube.
5. The method of claim 1, wherein the method comprises: in the step 2, the vacuum is pumped to 10-2MPa。
6. The method of claim 1, wherein the method comprises: in the step 1, an infrared lamp drying box quartz tube is adopted for drying operation.
7. The method of claim 1, wherein the method comprises: in the step 3, an infrared thermometer is adopted to assist in measuring the temperature of the furnace cavity.
8. The method of claim 1, wherein the method comprises: and in the step 5, the high-temperature high-pressure furnace is completely sealed when working.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115418719A (en) * | 2022-08-22 | 2022-12-02 | 峨眉山嘉美高纯材料有限公司 | Preparation method of low-oxygen compact ultra-high-purity arsenic rod |
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| DE1806647A1 (en) * | 1967-11-10 | 1969-06-26 | Boliden Ab | Process and device for the production of crystalline, metallic arsenic |
| CN102899712A (en) * | 2012-08-30 | 2013-01-30 | 东方电气集团峨嵋半导体材料有限公司 | Preparation method of ultra-high-purity arsenic monocrystal pieces |
| CN106222452A (en) * | 2016-07-26 | 2016-12-14 | 成都锦沪新材料有限公司 | A kind of preparation method of bar-shaped arsenic |
| CN111455460A (en) * | 2020-04-13 | 2020-07-28 | 中南大学 | Preparation method of metal arsenic single crystal |
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2020
- 2020-09-03 CN CN202010915130.3A patent/CN112030224A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE1806647A1 (en) * | 1967-11-10 | 1969-06-26 | Boliden Ab | Process and device for the production of crystalline, metallic arsenic |
| CN102899712A (en) * | 2012-08-30 | 2013-01-30 | 东方电气集团峨嵋半导体材料有限公司 | Preparation method of ultra-high-purity arsenic monocrystal pieces |
| CN106222452A (en) * | 2016-07-26 | 2016-12-14 | 成都锦沪新材料有限公司 | A kind of preparation method of bar-shaped arsenic |
| CN111455460A (en) * | 2020-04-13 | 2020-07-28 | 中南大学 | Preparation method of metal arsenic single crystal |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115418719A (en) * | 2022-08-22 | 2022-12-02 | 峨眉山嘉美高纯材料有限公司 | Preparation method of low-oxygen compact ultra-high-purity arsenic rod |
| CN115418719B (en) * | 2022-08-22 | 2023-08-29 | 峨眉山嘉美高纯材料有限公司 | Preparation method of low-oxygen compact ultra-high purity arsenic rod |
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