CN105537207A - Cleaning method of quartz tube for high temperature - Google Patents
Cleaning method of quartz tube for high temperature Download PDFInfo
- Publication number
- CN105537207A CN105537207A CN201510922980.5A CN201510922980A CN105537207A CN 105537207 A CN105537207 A CN 105537207A CN 201510922980 A CN201510922980 A CN 201510922980A CN 105537207 A CN105537207 A CN 105537207A
- Authority
- CN
- China
- Prior art keywords
- quartz ampoule
- metal fluoride
- quartz tube
- tube furnace
- fluorine gas
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B9/00—Cleaning hollow articles by methods or apparatus specially adapted thereto
- B08B9/02—Cleaning pipes or tubes or systems of pipes or tubes
- B08B9/027—Cleaning the internal surfaces; Removal of blockages
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B2209/00—Details of machines or methods for cleaning hollow articles
- B08B2209/02—Details of apparatuses or methods for cleaning pipes or tubes
- B08B2209/027—Details of apparatuses or methods for cleaning pipes or tubes for cleaning the internal surfaces
Abstract
The invention provides a cleaning method of a quartz tube for high temperature. The method includes the step of cleaning the tube wall of the quartz tube with fluorine gas generated through pyrogenic decomposition of metal fluoride powder, specifically, the metal fluoride powder is decomposed at high temperature to generate the fluorine gas, and residues on the inner wall of the quartz tube are taken away due to activity of the fluorine gas. The fluorine gas and the residues, generated through volatilization after the quartz tube is used for a long time, on the inner wall are combined into gas to be exhausted by a vacuum system, meanwhile, the fluorine gas is prevented from corroding the quartz tube on the dry and vacuum conditions. The inner wall of the cleaned quartz tube recovers to be clear, and no wear trace occurs to the surface.
Description
Technical field
The present invention relates to a kind of method, specifically disclose a kind of cleaning method of high temperature quartz ampoule.
Background technology
When quartz ampoule uses, such as light heated suspension zone melting furnace, can reach 2000 DEG C, and sample volatile matter is combined closely with silica tube wall, uses conventional method such as wiping, ultrasonic oscillation, organic matter solvent effectively can not remove residue.
The acid solutions such as hydrofluoric acid can be corroded quartz ampoule, react:
4HF+SiO
2=SiF
4(gas)+2H
2o
If there is water to exist,
2F
2+ 2H
2o=4HF+O
2(gas)
4HF+SiO
2=SiF
4(gas)+2H
2o
And the acid solutions such as hydrofluoric acid can occur as above to react with quartz ampoule, tube surfaces can be made to become hair, affect light therethrough to the corrosion of quartz ampoule, this is all fatal impact for the melting utilizing focused ray to heat and in real-time monitoring pipe, sample melts situation.Before finding suitable cleaning method, quartzy body is had to change frequently, produces higher financial cost.
High-purity fluorine gas (F
2) be the very active gas of a kind of character, have strong oxidizing property, can react at or below room temperature with most of inorganic matter or organic matter, high-purity fluorine gas is the important source material of field of fine chemical.Be widely used in the fields such as electronics, laser technology, medical plastics.Due to its strong oxidizing property, may be used for glass etch, the surface passivating treatment of metal material, pipeline.
Summary of the invention
The object of the invention is to the defect overcoming prior art, a kind of convenient, high temperature quartz ampoule cleaning method is thoroughly provided.
In order to realize above object and other objects, the present invention realizes by comprising following technical scheme:
A cleaning method for high temperature quartz ampoule, described method is that the fluorine gas using metal fluoride powder pyrolytic to produce cleans quartz ampoule tube wall.
More preferably, described metal fluoride is one or more in rare earth metal fluoride.
Preferably, described metal fluoride is one or more in neodymium fluoride or dysprosium fluoride.
Preferably, metal fluoride is put into described quartz ampoule, and put into vitreosil tube furnace together, rear heating is vacuumized to vitreosil tube furnace and reacts.
Preferably, be heated to temperature described in and reach 880 ~ 900 DEG C.
Preferably, the programming rate of the heating of described vitreosil tube furnace is 5 ~ 15 °/min.
More preferably, the programming rate of the heating of described vitreosil tube furnace is 10 DEG C/min.
Preferably, after vacuumizing, the vacuum in described vitreosil tube furnace will keep being less than 10
-2pa.
Preferably, the reaction time is 3 ~ 7 hours.
More preferably, the reaction time is 5 hours.
Preferably, the use amount of each quartz ampoule metal fluoride is 2 ~ 10g.
More preferably, the use amount of each quartz ampoule metal fluoride is 5g.
Preferably, reaction terminates rear stopping and being heated to outwell residue after quartz ampoule cools naturally, with alcohol swab wiping inwall.
The invention also discloses the purposes of method as described above in cleaning quartz ampoule.
In the present invention, method has following beneficial effect:
Common fluoride is as magnesium fluoride MgF
2there is severe toxicity, necessary protective articles need be dressed and just can operate; Aluminum fluoride AlF
3heat-flash does not decompose but distils, and character is highly stable; Calcirm-fluoride CaF
2can be luminous when being heated.Therefore use more stable rare earth fluoride in the present invention, neodymium fluoride and dysprosium fluoride etc. are water insoluble, are also insoluble to hydrochloric acid, nitric acid and sulfuric acid.Normal temperature shady and cool ventilation drying place is airtight to preserve.
Metal fluoride pyrolytic goes out fluorine gas, the activity of fluorine gas is utilized to make it to take away the residue on quartz ampoule inwall, be combined into gas at the residue of inwall and taken away by vacuum system with volatilizing after quartz ampoule Long-Time Service, meanwhile, its etch quartz pipe can be prevented under dry, vacuum condition again.Clean complete quartz ampoule inwall and recover thoroughly clear, and surface is without any wearing and tearing.
Accompanying drawing explanation
Fig. 1 is the temperature curve schematic diagram of cleaning process in the embodiment of the present invention 1.
Fig. 2 is the cleaning performance cross-reference figure of quartz ampoule in the embodiment of the present invention 1; Fig. 2 a is for before cleaning, and Fig. 2 b is for after cleaning.
Detailed description of the invention
The present invention is set forth further below in conjunction with embodiment.Should be understood that embodiment only for illustration of the present invention, but not limit the scope of the invention.
Embodiment 1
In the present embodiment, cleaning method comprises following steps:
1,5 grams of metal fluoride fluorinating neodymiums are loaded quartz ampoule to be cleaned, and quartz ampoule level is put into vitreosil tube furnace;
2, arrange heating schedule, programming rate is 10 DEG C/min, arranges the heating-up time according to room temperature, makes temperature reach 880 DEG C, and temperature retention time, after 5 hours, cools with stove.
3, open mechanical pump and be evacuated to below 10Pa, preheating diffusion pump, open diffusion pump and be evacuated to 10
-2after Pa, open heating schedule, stop vacuumizing.
4, note in insulating process observing vacuum meter, open mechanical pump 5 minutes when vacuum is greater than 20Pa, vacuum is down to 10
-1pa, then stops vacuumizing.So repeatedly, keep overpressure not too high in heating process.
5, cooling after take out quartz ampoule, outwell reacted after residue, with alcohol swab wiping inwall.
Embodiment 2
In the present embodiment, cleaning method comprises following steps:
1,5 grams of metal fluoride fluorinating dysprosiums are loaded quartz ampoule to be cleaned, and quartz ampoule level is put into vitreosil tube furnace;
2, arrange heating schedule, programming rate is 10 DEG C/min, arranges the heating-up time according to room temperature, makes temperature reach 900 DEG C, and temperature retention time, after 5 hours, cools with stove.
3, open mechanical pump and be evacuated to below 10Pa, preheating diffusion pump, open diffusion pump and be evacuated to 10
-2after Pa, open heating schedule, stop vacuumizing.
4, note in insulating process observing vacuum meter, open mechanical pump 5 minutes when vacuum is greater than 20Pa, vacuum is down to 10
-1pa, then stops vacuumizing.So repeatedly, keep overpressure not too high in heating process.
5, cooling after take out quartz ampoule, outwell reacted after residue, with alcohol swab wiping inwall.
Embodiment 3
In the present embodiment, cleaning method comprises following steps:
1,2 grams of metal fluoride fluorinating dysprosiums are loaded quartz ampoule to be cleaned, and quartz ampoule level is put into vitreosil tube furnace;
2, arrange heating schedule, programming rate is 5 DEG C/min, arranges the heating-up time according to room temperature, makes temperature reach 890 DEG C, and temperature retention time, after 3 hours, cools with stove.
3, open mechanical pump and be evacuated to below 10Pa, preheating diffusion pump, open diffusion pump and be evacuated to 10
-2after Pa, open heating schedule, stop vacuumizing.
4, note in insulating process observing vacuum meter, open mechanical pump 10 minutes when vacuum is greater than 20Pa, vacuum is down to 10
-1pa, then stops vacuumizing.So repeatedly, keep overpressure not too high in heating process.
5, cooling after take out quartz ampoule, outwell reacted after residue, with alcohol swab wiping inwall.
Embodiment 4
In the present embodiment, cleaning method comprises following steps:
1,2 grams of metal fluoride fluorinating neodymiums are loaded quartz ampoule to be cleaned, and quartz ampoule level is put into vitreosil tube furnace;
2, arrange heating schedule, programming rate is 15 DEG C/min, arranges the heating-up time according to room temperature, makes temperature reach 890 DEG C, and temperature retention time, after 7 hours, cools with stove.
3, open mechanical pump and be evacuated to below 10Pa, preheating diffusion pump, open diffusion pump and be evacuated to 10
-2after Pa, open heating schedule, stop vacuumizing.
4, note in insulating process observing vacuum meter, open mechanical pump 10 minutes when vacuum is greater than 20Pa, vacuum is down to 10
-1pa, then stops vacuumizing.So repeatedly, keep overpressure not too high in heating process.
5, cooling after take out quartz ampoule, outwell reacted after residue, with alcohol swab wiping inwall.
The above; be only preferred embodiment of the present invention; not to any formal and substantial restriction of the present invention; should be understood that; for those skilled in the art; under the prerequisite not departing from the inventive method, also can make some improvement and supplement, these improve and supplement and also should be considered as protection scope of the present invention.All those skilled in the art, without departing from the spirit and scope of the present invention, a little change made when utilizing disclosed above technology contents, the equivalent variations of modifying and developing, be Equivalent embodiments of the present invention; Meanwhile, all according to substantial technological of the present invention to the change of any equivalent variations that above-described embodiment is done, modify and differentiation, all still belong in the scope of technical scheme of the present invention.
Claims (10)
1. a cleaning method for high temperature quartz ampoule, described method is that the fluorine gas using metal fluoride powder pyrolytic to produce cleans quartz ampoule tube wall.
2. method as claimed in claim 1, is characterized in that: described metal fluoride is one or more in rare earth metal fluoride.
3. method as claimed in claim 1, is characterized in that: metal fluoride is put into described quartz ampoule, and puts into vitreosil tube furnace together, vacuumize rear heating react vitreosil tube furnace.
4. method as claimed in claim 3, is characterized in that: described in be heated to temperature and reach 880 ~ 900 DEG C.
5. method as claimed in claim 3, is characterized in that: the programming rate of the heating of described vitreosil tube furnace is 5 ~ 15 DEG C/min.
6. method as claimed in claim 3, it is characterized in that: after vacuumizing, the vacuum in described vitreosil tube furnace will keep being less than 10
-2pa.
7. method as claimed in claim 3, is characterized in that: the reaction time is 3 ~ 7 hours.
8. method as claimed in claim 1, is characterized in that: the use amount of each quartz ampoule metal fluoride is 2 ~ 10g.
9. method as claimed in claim 3, is characterized in that: reaction terminates rear stopping and being heated to outwell residue after quartz ampoule cools naturally, with alcohol swab wiping inwall.
10. the purposes of method as described in as arbitrary in claim 1 ~ 9 in cleaning quartz ampoule.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510922980.5A CN105537207B (en) | 2015-12-11 | 2015-12-11 | A kind of cleaning method of high temperature quartz ampoule |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510922980.5A CN105537207B (en) | 2015-12-11 | 2015-12-11 | A kind of cleaning method of high temperature quartz ampoule |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105537207A true CN105537207A (en) | 2016-05-04 |
| CN105537207B CN105537207B (en) | 2018-09-25 |
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|---|---|---|---|
| CN201510922980.5A Expired - Fee Related CN105537207B (en) | 2015-12-11 | 2015-12-11 | A kind of cleaning method of high temperature quartz ampoule |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112871891A (en) * | 2021-01-13 | 2021-06-01 | 哈尔滨科友半导体产业装备与技术研究院有限公司 | Method for cleaning quartz tube of silicon carbide crystal growth furnace |
| CN114956605A (en) * | 2022-06-28 | 2022-08-30 | 安徽光智科技有限公司 | Recycling method of quartz tube |
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| CN105502410A (en) * | 2015-12-23 | 2016-04-20 | 中国船舶重工集团公司第七一八研究所 | Preparation and purification methods of silicon tetrafluoride |
-
2015
- 2015-12-11 CN CN201510922980.5A patent/CN105537207B/en not_active Expired - Fee Related
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1565710A (en) * | 1998-12-15 | 2005-01-19 | 高级技术材料公司 | Apparatus and method for point-of-use treatment of effluent gas streams |
| CN1592798A (en) * | 2001-12-13 | 2005-03-09 | 昭和电工株式会社 | Cleaning gas for semiconductor production equipment and cleaning method using the gas |
| CN101327487A (en) * | 2007-06-21 | 2008-12-24 | 中芯国际集成电路制造(上海)有限公司 | Method and system for cleaning boiler tube |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112871891A (en) * | 2021-01-13 | 2021-06-01 | 哈尔滨科友半导体产业装备与技术研究院有限公司 | Method for cleaning quartz tube of silicon carbide crystal growth furnace |
| CN114956605A (en) * | 2022-06-28 | 2022-08-30 | 安徽光智科技有限公司 | Recycling method of quartz tube |
| CN114956605B (en) * | 2022-06-28 | 2023-12-29 | 安徽光智科技有限公司 | Method for recycling quartz tube |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105537207B (en) | 2018-09-25 |
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