CN105537207B - A kind of cleaning method of high temperature quartz ampoule - Google Patents
A kind of cleaning method of high temperature quartz ampoule Download PDFInfo
- Publication number
- CN105537207B CN105537207B CN201510922980.5A CN201510922980A CN105537207B CN 105537207 B CN105537207 B CN 105537207B CN 201510922980 A CN201510922980 A CN 201510922980A CN 105537207 B CN105537207 B CN 105537207B
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- CN
- China
- Prior art keywords
- quartz ampoule
- metal fluoride
- heating
- wall
- high temperature
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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
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Chemical Vapour Deposition (AREA)
Abstract
The present invention provides a kind of cleaning method of high temperature quartz ampoule, and the method is to clean quartzy tube wall using the fluorine gas that metal fluoride powder pyrolytic generates.Metal fluoride pyrolytic goes out fluorine gas, it is allowed to take away the residue on quartzy inside pipe wall using the activity of fluorine gas, volatilization is combined into gas in the residue of inner wall and is taken away by vacuum system after being used for a long time with quartz ampoule, meanwhile, and its etch quartz pipe can be prevented under drying, vacuum condition.It cleans the quartzy inside pipe wall finished and restores clear, and surface does not have any abrasion.
Description
Technical field
The present invention relates to a kind of methods, specifically disclose a kind of cleaning method of high temperature quartz ampoule.
Background technology
Quartz ampoule is 2000 DEG C reachable in use, such as light heating suspension zone melting furnace, sample volatile matter and silica tube wall
It is tightly combined, cannot be removed effectively residue using conventional method such as wiping, ultrasonic oscillation, organic matter solvent.
The acid solutions such as hydrofluoric acid can corrode quartz ampoule, react：
4HF+SiO2=SiF4(gas)+2H2O
If there is water exists,
2F2+2H2O=4HF+O2(gas)
4HF+SiO2=SiF4(gas)+2H2O
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 the corrosion of quartz ampoule,
It influences light to penetrate, this is for being all fatal using focusing light heating and monitoring the melting that sample melts situation in pipe in real time
It influences.Before finding suitable cleaning method, quartzy tube body is had to replace frequently, generates higher economic cost.
High-purity fluorine gas (F2) be a kind of gas that property is very active, have strong oxidizing property, can with most of inorganic matters or
Organic matter reacts at or below room temperature, and high-purity fluorine gas is the important source material of field of fine chemical.Be widely used in electronics,
The fields such as laser technology, medical plastics.Due to its strong oxidizing property, can be used for glass etch, metal material, pipeline surface
Passivation Treatment.
Invention content
It is an object of the invention to overcome the deficiencies of existing technologies, provide it is a kind of it is convenient, thorough high temperature quartz ampoule is clear
Washing method.
In order to realize object above and other purposes, the present invention including following technical scheme by realizing：
A kind of cleaning method of high temperature quartz ampoule, the method are generated using metal fluoride powder pyrolytic
The quartzy tube wall of fluorine gas cleaning.
It is highly preferred that the metal fluoride is one or more in rare earth metal fluoride.
Preferably, the metal fluoride is one or more in neodymium fluoride or dysprosium fluoride.
Preferably, metal fluoride is put into the quartz ampoule, and be put into togerther in vitreosil tube furnace, to vacuum
Heating is reacted after quartz tube type stove evacuation.
Preferably, the temperature that is heated to reaches 880~900 DEG C.
Preferably, the heating rate of the heating of the vitreosil tube furnace is 5~15 °/min.
It is highly preferred that the heating rate of the heating of the vitreosil tube furnace is 10 DEG C/min.
Preferably, after vacuumizing, the vacuum degree in the vitreosil tube furnace will remain less than 10-2Pa。
Preferably, the reaction time is 3~7 hours.
It is highly preferred that the reaction time is 5 hours.
Preferably, the usage amount of each quartz ampoule metal fluoride is 2~10g.
It is highly preferred that the usage amount of each quartz ampoule metal fluoride is 5g.
Preferably, stop outwelling residue after being heated to quartz ampoule natural cooling after reaction, inner wall is wiped with alcohol swab.
The invention also discloses purposes of the method as described above in terms of cleaning quartz ampoule.
Method has the advantages that in the present invention：
Common fluoride such as magnesium fluoride MgF2There is severe toxicity, it is just operable that necessary protective articles need to be dressed；Aluminum fluoride AlF3
Heat-flash is not decomposed but is distilled, and property is highly stable；Calcirm-fluoride CaF2It can shine when heated.Therefore using more stable in the present invention
Rare earth fluoride, neodymium fluoride and dysprosium fluoride etc. are not soluble in water, are also insoluble in hydrochloric acid, nitric acid and sulfuric acid.Room temperature shady and cool ventilation is dry
The dry closed preservation in place.
Metal fluoride pyrolytic goes out fluorine gas, is allowed to take away the residual on quartzy inside pipe wall using the activity of fluorine gas
Volatilization is combined into gas in the residue of inner wall and is taken away by vacuum system after object, with quartz ampoule long-time service, meanwhile, and can be dry
Its etch quartz pipe is prevented under dry, vacuum condition.It cleans the quartzy inside pipe wall finished and restores clear, and surface does not have any mill
Damage.
Description of the drawings
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 are before cleaning, and Fig. 2 b are clear
After washing.
Specific implementation mode
With reference to embodiment, the present invention is further explained.It should be understood that embodiment is merely to illustrate the present invention, and it is unrestricted
The scope of the present invention.
Embodiment 1
Cleaning method comprises the following steps in the present embodiment：
1,5 grams of metal fluoride fluorinating neodymiums are packed into quartz ampoule to be cleaned, and quartz ampoule level is put into vitreosil pipe
Formula stove；
2, temperature program is set, heating rate is 10 DEG C/min, and the heating-up time is arranged according to room temperature, temperature is made to reach 880
DEG C, soaking time is after 5 hours, furnace cooling.
3, it opens mechanical pump and is evacuated to 10Pa hereinafter, preheating diffusion pump, opens diffusion pump and be evacuated to 10-2After Pa,
Heating schedule is opened, stops vacuumizing.
4, observation vacuum meter is paid attention in insulating process, mechanical pump is opened when vacuum degree is more than 20Pa 5 minutes, by vacuum degree
It is down to 10-1Then Pa stops vacuumizing.Repeatedly, keep overpressure should not be excessively high in heating process.
5, quartz ampoule is taken out after cooling, outwells the residue after reaction, inner wall is wiped with alcohol swab.
Embodiment 2
Cleaning method comprises the following steps in the present embodiment：
1,5 grams of metal fluoride fluorinating dysprosiums are packed into quartz ampoule to be cleaned, and quartz ampoule level is put into vitreosil pipe
Formula stove；
2, temperature program is set, heating rate is 10 DEG C/min, and the heating-up time is arranged according to room temperature, temperature is made to reach 900
DEG C, soaking time is after 5 hours, furnace cooling.
3, it opens mechanical pump and is evacuated to 10Pa hereinafter, preheating diffusion pump, opens diffusion pump and be evacuated to 10-2After Pa,
Heating schedule is opened, stops vacuumizing.
4, observation vacuum meter is paid attention in insulating process, mechanical pump is opened when vacuum degree is more than 20Pa 5 minutes, by vacuum degree
It is down to 10-1Then Pa stops vacuumizing.Repeatedly, keep overpressure should not be excessively high in heating process.
5, quartz ampoule is taken out after cooling, outwells the residue after reaction, inner wall is wiped with alcohol swab.
Embodiment 3
Cleaning method comprises the following steps in the present embodiment：
1,2 grams of metal fluoride fluorinating dysprosiums are packed into quartz ampoule to be cleaned, and quartz ampoule level is put into vitreosil pipe
Formula stove；
2, temperature program is set, heating rate is 5 DEG C/min, and the heating-up time is arranged according to room temperature, temperature is made to reach 890
DEG C, soaking time is after 3 hours, furnace cooling.
3, it opens mechanical pump and is evacuated to 10Pa hereinafter, preheating diffusion pump, opens diffusion pump and be evacuated to 10-2After Pa,
Heating schedule is opened, stops vacuumizing.
4, observation vacuum meter is paid attention in insulating process, mechanical pump is opened when vacuum degree is more than 20Pa 10 minutes, by vacuum
Degree is down to 10-1Then Pa stops vacuumizing.Repeatedly, keep overpressure should not be excessively high in heating process.
5, quartz ampoule is taken out after cooling, outwells the residue after reaction, inner wall is wiped with alcohol swab.
Embodiment 4
Cleaning method comprises the following steps in the present embodiment：
1,2 grams of metal fluoride fluorinating neodymiums are packed into quartz ampoule to be cleaned, and quartz ampoule level is put into vitreosil pipe
Formula stove；
2, temperature program is set, heating rate is 15 DEG C/min, and the heating-up time is arranged according to room temperature, temperature is made to reach 890
DEG C, soaking time is after 7 hours, furnace cooling.
3, it opens mechanical pump and is evacuated to 10Pa hereinafter, preheating diffusion pump, opens diffusion pump and be evacuated to 10-2After Pa,
Heating schedule is opened, stops vacuumizing.
4, observation vacuum meter is paid attention in insulating process, mechanical pump is opened when vacuum degree is more than 20Pa 10 minutes, by vacuum
Degree is down to 10-1Then Pa stops vacuumizing.Repeatedly, keep overpressure should not be excessively high in heating process.
5, quartz ampoule is taken out after cooling, outwells the residue after reaction, inner wall is wiped with alcohol swab.
The above, only presently preferred embodiments of the present invention, not to the present invention in any form with substantial limitation,
It should be pointed out that for those skilled in the art, under the premise of not departing from the method for the present invention, can also make
Several improvement and supplement, these are improved and supplement also should be regarded as protection scope of the present invention.All those skilled in the art,
Without departing from the spirit and scope of the present invention, when made using disclosed above technology contents it is a little more
Dynamic, modification and the equivalent variations developed, are the equivalent embodiment of the present invention；Meanwhile all substantial technologicals pair according to the present invention
The variation, modification and evolution of any equivalent variations made by above-described embodiment, still fall within the range of technical scheme of the present invention
It is interior.
Claims (6)
1. a kind of cleaning method of high temperature quartz ampoule, the method is the fluorine generated using metal fluoride powder pyrolytic
The quartzy tube wall of gas cleaning；
The metal fluoride is one or more in rare earth metal fluoride；
Metal fluoride is put into the quartz ampoule, and is put into togerther in vitreosil tube furnace, to vitreosil tube furnace
Heating is reacted after vacuumizing；
The temperature that is heated to reaches 880~900 DEG C.
2. method as described in claim 1, it is characterised in that：The heating rate of the heating of the vitreosil tube furnace be 5~
15℃/min。
3. method as described in claim 1, it is characterised in that：After vacuumizing, the vacuum degree in the vitreosil tube furnace is wanted
Remain less than 10-2Pa。
4. method as described in claim 1, it is characterised in that：Reaction time is 3~7 hours.
5. method as described in claim 1, it is characterised in that：The usage amount of each quartz ampoule metal fluoride is 2~10g.
6. method as described in claim 1, it is characterised in that：Stop outwelling after being heated to quartz ampoule natural cooling after reaction
Residue wipes inner wall with alcohol swab.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201510922980.5A CN105537207B (en) | 2015-12-11 | 2015-12-11 | A kind of cleaning method of high temperature quartz ampoule |
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| CN201510922980.5A CN105537207B (en) | 2015-12-11 | 2015-12-11 | A kind of cleaning method of high temperature quartz ampoule |
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| CN105537207A CN105537207A (en) | 2016-05-04 |
| CN105537207B true CN105537207B (en) | 2018-09-25 |
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| 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 |
| CN114956605B (en) * | 2022-06-28 | 2023-12-29 | 安徽光智科技有限公司 | Method for recycling quartz tube |
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| 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 |
| JP2003178986A (en) * | 2001-12-13 | 2003-06-27 | Showa Denko Kk | Cleaning gas and cleaning method of semiconductor manufacturing apparatus |
| CN101327487B (en) * | 2007-06-21 | 2010-12-22 | 中芯国际集成电路制造(上海)有限公司 | Method and system for cleaning boiler tube |
| JP4918453B2 (en) * | 2007-10-11 | 2012-04-18 | 東京エレクトロン株式会社 | Gas supply apparatus and thin film forming apparatus |
| CN201305466Y (en) * | 2008-10-23 | 2009-09-09 | 俞月明 | Heating device for preparing nanometer silicon powders |
| CA2690697A1 (en) * | 2009-01-27 | 2010-07-27 | Air Products And Chemicals, Inc. | Selective etching and formation of xenon difluoride |
| CN102755969B (en) * | 2011-04-28 | 2014-12-10 | 中芯国际集成电路制造(上海)有限公司 | Method for improving surface cleaning ability of reaction unit |
| CN102825036B (en) * | 2012-08-23 | 2014-12-24 | 英利能源（中国）有限公司 | Cleaning method for furnace tube for diffusion |
| 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 |
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Granted publication date: 20180925 Termination date: 20201211 |