CN1119300C - Process for preparing low-hydroxyl quartz tube - Google Patents

Process for preparing low-hydroxyl quartz tube Download PDF

Info

Publication number
CN1119300C
CN1119300C CN00112310A CN00112310A CN1119300C CN 1119300 C CN1119300 C CN 1119300C CN 00112310 A CN00112310 A CN 00112310A CN 00112310 A CN00112310 A CN 00112310A CN 1119300 C CN1119300 C CN 1119300C
Authority
CN
China
Prior art keywords
quartz tube
hydroxyl
temperature
production method
heating chamber
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.)
Expired - Fee Related
Application number
CN00112310A
Other languages
Chinese (zh)
Other versions
CN1273948A (en
Inventor
李长虹
张庆观
尹保文
何书臣
王海英
朱文飞
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
DONGHAI QUARTZ PRODUCTS GENERAL FACTORY JIANGSU PROV
Original Assignee
DONGHAI QUARTZ PRODUCTS GENERAL FACTORY JIANGSU PROV
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by DONGHAI QUARTZ PRODUCTS GENERAL FACTORY JIANGSU PROV filed Critical DONGHAI QUARTZ PRODUCTS GENERAL FACTORY JIANGSU PROV
Priority to CN00112310A priority Critical patent/CN1119300C/en
Publication of CN1273948A publication Critical patent/CN1273948A/en
Application granted granted Critical
Publication of CN1119300C publication Critical patent/CN1119300C/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

Links

Landscapes

  • Glass Melting And Manufacturing (AREA)
  • Silicon Compounds (AREA)

Abstract

The present invention relates to a production method for a low-hydroxyl quartz tube. A quartz tube which is already treated by drawing is placed in a closed heating chamber. The internal pressure of the closed heating chamber can reach 5*10<-1>-5*10<-4> pascals by pumping air to the outside, and the temperature is gradually raised to 950 to 1250 DEG C; the quartz tube is calcined for 3 to 20 hours at a constant temperature, and the internal air pressure is stabilized to 5*10<-1>-5*10<-4> pascals by continuously pumping air out. The quartz tube is cooled, normal pressure is recovered, and the quartz tube can be taken out after the chamber is opened. Due to the adoption of high temperature and high vacuum de-hydroxyl technology, large negative pressure is formed inside and outside the quartz glass tube; thus, hydroxyls in the deep layers among lattices of silicon dioxide are easier to escape, the de-hydroxyl operation is more thorough, and the content of hydroxyls in the quartz tube treated by the de-hydroxyl operation can be greatly reduced.

Description

A kind of production method of low-hydroxyl quartz tube
The present invention relates to a kind of production method of silica tube, particularly reduce the method for hydroxy radical content in the silica tube.
Have now in the manufacturing process of public low-hydroxyl quartz tube, the deshydroxy way that reduces hydroxy radical content in the silica tube is: will draw good silica tube and insert in the airtight heating chamber, carry out under nitrogen atmosphere 1000-1050 ℃ of following high-temperature roasting 3-5 hour.Hydroxyl in the silica tube is present between the silicon-dioxide lattice; comparatively stable under the normal temperature; can slowly discharge under the high temperature, overflow; but owing to pass to the malleation that nitrogen protection forms 111.46 pascals in the conventional deshydroxy process; the deep layer hydroxyl is overflowed comparatively difficult; so adopt this method can only slough the hydroxyl on surface and top layer, and silica tube deep layer and whole deshydroxy can not be thorough.As: to original impurity 30ppm, the silica tube of hydroxy radical content 130ppm, adopt this method deshydroxy after, hydroxy radical content still reaches 8-20ppm in the silica tube.In addition, if nitrogen gas purity also can cause new pollution to silica tube inadequately.
The purpose of invention is to overcome above-mentioned the deficiencies in the prior art part exactly, and a kind of production method of utilizing the low-hydroxyl quartz tube of the hydroxy radical content in the negative pressure drop low quartz pipe is provided.
Purpose of the present invention and task can be finished by implementing following technical proposal: a kind of production method of low-hydroxyl quartz tube, good silica tube will be drawn, insert in the airtight heating chamber, carry out high-temperature roasting, be characterized in: before high-temperature roasting, make airtight heating chamber internal pressure reach 5 * 10 by outside pump drainage air earlier -1-5 * 10 -4Pascal rises to 950-1250 ℃ gradually with temperature then, keeps constant temperature calcining 3-20 hour, and the pump drainage air makes airtight heating chamber internal gas pressure be stabilized in 5 * 10 continuously simultaneously -1-5 * 10 -4Pascal after high-temperature roasting, through cooling, recovers normal pressure, and the chamber of opening goes out pipe.Significantly reduce the technique effect of the hydroxy radical content in the silica tube with negative pressure with the Dary.
Purpose of the present invention can also further reach by following scheme.The production method of aforesaid low-hydroxyl quartz tube is characterized in that in the process of high-temperature roasting, the pressure-stabilisation that makes heating chamber is 3 * 10 -3Near the pascal.To obtain best effect, value at cost.
Purpose of the present invention can also further reach by following scheme.The production method of aforesaid low-hydroxyl quartz tube is characterized in that temperature remains on 1000-1200 ℃ in above-mentioned roasting process, and keeps constant temperature 5-8 hour.To obtain best effect, value at cost.
Purpose of the present invention can also further reach by following scheme.The production method of aforesaid low-hydroxyl quartz tube is characterized in before blow-on goes out pipe, feeds the protection of high pure nitrogen or argon gas or helium.To prevent atmospheric pollution.
The present invention compared with prior art, owing to adopted high temperature, high vacuum deshydroxy technology, formed very big negative pressure inside and outside the quartz glass tube, the feasible hydroxyl that was present in the deep layer between quartz glass tube silicon-dioxide lattice originally, easier effusion, the quartz glass tube deshydroxy is more thorough, behind the deshydroxy in the silica tube hydroxy radical content reduce significantly.As: original impurity 30ppm, the silica tube of hydroxy radical content 130ppm, behind method deshydroxy of the present invention, its hydroxy radical content is no more than 3ppm, and hydroxy radical content is well below original technology.
Embodiment one.The following examples have further described summary of the invention of the present invention.The production method of the low-hydroxyl quartz tube of present embodiment is with original impurity 30ppm, and the silica tube of hydroxy radical content 130ppm places in the airtight process furnace, opens vacuum system, treats that vacuum tightness reaches 3 * 10 in the stove -3Behind the pascal, progressively temperature in the stove is increased to 1200 ℃, the pump drainage air makes the interior vacustat of stove 3 * 10 continuously -3Pascal.Keep constant temperature calcining progressively cooling after 6 hours, lead to into an amount of high-pure helium gas shiled at last before blow-on, prevent atmospheric pollution, recover normal pressure, blow-on goes out pipe.Its silica tube product hydroxy radical content is reduced to 2.5ppm after testing, has reduced 8ppm than the same raw produce of original technology.
Embodiment two.The following examples continue to describe summary of the invention of the present invention, and the production method of the low-hydroxyl quartz tube of present embodiment is with original impurity 30ppm, and the silica tube of hydroxy radical content 130ppm places in the airtight process furnace, open vacuum system, treat that furnace pressure reaches 5 * 10 -1After pascal's vacuum tightness, progressively temperature in the stove is increased to 1000 ℃, the pump drainage air makes the interior vacustat of stove 5 * 10 continuously -1Pascal.Keep constant temperature calcining progressively cooling after 20 hours, recover normal pressure, blow-on goes out pipe.Its silica tube product hydroxy radical content is reduced to below the 3ppm after testing, has reduced 7.5ppm than the same raw produce of original technology.
Embodiment three.The following examples continue to describe summary of the invention of the present invention.The production method of the low-hydroxyl quartz tube of present embodiment is with original impurity 30ppm, and the silica tube of hydroxy radical content 130ppm places in the airtight process furnace, opens vacuum system, treats that vacuum tightness reaches 5 * 10 in the stove -4Behind the pascal, progressively temperature in the stove is increased to 1250 ℃, the pump drainage air makes the interior vacustat of stove 5 * 10 continuously -4Pascal.Keep constant temperature calcining progressively cooling after 3 hours, lead to into an amount of high-purity argon gas protection at last and prevent atmospheric pollution before blow-on, recover normal pressure, blow-on goes out pipe.Its silica tube product hydroxy radical content is reduced to 2.8ppm after testing, has reduced 7.7ppm than the same raw produce of original technology.
Embodiment four.The following examples continue to describe summary of the invention of the present invention.The production method of the low-hydroxyl quartz tube of present embodiment is with original impurity 30ppm, and the silica tube of hydroxy radical content 130ppm places in the airtight process furnace, opens vacuum system, treats that vacuum tightness reaches 3 * 10 in the stove -3Behind the pascal, progressively temperature in the stove is increased to 950 ℃, the pump drainage air makes the interior vacustat of stove 3 * 10 continuously -3Pascal.Keep constant temperature calcining progressively cooling after 8 hours, lead to into an amount of high pure nitrogen protection at last and prevent atmospheric pollution before blow-on, recover normal pressure, blow-on goes out pipe.Its silica tube product hydroxy radical content is reduced to 2.9ppm after testing, has reduced 7.6ppm than the same raw produce of original technology.

Claims (4)

1, a kind of production method of low-hydroxyl quartz tube with drawing good silica tube, is inserted in the airtight heating chamber, carries out high-temperature roasting, it is characterized in that: before high-temperature roasting, make airtight heating chamber internal pressure reach 5 * 10 by outside pump drainage air earlier -1-5 * 10 -4Pascal rises to 950-1250 ℃ gradually with temperature then, keeps constant temperature calcining 3-20 hour, and the pump drainage air makes airtight heating chamber internal gas pressure be stabilized in 5 * 10 continuously simultaneously -1-5 * 10 -4Pascal after high-temperature roasting, through cooling, recovers normal pressure, and the chamber of opening goes out pipe.
2, the production method of low-hydroxyl quartz tube according to claim 1 is characterized in that in the process of high-temperature roasting, the pressure-stabilisation that makes heating chamber is 3 * 10 -3Pascal.
3, the production method of low-hydroxyl quartz tube according to claim 1 is characterized in that temperature remains on 1000-1200 ℃ in above-mentioned roasting process, and keeps constant temperature 5-8 hour.
4, the production method of low-hydroxyl quartz tube according to claim 1 is characterized in that before blow-on goes out pipe, feeds the protection of high pure nitrogen or argon gas or helium.
CN00112310A 2000-05-25 2000-05-25 Process for preparing low-hydroxyl quartz tube Expired - Fee Related CN1119300C (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN00112310A CN1119300C (en) 2000-05-25 2000-05-25 Process for preparing low-hydroxyl quartz tube

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN00112310A CN1119300C (en) 2000-05-25 2000-05-25 Process for preparing low-hydroxyl quartz tube

Publications (2)

Publication Number Publication Date
CN1273948A CN1273948A (en) 2000-11-22
CN1119300C true CN1119300C (en) 2003-08-27

Family

ID=4582177

Family Applications (1)

Application Number Title Priority Date Filing Date
CN00112310A Expired - Fee Related CN1119300C (en) 2000-05-25 2000-05-25 Process for preparing low-hydroxyl quartz tube

Country Status (1)

Country Link
CN (1) CN1119300C (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105859112A (en) * 2016-03-30 2016-08-17 江苏圣达石英制品有限公司 Treating process for photosensitive quartz tube

Families Citing this family (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101323501B (en) 2007-01-02 2015-10-07 德雷卡通信技术公司 For the extended baking process of quartz glass deposition tubes
CN102311219A (en) * 2011-09-29 2012-01-11 连云港华源石英制品有限公司 Production method of low-hydroxylic bactericidal deodorant quartz tube
CN111087179B (en) * 2019-12-03 2021-09-21 连云港海源石英制品有限公司 Preparation method of colorless transparent low-hydroxyl ultraviolet-filtering quartz glass tube for car lamp
CN111362565A (en) * 2020-02-24 2020-07-03 东海县奥博石英制品有限公司 Large-diameter quartz tube expanding and shrinking method
CN115557677B (en) * 2022-10-21 2024-03-15 高晓云 Quartz tube manufacturing method and quartz tube
CN115872606B (en) * 2022-10-21 2024-05-14 高晓云 Method for melting quartz tube by utilizing electric arc and quartz tube electric arc melting equipment
CN117682753A (en) * 2023-03-31 2024-03-12 福耀高性能玻璃科技(福建)有限公司 Method and device for exhausting glass body, vacuum glass and manufacturing method thereof

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1122783A (en) * 1994-05-26 1996-05-22 赫罗伊斯石英玻璃有限公司 Method and apparatus for making quartz glass plate

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1122783A (en) * 1994-05-26 1996-05-22 赫罗伊斯石英玻璃有限公司 Method and apparatus for making quartz glass plate

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105859112A (en) * 2016-03-30 2016-08-17 江苏圣达石英制品有限公司 Treating process for photosensitive quartz tube
CN105859112B (en) * 2016-03-30 2018-10-23 江苏圣达石英制品有限公司 A kind for the treatment of process of photosensitive quartz ampoule

Also Published As

Publication number Publication date
CN1273948A (en) 2000-11-22

Similar Documents

Publication Publication Date Title
CN1119300C (en) Process for preparing low-hydroxyl quartz tube
US6826927B2 (en) Synthetic quartz powder, its production process, and synthetic quartz crucible
US7736613B2 (en) Modification process of synthetic silica powder and its quartz glass product
CN111320177A (en) Method for removing hydroxyl in quartz sand powder
CN113735110B (en) Purification method of semiconductor-grade graphite powder
CN112670374A (en) Low-voltage annealing method for crystalline silicon solar cell
CN112820642A (en) Heat treatment method of semiconductor silicon wafer
CN112340726A (en) Preparation method of high-purity graphite crucible
CN106449873A (en) Aluminium gettering method for ingot polycrystalline silicon chips
CN101774589A (en) Method for preparing low-hydroxyl and high-purity crystal powder
CN114232095B (en) Method for optimizing initial nucleation on surface of silicon carbide seed crystal
CN111087179B (en) Preparation method of colorless transparent low-hydroxyl ultraviolet-filtering quartz glass tube for car lamp
CN211125680U (en) Passivation coating film system
CN113999981A (en) Impurity removal method for high-purity metal through vacuum sublimation
CN108878289B (en) High-efficiency battery annealing process
CN113594267A (en) Method for forming oxide layer
CN111188085A (en) Method for preparing large-area Cu (100) single crystal copper foil
CN109427928B (en) Anaerobic annealing process for solar cell
CN113772669A (en) Method for removing residual fluorine gas in purified graphite material
CN117552017A (en) Cleaning method of iridium crucible for gallium oxide crystal growth
CN1962503A (en) Method for reducing hydroxyl content of quartz glass tube
CN114525586B (en) Growth method for preparing large-size high-purity semi-insulating silicon carbide single crystal
CN210150951U (en) Electric melting furnace for producing large-size high-purity quartz glass
CN115172514A (en) In-situ gas seal annealing method for improving quality of cadmium selenide film
CN200940169Y (en) Crystal pulling device

Legal Events

Date Code Title Description
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C06 Publication
PB01 Publication
C14 Grant of patent or utility model
GR01 Patent grant
C19 Lapse of patent right due to non-payment of the annual fee
CF01 Termination of patent right due to non-payment of annual fee