CN105502897B - The preparation method of super pure silica glass - Google Patents
The preparation method of super pure silica glass Download PDFInfo
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- CN105502897B CN105502897B CN201610019268.9A CN201610019268A CN105502897B CN 105502897 B CN105502897 B CN 105502897B CN 201610019268 A CN201610019268 A CN 201610019268A CN 105502897 B CN105502897 B CN 105502897B
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- quartz glass
- pure silica
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/14—Other methods of shaping glass by gas- or vapour- phase reaction processes
- C03B19/1415—Reactant delivery systems
- C03B19/1423—Reactant deposition burners
- C03B19/143—Plasma vapour deposition
Abstract
The present invention relates to a kind of preparation methods of super pure silica glass, using chemical vapor deposition method, using inductively coupled plasma flame as heat source, using the mixed gas of air and argon gas as plasma ionized gas, using silicon-containing compound as raw material, using the mixed gas of oxygen and helium as material containing gas, the above-mentioned silicon-containing material of the material containing gas carrying gasification, which is passed through by feeder in segmentation heat preserving type cvd furnace, to react, generate silica dioxide granule, it is deposited on quartz glass substrate, with the growth of depositional plane, quartz glass substrate is reduced to keep depositional plane height constant, gradually form quartz glass block.For the preparation method deposition rate of quartz glass of the present invention up to 180g/h, obtained quartz glass hydroxy radical content is less than 1ppm, and metals content impurity is less than 1ppm, and diameter is in 200mm or more, the defects of optical homogeneity is high, bubble-free, miscellaneous point, striped.
Description
Technical field
The present invention relates to a kind of preparation methods of quartz glass, more particularly to a kind of preparation side of super pure silica glass
Method.
Background technology
Quartz glass is SiO2Single component glass, distinctive structure make it have other materials can not replace physics,
Chemical property occupies irreplaceable status in high-tech area.
A kind of side preparing quartz glass using plasma chemical vapor deposition (PCVD) technique is proposed in the prior art
Method.It uses high frequency plasma directly to produce quartz glass as heat source, and chemical reaction and the production of quartz glass are existing
It is completed in quartz deposition stove.Plasma arc body is introduced to as heat source in cvd furnace, and arc body end is heavy away from what is be disposed vertically in stove
Product target surface about 5-20cm;Waiting for that target surface temperature rises to 1600 DEG C or more, arc temperature is reacted at 2000-3000 DEG C,
Introducing O2The SiCl of carrying4(material) gas stream makes air-flow add to away from about 5-10cm above target surface;O2And SiCl4In high temperature
Under nano level SiO is obtained by the reaction2Particle is deposited directly under the action of air-flow and gravity on target surface, and by target surface
Vitrified process be formed as quartz glass.Wherein, using O2As working gas, and by using O2It is taken as strip gas
Band SiCl4Into cvd furnace.Wherein, the flow control of rational cutting mode and gas stream is crucial, only with O when blanking2Make
For carrier gas, other components are not introduced, gas flow control is in 0.08-0.20m when feeding intake into cvd furnace3/h。
But it has the following disadvantages:(1) since plasma flame arc body terminal temperature used in this method this method is only
2000 DEG C -3000 DEG C, depositional plane temperature is low, and high-temperature region is small, and temperature gradient is big, and the quartz glass diameter prepared is caused to be no more than
150mm, in marginal existence bubble, optical homogeneity is more than 3 × 10-5;(2) due to plasma temperature and the limit of strip gas
It makes, the flow of strip oxygen used in this method need to be less than 0.2m3/ h, otherwise will cause silica dioxide granule that cannot effectively deposit,
Melting, leads to the defects of there are bubble, stripeds in quartz glass;Therefore, this method prepares the less efficient of quartz glass, causes
The significant wastage of the energy, raw material;(3) this method does not make requirement to ionized gas, cvd furnace pressure, leads to quartz glass still
There are the hydroxyl of 2ppm or more, this quartz glass, there are apparent absorption peak, limits it in optics at 2730nm wavelength
The application in field.
Invention content
It is a primary object of the present invention to provide a kind of preparation method of super pure silica glass, technology to be solved is asked
Topic is to shorten the preparation time of quartz glass, efficiently synthesizes large scale, high uniformity super pure silica glass, reduces manufacturing cost,
It is practical thus more suitable for production.
The object of the invention to solve the technical problems is realized using following technical scheme.
The present invention proposes a kind of preparation method of super pure silica glass, using chemical vapor deposition method, uses inductance coupling
Plasma flame is closed as heat source, using the mixed gas of air and argon gas as plasma ionized gas, with siliceous chemical combination
Object is raw material, and using the mixed gas of oxygen and helium as material containing gas, the material containing gas carries the above-mentioned siliceous original of gasification
Material is passed through in segmentation heat preserving type cvd furnace by feeder and is reacted, and is generated silica dioxide granule, is deposited on quartz glass substrate
On body, with the growth of depositional plane, quartz glass substrate is reduced to keep depositional plane height constant, gradually forms quartz glass block
Body.
Preferably, the preparation method of super pure silica glass above-mentioned, wherein the plasma ionized gas, described
The flow of argon gas is 0.1-10m3The dew point of/h, the air are less than -60 DEG C.
Preferably, the preparation method of super pure silica glass above-mentioned, wherein the inductively coupled plasma flame, is
Air and argon gas mixed gas are ionized by power high frequency equipment.
Preferably, inductively coupled plasma flame above-mentioned, wherein the high-frequency apparatus power is 10-500kW, frequency
Rate is 2-30MHz.
Preferably, the preparation method of super pure silica glass above-mentioned, wherein the inductively coupled plasma flame is 1
Or it is multiple.
Preferably, the preparation method of super pure silica glass above-mentioned, wherein the silicon-containing material is silicon tetrachloride or four
Silicon fluoride.
Preferably, the preparation method of super pure silica glass above-mentioned, wherein the material containing gas bag includes:With volume fraction
Meter:Oxygen content 70-95%, helium content 5-30%;Wherein oxygen flow is 0.1-1m3/h。
Preferably, the preparation method of super pure silica glass above-mentioned, wherein the segmentation heat preserving type cvd furnace, furnace body top section
It for arc header field, assists heating using electric calorifie installation, it is 1500 DEG C -1800 DEG C to make top section temperature;Stage casing is divided into 2-5 guarantor
Temperature section assists heating using electric calorifie installation, and it is 1000 DEG C -1500 DEG C to make furnace body middle portion temperature, and temperature is from top to bottom successively
It reduces;Hypomere uses circulating water cooling device, and lower portion of furnace body temperature is made to be maintained at 500 DEG C or less.
Preferably, the preparation method of super pure silica glass above-mentioned, wherein the cvd furnace inboard wall of furnace body uses high pure oxygen
Change aluminium refractory material, outside uses thermal insulation material, and middle part is equipped with exhaust outlet, and exhaust outlet quantity is one or more;Exhaust outlet connects
It is higher 1-50Pa than atmospheric pressure to control cvd furnace upper pressure by bleeding regulating wind pressure for air extractor.
Preferably, the preparation method of super pure silica glass above-mentioned feeds wherein the feeder is one or more
Device is inside lamp torch or outside lamp torch.
By above-mentioned technical proposal, the present invention at least has following advantages:(1) the quartz glass hydroxy radical content prepared is less than
1ppm, metals content impurity is less than 1ppm, and the defects of bubble-free, miscellaneous point and striped, diameter is in 200mm or more, optical homogeneity
Up to 2 × 10-6;(2) deposition rate is fast, in 100g/h or more, effectively reduces the waste of raw material.
Above description is only the general introduction of technical solution of the present invention, in order to better understand the technical means of the present invention,
And can be implemented in accordance with the contents of the specification, below with presently preferred embodiments of the present invention and after coordinating attached drawing to be described in detail such as.
Description of the drawings
Fig. 1 is quartz glass preparation facilities schematic diagram of the present invention.
Fig. 2 is cvd furnace structural schematic diagram of the present invention.
Specific implementation mode
It is of the invention to reach the technological means and effect that predetermined goal of the invention is taken further to illustrate, below in conjunction with
Attached drawing and preferred embodiment, the preparation method to the quartz glass proposed according to the present invention, specific implementation mode, structure, spy
Sign and its effect are described in detail as after.In the following description, what different " embodiment " or " embodiment " referred to is not necessarily same
One embodiment.In addition, the special characteristic, structure or feature in one or more embodiments can be combined by any suitable form.
As shown in Figure 1, a kind of method preparing super pure silica glass that one embodiment of the present of invention proposes, used
Equipment includes:Inductor coil 1, quartz lamp torch 2, inlet duct 3, plasma flame 4, cvd furnace 5, quartz glass substrate 6,
Material containing gas+silicon-containing material 7, feeder 8, protective gas 9, ionized gas 10 and obtained quartz glass block 11.
Using chemical vapor deposition method, using inductively coupled plasma flame as heat source, with air and argon gas
Mixed gas is as plasma ionized gas, using silicon-containing compound as raw material, using the mixed gas of oxygen and helium as load
Expect gas, the material containing gas, which carries the above-mentioned silicon-containing material to gasify and is passed through in segmentation heat preserving type cvd furnace by feeder, to be occurred
Reaction generates silica dioxide granule, is deposited on quartz glass substrate, with the growth of depositional plane, reduces quartz glass substrate
To keep depositional plane height constant, quartz glass block is gradually formed.
Plasma is obtained using double-layer air-flow.Internal layer gas is ionized gas, and stable high temperature etc. is formed after being ionized
Gas ions flame;Outer layer gas is protective gas, to guard lamp torch.The plasma arcs body that this mode obtains is stable, high
Warm area diameter is big, is conducive to prepare the good quartz glass of uniformity.The equal air of ionized gas, protective gas, can in ionized gas
Incorporation argon gas improves plasma flame temperature to improve ionization effect.
As shown in Fig. 2, a kind of deposition furnace structure that one embodiment of the present of invention proposes comprising:Exhaust outlet 12, deposition
Stove inner wall 13, thermal insulation material 14, bottom plate 15, cvd furnace stage casing 16, electric heater unit 17 and 18 and 20 and circulating water
Device 19.
The segmentation heat preserving type cvd furnace, furnace body top section are arc header field, assist heating using electric calorifie installation, make top
Duan Wendu is 1500 DEG C -1800 DEG C;Stage casing is divided into 2-5 soaking zone, assists heating using electric calorifie installation, makes furnace body middle portion temperature
It it is 1000 DEG C -1500 DEG C, and temperature reduces successively from top to bottom;Hypomere uses circulating water cooling device, makes lower portion of furnace body temperature
Degree is maintained at 500 DEG C or less.The heat radiation that high temperature generates at the top of this cvd furnace can make depositional plane be maintained at higher temperature, have
Conducive to improving deposition quality and expand the diameter of quartz glass;Controllable side wall temperatures make quartz glass slowly drop from top to bottom
Temperature is conducive to the shape for maintaining quartz glass, and internal structure is more uniform.
Cvd furnace inboard wall of furnace body uses high purity aluminium oxide refractory material, outside to use thermal insulation material, and middle part is equipped with exhaust outlet,
Exhaust outlet quantity is one or more.Exhaust outlet connects air extractor, and cvd furnace upper pressure ratio is controlled by bleeding regulating wind pressure
The high 1-50Pa of atmospheric pressure, to ensure the cleaning of atmosphere in reactor.
Preferably, a kind of preparation method for quartz glass that one embodiment of the present of invention proposes, uses power 10-
The high-frequency apparatus of 500kW, frequency 2-30MHz ionize plasma gas to generate high-frequency plasma flame.To ensure stone
The purity of English glass, air must pass through filtering and drying, air dew point made to be less than -60 DEG C.It, can be to air to improve ionization effect
Middle incorporation 0.1-10m3The argon gas of/h.Material containing gas O2Flow can be controlled in 0.1-1m3Between/h, while mixing the helium of 5%-30%
Gas.After silica dioxide granule is adsorbed to depositional plane, there are melting, the processes of desorption, and particle surface is adsorbed
Gas is discharged.The incorporation of helium contributes to the discharge of gas, and bubble is formed to avoid inside glass.But helium incorporation should not mistake
It is more, it otherwise will influence the oxidation reaction of raw material.
Example 1
It is that inductor coil 1 provides the high-frequency current that frequency is 10MHz using the high-frequency apparatus that power is 100kW, toward stone
It is passed through the air that dew point is -70 DEG C in English lamp torch 2 as ionized gas 10, and mixes 1m3The argon gas of/h, gas is by high-frequency current
The electromagnetism field ionization of generation forms plasma flame 4.Plasma flame 4 enters in cvd furnace 5 and heated quartz glass base
Body 6.Plasma flame enters in cvd furnace and heated quartz glass matrix.Using segmentation heat preserving type cvd furnace, stage casing is by 2
Soaking zone forms.By electric heater unit 17, top section temperature is set to be maintained at 1700 ± 20 DEG C, stage casing upper temp is maintained at 1400
± 20 DEG C, stage casing temperature of lower is maintained at 1100 ± 20 DEG C.Using circulating water cooling device 19, lower portion of furnace body temperature is made to be maintained at
500 DEG C or less.16 are equipped with 2 exhaust outlets 12 in the middle part of cvd furnace, and cvd furnace upper pressure is controlled than big by bleeding regulating wind pressure
The high 20Pa of air pressure.Material containing gas O2Carry SiCl4Raw material 7 enters cvd furnace, O by feeder 82Flow is 0.3m3/ h, material containing
Gas O2Middle incorporation 0.05m3The helium of/h.SiCl4With O2It reacts and generates SiO2And be deposited on quartz glass substrate 6, with
The growth of depositional plane, quartz glass substrate is slowly reduced to keep its upper level constant, gradually forms quartz glass block
Body 10.
Quartz glass diameter 250mm, the weight 8kg of preparation, without containing bubble, miscellaneous point, striped the defects of, deposition rate is
180g/h, it is 0.5ppm to measure its hydroxy radical content, and metals content impurity 0.6ppm, wavelength is that transmitance is 90% at 2730nm,
Optical homogeneity is 2 × 10-6。
Example 2
It is that inductor coil 1 provides the high-frequency current that frequency is 30MHz using the high-frequency apparatus that power is 50kW, toward stone
It is passed through the air that dew point is -60 DEG C in English lamp torch 2 as ionized gas 10, and mixes 0.1m3The argon gas of/h, gas is by high-frequency electrical
The raw electromagnetism field ionization of miscarriage, forms plasma flame 4.Plasma flame 4 enters in cvd furnace 5 and heated quartz glass
Matrix 6.Plasma flame enters in cvd furnace and heated quartz glass matrix.Using segmentation heat preserving type cvd furnace, stage casing is by 4
A soaking zone composition.By electric heater unit 17, top section temperature is made to be maintained at 1780 ± 20 DEG C, stage casing temperature is from top to bottom successively
It is maintained at 1400 ± 20 DEG C, 1300 ± 20 DEG C, 1200 ± 20 DEG C, 1100 ± 20 DEG C.Using circulating water cooling device 19, make furnace body
Temperature of lower is maintained at 500 DEG C or less.16 are equipped with 4 exhaust outlets 12 in the middle part of cvd furnace, are controlled and are deposited by bleeding regulating wind pressure
Stove upper pressure is higher 50Pa than atmospheric pressure.Material containing gas O2Carry SiF4Raw material 7 enters cvd furnace, O by feeder 82Flow is
0.1m3/ h, material containing gas O2Middle incorporation 0.05m3The helium of/h.SiF4With O2It reacts and generates SiO2And it is deposited on quartz glass
On matrix 6, with the growth of depositional plane, quartz glass substrate is slowly reduced to keep its upper level constant, is gradually formed
Quartz glass block 10.
The defects of quartz glass a diameter of 200mm, quality 9kg, bubble-free, miscellaneous point, striped of preparation, deposition rate is
100g/h, it is 0.7ppm to measure its hydroxy radical content, and metals content impurity 0.4ppm, wavelength is that transmitance is 90% at 2730nm.
Example 3
It is that inductor coil 1 provides the high-frequency current that frequency is 2MHz using the high-frequency apparatus that power is 200kW, toward stone
It is passed through the air that dew point is -60 DEG C in English lamp torch 2 as ionized gas 10, and mixes 10m3The argon gas of/h, gas is by high-frequency electrical
The raw electromagnetism field ionization of miscarriage, forms plasma flame 4.Using segmentation heat preserving type cvd furnace, stage casing is by 5 soaking zone groups
At.By electric heater unit 17, top section temperature is set to be maintained at 1520 ± 20 DEG C, stage casing temperature is maintained at 1430 successively from top to bottom
±20℃、1360±20℃、1300±20℃、1200±20℃、1100±20℃.Using circulating water cooling device 19, make stove
Body temperature of lower is maintained at 500 DEG C or less.16 are equipped with 1 exhaust outlet 12 in the middle part of cvd furnace, and it is heavy to be controlled by bleeding regulating wind pressure
Product stove upper pressure is higher 1Pa than atmospheric pressure.Plasma flame 4 enters in cvd furnace 5 and heated quartz glass matrix 6.Material containing
Gas O2Carry SiCl4Raw material 7 enters cvd furnace, O by feeder 82Flow is 1m3/ h, material containing gas O2Middle incorporation 0.3m3/h
Helium.SiCl4With O2It reacts and generates SiO2And be deposited on quartz glass substrate 6, with the growth of depositional plane, slowly
Quartz glass substrate is reduced to keep its upper level constant, gradually forms quartz glass block 10.
The defects of quartz glass a diameter of 300mm, quality 15kg, bubble-free, miscellaneous point, striped of preparation, deposition rate
For 190g/h, it is 0.4ppm to measure its hydroxy radical content, and metals content impurity 0.9ppm, wavelength is that transmitance is at 2730nm
90%, optical homogeneity is 2 × 10-6。
The above described is only a preferred embodiment of the present invention, be not intended to limit the present invention in any form, according to
According to the technical spirit of the present invention to any simple modification, equivalent change and modification made by above example, this hair is still fallen within
In the range of bright technical solution.
Claims (9)
1. a kind of preparation method of super pure silica glass, which is characterized in that use chemical vapor deposition method, use inductive coupling
Plasma flame is as heat source, using the mixed gas of air and argon gas as plasma ionized gas, with silicon-containing compound
For raw material, using the mixed gas of oxygen and helium as material containing gas, the material containing gas carries the above-mentioned silicon-containing material of gasification
It is passed through in segmentation heat preserving type cvd furnace and is reacted by feeder, generated silica dioxide granule, be deposited on quartz glass substrate
On, with the growth of depositional plane, quartz glass substrate is reduced to keep depositional plane height constant, gradually forms quartz glass block
Body;
The segmentation heat preserving type cvd furnace, furnace body top section are arc header field, assist heating using electric calorifie installation, make top Duan Wen
Degree is 1500 DEG C -1800 DEG C;Stage casing is divided into 2-5 soaking zone, assists heating using electric calorifie installation, makes the furnace body middle portion temperature be
1000 DEG C -1500 DEG C, and temperature reduces successively from top to bottom;Hypomere uses circulating water cooling device, makes lower portion of furnace body temperature
It is maintained at 500 DEG C or less.
2. the preparation method of super pure silica glass according to claim 1, which is characterized in that the plasma ionization
The flow of gas, the argon gas is 0.1-10m3The dew point of/h, the air are less than -60 DEG C.
3. the preparation method of super pure silica glass according to claim 1, which is characterized in that described inductive coupling etc. from
Air and argon gas mixed gas are ionized to obtain by daughter flame by power high frequency equipment.
4. the preparation method of super pure silica glass according to claim 3, which is characterized in that the high-frequency apparatus, work(
Rate is 10-500kW, frequency 2-30MHz.
5. the preparation method of super pure silica glass according to claim 1, which is characterized in that described inductive coupling etc. from
Sub- flame is one or more.
6. the preparation method of super pure silica glass according to claim 1, which is characterized in that the silicon-containing material is four
Silicon chloride or ocratation.
7. the preparation method of super pure silica glass according to claim 1, which is characterized in that the material containing gas bag includes:
With volume fraction:Oxygen content 70-95%, helium content 5-30%;Wherein oxygen flow is 0.1-1m3/h。
8. the preparation method of super pure silica glass according to claim 1, which is characterized in that the cvd furnace inboard wall of furnace body
Using high purity aluminium oxide refractory material, outside uses thermal insulation material, and middle part is equipped with exhaust outlet, and exhaust outlet quantity is one or more;
Exhaust outlet connects air extractor, and it is higher 1-50Pa than atmospheric pressure to control cvd furnace upper pressure by bleeding regulating wind pressure.
9. the preparation method of super pure silica glass according to claim 1, which is characterized in that the feeder is 1
Or it is multiple.
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CN105967499A (en) * | 2016-05-11 | 2016-09-28 | 施庭樟 | Preparation technology of quartz glass plate |
JP2018193279A (en) * | 2017-05-18 | 2018-12-06 | 住友電気工業株式会社 | Method for manufacturing glass fine particle deposit, method for manufacturing glass preform and glass fine particle deposit |
CN107902875A (en) * | 2017-11-22 | 2018-04-13 | 中国建筑材料科学研究总院有限公司 | Quartz glass and preparation method thereof |
CN111943215B (en) * | 2019-05-14 | 2022-02-22 | 中天科技精密材料有限公司 | Preparation method of quartz powder |
CN114315106A (en) * | 2020-10-12 | 2022-04-12 | 中天科技精密材料有限公司 | Deposition equipment and preparation method of high-purity quartz glass |
CN112876044B (en) * | 2021-02-03 | 2024-01-05 | 江苏亨通智能科技有限公司 | Chemical deposition method and device for high-purity low-hydroxyl high-uniformity quartz glass |
CN117550787B (en) * | 2024-01-11 | 2024-03-15 | 内蒙古金沙布地恒通光电科技有限公司 | High-stability preparation system based on high-purity low-hydroxyl quartz glass |
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JP4474736B2 (en) * | 2000-05-26 | 2010-06-09 | 株式会社ニコン | Quartz glass manufacturing method |
CN1314608C (en) * | 2005-06-10 | 2007-05-09 | 中国建筑材料科学研究院 | High-frequency plasma vapor phase synthesis method for quartz glass |
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