CN105502897A - Preparing method for ultra-pure quartz glass - Google Patents
Preparing method for ultra-pure quartz glass Download PDFInfo
- Publication number
- CN105502897A CN105502897A CN201610019268.9A CN201610019268A CN105502897A CN 105502897 A CN105502897 A CN 105502897A CN 201610019268 A CN201610019268 A CN 201610019268A CN 105502897 A CN105502897 A CN 105502897A
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- Prior art keywords
- silica glass
- gas
- preparation
- quartz glass
- pure silica
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Classifications
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B20/00—Processes specially adapted for the production of quartz or fused silica articles, not otherwise provided for
-
- 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
-
- 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
- C03B19/1407—Deposition reactors therefor
Abstract
The invention relates to a preparing method for ultra-pure quartz glass. The chemical vapor deposition method is adopted, inductive coupling plasma flames serve as a heat source, mixed gas of air and argon serves as plasma ionized gas, a silicon-containing compound serves as a raw material, mixed gas of oxygen and helium serves as material carrying gas, the material carrying gas carries a gasified silicon-containing raw material to be introduced into a segmented heat-preserving type deposition furnace through a feeder to be subjected to a reaction, so that silicon dioxide particles are generated and deposit on a quartz glass matrix, as the deposition face grows, the quartz glass matrix is lowered so as to keep the height of the deposition face unchanged, and a quartz glass block is gradually formed. According to the preparing method for the quartz glass, the deposition rate can reach 180 g/h, the content of hydroxyl in the obtained quartz glass is smaller than 1 ppm, the content of metal impurities is smaller than 1 ppm, the diameter is over 200 mm, optical uniformity is high, and defects such as bubbles, impure points and stripes are avoided.
Description
Technical field
The present invention relates to a kind of preparation method of silica glass, particularly relate to a kind of preparation method of super pure silica glass.
Background technology
Silica glass is SiO
2single component glass, physics, chemical property that its distinctive structure makes it have other material cannot to replace, occupy irreplaceable status in high-tech area.
A kind of method adopting PCVD (PCVD) technique to prepare silica glass is proposed in the prior art.It adopts high frequency plasma as thermal source direct production silica glass, and the production of chemical reaction and silica glass completes in existing quartz deposition stove.Plasma arc body is introduced in cvd furnace as thermal source, the vertical about 5-20cm of deposition target surface placed in arc body end-to-end distance stove; Treat that target surface temperature rises to more than 1600 DEG C, arc temperature reacts when 2000-3000 DEG C, introducing O
2the SiCl carried
4(material) gas stream, makes air-flow add to about 5-10cm place above target surface; O
2and SiCl
4at high temperature be obtained by reacting nano level SiO
2particulate, is deposited directly on target surface under the effect of air-flow and gravity, and through being formed as silica glass in vitrified process of target surface.Wherein, O is adopted
2as working gas, and by adopting O
2siCl is carried as band material gas
4enter cvd furnace.Wherein, the flow control of rational cutting mode and gas stream is crucial, only with O during blanking
2as carrier gas, do not introduce other components, when feeding intake in cvd furnace, gas flow controls at 0.08-0.20m
3/ h.
But have the following disadvantages: (1) is only 2000 DEG C-3000 DEG C due to the method the method plasma flame arc used body terminal temperature, depositional plane temperature is low, high-temperature zone is little, thermograde is large, the silica glass diameter prepared is caused to be no more than 150mm, at marginal existence bubble, optical homogeneity is greater than 3 × 10
-5; (2) because the restriction of gas expected by plasma temperature and band, the flow of the method band material used oxygen need be less than 0.2m
3/ h, otherwise will cause that silica dioxide granule can not effectively deposit, melting, cause in silica glass, there is the defect such as bubble, striped; Therefore, the efficiency that the method prepares silica glass is lower, causes the significant wastage of the energy, raw material; (3) the method does not make requirement to ionized gas, cvd furnace pressure, causes silica glass still to there is the hydroxyl of more than 2ppm, and this silica glass exists obvious absorption peak at 2730nm wavelength place, limits its application at optical field.
Summary of the invention
Main purpose of the present invention is, there is provided a kind of preparation method of super pure silica glass, technical problem to be solved shortens the preparation time of silica glass, efficiently synthesizes large size, high uniformity super pure silica glass, reduce manufacturing cost, thus be more suitable for producing practicality.
The object of the invention to solve the technical problems realizes by the following technical solutions.
The present invention proposes a kind of preparation method of super pure silica glass, adopt chemical vapor deposition method, use inductively coupled plasma flame as thermal source, gas is ionized as plasma body using the mixed gas of air and argon gas, take silicon-containing compound as raw material, using the mixed gas of oxygen and helium as material containing gas, the above-mentioned silicon-containing material that described material containing gas carries gasification is passed in segmentation heat preserving type cvd furnace by feeder and reacts, generate silica dioxide granule, be deposited on quartz glass substrate, along with the growth of depositional plane, reduce quartz glass substrate to keep depositional plane height constant, form silica glass block gradually.
Preferably, the preparation method of aforesaid super pure silica glass, wherein said plasma body ionization gas, the flow of described argon gas is 0.1-10m
3/ h, the dew point of described air is less than-60 DEG C.
Preferably, the preparation method of aforesaid super pure silica glass, wherein said inductively coupled plasma flame, is obtained air and the ionization of argon gas mixed gas by power high frequency equipment.
Preferably, aforesaid inductively coupled plasma flame, wherein said high-frequency apparatus power is 10-500kW, frequency is 2-30MHz.
Preferably, the preparation method of aforesaid super pure silica glass, wherein said inductively coupled plasma flame is one or more.
Preferably, the preparation method of aforesaid super pure silica glass, wherein said silicon-containing material is silicon tetrachloride or silicon tetrafluoride.
Preferably, the preparation method of aforesaid super pure silica glass, wherein said material containing gas bag is drawn together: with volume fraction: oxygen content 70-95%, helium content 5-30%; Wherein oxygen flow is 0.1-1m
3/ h.
Preferably, the preparation method of aforesaid super pure silica glass, wherein said segmentation heat preserving type cvd furnace, body of heater top section is arched top cover, uses electric heating device boosting, makes top section temperature be 1500 DEG C-1800 DEG C; Stage casing is divided into 2-5 holding-zone, adopts electric heating device boosting, make body of heater middle portion temperature be 1000 DEG C-1500 DEG C, and temperature reduces successively from top to bottom; Hypomere adopts circulating water cooling device, makes lower portion of furnace body temperature remain on less than 500 DEG C.
Preferably, the preparation method of aforesaid super pure silica glass, wherein said cvd furnace inboard wall of furnace body uses high purity aluminium oxide refractory materials, and outside uses thermal insulation material, and middle part is provided with exhaust outlet, and exhaust outlet quantity is one or more; Exhaust outlet connects air extractor, controls cvd furnace upper pressure than normal atmosphere height 1-50Pa by bleeding regulating blast.
Preferably, the preparation method of aforesaid super pure silica glass, wherein said feeder is one or more, and feeder is inner or lamp torch outside at lamp torch.
By technique scheme, the present invention at least has following advantages: silica glass hydroxy radical content prepared by (1) is less than 1ppm, and metals content impurity is less than 1ppm, the defects such as bubble-free, assorted point and striped, diameter is at more than 200mm, and optical homogeneity can reach 2 × 10
-6; (2) sedimentation rate is fast, at more than 100g/h, effectively reduces the waste of raw material.
Above-mentioned explanation is only the general introduction of technical solution of the present invention, in order to better understand technique means of the present invention, and can be implemented according to the content of specification sheets, coordinates accompanying drawing to be described in detail as follows below with preferred embodiment of the present invention.
Accompanying drawing explanation
Fig. 1 is silica glass preparation facilities schematic diagram of the present invention.
Fig. 2 is cvd furnace structural representation of the present invention.
Embodiment
For further setting forth the present invention for the technique means reaching predetermined goal of the invention and take and effect, below in conjunction with accompanying drawing and preferred embodiment, to the preparation method of the silica glass proposed according to the present invention, its embodiment, structure, feature and effect thereof, be described in detail as follows.In the following description, the not necessarily same embodiment that different " embodiment " or " embodiment " refers to.In addition, special characteristic, structure or feature in one or more embodiment 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 propose, the equipment adopted comprises: inductor coil 1, quartz lamp torch 2, diffuser 3, plasma flame 4, cvd furnace 5, quartz glass substrate 6, material containing gas+silicon-containing material 7, feeder 8, shielding gas 9, ionized gas 10 and obtained silica glass block 11.
Adopt chemical vapor deposition method, use inductively coupled plasma flame as thermal source, gas is ionized as plasma body using the mixed gas of air and argon gas, take silicon-containing compound as raw material, using the mixed gas of oxygen and helium as material containing gas, the above-mentioned silicon-containing material that described material containing gas carries gasification is passed in segmentation heat preserving type cvd furnace by feeder and reacts, generate silica dioxide granule, be deposited on quartz glass substrate, along with the growth of depositional plane, reduce quartz glass substrate to keep depositional plane height constant, form silica glass block gradually.
Double-layer air-flow is adopted to obtain plasma body.Internal layer gas is ionized gas, is ionized the high temperature plasma flame that rear formation is stable; Outer gas is shielding gas, in order to guard lamp torch.The plasma arcs body that this mode obtains is stable, high-temperature zone diameter is large, is conducive to the silica glass preparing good uniformity.The equal air of ionized gas, shielding gas, can mix argon gas to improve ionization effect, improve plasma flame temperature in ionized gas.
As shown in Figure 2, a kind of cvd furnace structure that one embodiment of the present of invention propose, it comprises: exhaust outlet 12, cvd furnace inwall 13, lagging material 14, bottom plate 15, cvd furnace stage casing 16, electric heater unit 17 and 18 and 20 and circulating water cooling device 19.
Described segmentation heat preserving type cvd furnace, body of heater top section is arched top cover, uses electric heating device boosting, makes top section temperature be 1500 DEG C-1800 DEG C; Stage casing is divided into 2-5 holding-zone, adopts electric heating device boosting, make body of heater middle portion temperature be 1000 DEG C-1500 DEG C, and temperature reduces successively from top to bottom; Hypomere adopts circulating water cooling device, makes lower portion of furnace body temperature remain on less than 500 DEG C.The thermal radiation that this cvd furnace top high temperature produces can make depositional plane remain on comparatively high temps, is conducive to improving deposition quality and the diameter expanding silica glass; Controlled side wall temperatures makes silica glass slow cooling from top to bottom, be conducive to the shape maintaining silica glass, and internal structure is comparatively even.
Cvd furnace inboard wall of furnace body uses high purity aluminium oxide refractory materials, and outside uses thermal insulation material, and middle part is provided with exhaust outlet, and exhaust outlet quantity is one or more.Exhaust outlet connects air extractor, controls cvd furnace upper pressure than normal atmosphere height 1-50Pa, to ensure the cleaning of atmosphere in reactor by bleeding regulating blast.
Preferably, the preparation method of a kind of silica glass that one embodiment of the present of invention propose, uses the high-frequency apparatus of power 10-500kW, frequency 2-30MHz, by plasma gas ionization to produce high frequency plasma flame.For ensureing the purity of silica glass, air must, through filtering with dry, make air dew point be less than-60 DEG C.For improving ionization effect, 0.1-10m can be mixed in air
3the argon gas of/h.Material containing gas O
2flow can be controlled in 0.1-1m
3between/h, mix the helium of 5%-30% simultaneously.After silica dioxide granule is adsorbed to depositional plane, there is the process of melting, desorption, discharge with the gas that particle surface is adsorbed.Helium be mixed with the discharge helping gas, with avoid inside glass formed bubble.But helium incorporation is too much unsuitable, otherwise will affect the oxidizing reaction of raw material.
Example 1
The high-frequency apparatus that uses power to be 100kW, for inductor coil 1 provides frequency to be the high-frequency current of 10MHz, pass in quartz lamp torch 2 dew point be the air of-70 DEG C as ionized gas 10, and mix 1m
3the argon gas of/h, gas is ionized by the electromagnetic field that high-frequency current produces, and forms plasma flame 4.Plasma flame 4 enters the interior also heated quartz glass basis 6 of cvd furnace 5.Plasma flame enters the interior also heated quartz glass basis of cvd furnace.Use segmentation heat preserving type cvd furnace, stage casing is made up of 2 holding-zones.By electric heater unit 17, make top section temperature remain on 1700 ± 20 DEG C, stage casing upper temp remains on 1400 ± 20 DEG C, and stage casing temperature of lower remains on 1100 ± 20 DEG C.Use circulating water cooling device 19, make lower portion of furnace body temperature remain on less than 500 DEG C.In the middle part of cvd furnace, 16 are provided with 2 exhaust outlets 12, control cvd furnace upper pressure than normal atmosphere height 20Pa by bleeding regulating blast.Material containing gas O
2carry SiCl
4raw material 7 enters cvd furnace by feeder 8, O
2flow is 0.3m
3/ h, material containing gas O
2in mix 0.05m
3the helium of/h.SiCl
4with O
2react and generate SiO
2and be deposited on quartz glass substrate 6, along with the growth of depositional plane, slowly reduce quartz glass substrate to keep its upper level constant, form silica glass block 10 gradually.
The silica glass diameter 250mm of preparation, weight 8kg, not containing defects such as bubble, assorted point, stripeds, sedimentation rate is 180g/h, and recording its hydroxy radical content is 0.5ppm, metals content impurity 0.6ppm, wavelength is 2730nm place transmitance is 90%, and optical homogeneity is 2 × 10
-6.
Example 2
The high-frequency apparatus that uses power to be 50kW, for inductor coil 1 provides frequency to be the high-frequency current of 30MHz, pass in quartz lamp torch 2 dew point be the air of-60 DEG C as ionized gas 10, and mix 0.1m
3the argon gas of/h, gas is ionized by the electromagnetic field that high-frequency current produces, and forms plasma flame 4.Plasma flame 4 enters the interior also heated quartz glass basis 6 of cvd furnace 5.Plasma flame enters the interior also heated quartz glass basis of cvd furnace.Use segmentation heat preserving type cvd furnace, stage casing is made up of 4 holding-zones.By electric heater unit 17, make top section temperature remain on 1780 ± 20 DEG C, stage casing temperature remains on 1400 ± 20 DEG C, 1300 ± 20 DEG C, 1200 ± 20 DEG C, 1100 ± 20 DEG C from top to bottom successively.Use circulating water cooling device 19, make lower portion of furnace body temperature remain on less than 500 DEG C.In the middle part of cvd furnace, 16 are provided with 4 exhaust outlets 12, control cvd furnace upper pressure than normal atmosphere height 50Pa by bleeding regulating blast.Material containing gas O
2carry SiF
4raw material 7 enters cvd furnace by feeder 8, O
2flow is 0.1m
3/ h, material containing gas O
2in mix 0.05m
3the helium of/h.SiF
4with O
2react and generate SiO
2and be deposited on quartz glass substrate 6, along with the growth of depositional plane, slowly reduce quartz glass substrate to keep its upper level constant, form silica glass block 10 gradually.
The silica glass diameter of preparation is 200mm, and quality is 9kg, and the defects such as bubble-free, assorted point, striped, sedimentation rate is 100g/h, and recording its hydroxy radical content is 0.7ppm, metals content impurity 0.4ppm, and wavelength is 2730nm place transmitance is 90%.
Example 3
The high-frequency apparatus that uses power to be 200kW, for inductor coil 1 provides frequency to be the high-frequency current of 2MHz, pass in quartz lamp torch 2 dew point be the air of-60 DEG C as ionized gas 10, and mix 10m
3the argon gas of/h, gas is ionized by the electromagnetic field that high-frequency current produces, and forms plasma flame 4.Use segmentation heat preserving type cvd furnace, stage casing is made up of 5 holding-zones.By electric heater unit 17, make top section temperature remain on 1520 ± 20 DEG C, stage casing temperature remains on 1430 ± 20 DEG C, 1360 ± 20 DEG C, 1300 ± 20 DEG C, 1200 ± 20 DEG C, 1100 ± 20 DEG C from top to bottom successively.Use circulating water cooling device 19, make lower portion of furnace body temperature remain on less than 500 DEG C.In the middle part of cvd furnace, 16 are provided with 1 exhaust outlet 12, control cvd furnace upper pressure than normal atmosphere height 1Pa by bleeding regulating blast.Plasma flame 4 enters the interior also heated quartz glass basis 6 of cvd furnace 5.Material containing gas O
2carry SiCl
4raw material 7 enters cvd furnace by feeder 8, O
2flow is 1m
3/ h, material containing gas O
2in mix 0.3m
3the helium of/h.SiCl
4with O
2react and generate SiO
2and be deposited on quartz glass substrate 6, along with the growth of depositional plane, slowly reduce quartz glass substrate to keep its upper level constant, form silica glass block 10 gradually.
The silica glass diameter of preparation is 300mm, and quality is 15kg, the defects such as bubble-free, assorted point, striped, sedimentation rate is 190g/h, and recording its hydroxy radical content is 0.4ppm, metals content impurity 0.9ppm, wavelength is 2730nm place transmitance is 90%, and optical homogeneity is 2 × 10
-6.
The above, it is only preferred embodiment of the present invention, not do any pro forma restriction to the present invention, any simple modification done above embodiment according to technical spirit of the present invention, equivalent variations and modification, all still belong in the scope of technical solution of the present invention.
Claims (10)
1. the preparation method of a super pure silica glass, it is characterized in that, adopt chemical vapor deposition method, use inductively coupled plasma flame as thermal source, gas is ionized as plasma body using the mixed gas of air and argon gas, take silicon-containing compound as raw material, using the mixed gas of oxygen and helium as material containing gas, the above-mentioned silicon-containing material that described material containing gas carries gasification is passed in segmentation heat preserving type cvd furnace by feeder and reacts, generate silica dioxide granule, be deposited on quartz glass substrate, along with the growth of depositional plane, reduce quartz glass substrate to keep depositional plane height constant, form silica glass block gradually.
2. the preparation method of super pure silica glass according to claim 1, is characterized in that, described plasma body ionization gas, the flow of described argon gas is 0.1-10m
3/ h, the dew point of described air is less than-60 DEG C.
3. the preparation method of super pure silica glass according to claim 1, is characterized in that, described inductively coupled plasma flame, air and the ionization of argon gas mixed gas is obtained by power high frequency equipment.
4. inductively coupled plasma flame according to claim 3, is characterized in that, described high-frequency apparatus, and power is 10-500kW, frequency is 2-30MHz.
5. the preparation method of super pure silica glass according to claim 1, is characterized in that, described inductively coupled plasma flame is one or more.
6. the preparation method of super pure silica glass according to claim 1, is characterized in that, described silicon-containing material is silicon tetrachloride or silicon tetrafluoride.
7. the preparation method of super pure silica glass according to claim 1, is characterized in that, described material containing gas bag is drawn together: with volume fraction: oxygen content 70-95%, helium content 5-30%; Wherein oxygen flow is 0.1-1m
3/ h.
8. the preparation method of super pure silica glass according to claim 1, is characterized in that, described segmentation heat preserving type cvd furnace, and body of heater top section is arched top cover, uses electric heating device boosting, makes top section temperature be 1500 DEG C-1800 DEG C; Stage casing is divided into 2-5 holding-zone, adopts electric heating device boosting, make body of heater middle portion temperature be 1000 DEG C-1500 DEG C, and temperature reduces successively from top to bottom; Hypomere adopts circulating water cooling device, makes lower portion of furnace body temperature remain on less than 500 DEG C.
9. the preparation method of super pure silica glass according to claim 1, is characterized in that, described cvd furnace inboard wall of furnace body uses high purity aluminium oxide refractory materials, and outside uses thermal insulation material, and middle part is provided with exhaust outlet, and exhaust outlet quantity is one or more; Exhaust outlet connects air extractor, controls cvd furnace upper pressure than normal atmosphere height 1-50Pa by bleeding regulating blast.
10. the preparation method of super pure silica glass according to claim 1, is characterized in that, described feeder is one or more, and feeder is inner or lamp torch outside at lamp torch.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105967499A (en) * | 2016-05-11 | 2016-09-28 | 施庭樟 | Preparation technology of quartz glass plate |
| 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 |
| CN108947212A (en) * | 2017-05-18 | 2018-12-07 | 住友电气工业株式会社 | Glass microbead deposit manufacturing method, base glass material manufacturing method and glass microbead deposit |
| WO2020228115A1 (en) * | 2019-05-14 | 2020-11-19 | 中天科技精密材料有限公司 | Quartz powder and preparation method therefor |
| CN112876044A (en) * | 2021-02-03 | 2021-06-01 | 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 |
| 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 |
| CN117550787A (en) * | 2024-01-11 | 2024-02-13 | 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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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105967499A (en) * | 2016-05-11 | 2016-09-28 | 施庭樟 | Preparation technology of quartz glass plate |
| CN108947212A (en) * | 2017-05-18 | 2018-12-07 | 住友电气工业株式会社 | Glass microbead deposit manufacturing method, base glass material manufacturing method and glass microbead deposit |
| CN108947212B (en) * | 2017-05-18 | 2022-08-19 | 住友电气工业株式会社 | Method for producing glass microparticle deposit, method for producing glass base material, and glass microparticle 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 |
| WO2020228115A1 (en) * | 2019-05-14 | 2020-11-19 | 中天科技精密材料有限公司 | Quartz powder and preparation method therefor |
| 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 |
| CN112876044A (en) * | 2021-02-03 | 2021-06-01 | 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 |
| 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 |
| CN117550787A (en) * | 2024-01-11 | 2024-02-13 | 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 |
| 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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|---|---|
| CN105502897B (en) | 2018-08-24 |
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