CN1314608C - High-frequency plasma vapor phase synthesis method for quartz glass - Google Patents
High-frequency plasma vapor phase synthesis method for quartz glass Download PDFInfo
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- CN1314608C CN1314608C CNB2005100766134A CN200510076613A CN1314608C CN 1314608 C CN1314608 C CN 1314608C CN B2005100766134 A CNB2005100766134 A CN B2005100766134A CN 200510076613 A CN200510076613 A CN 200510076613A CN 1314608 C CN1314608 C CN 1314608C
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- 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
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- C03B19/143—Plasma vapour deposition
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Abstract
The present invention discloses a high-frequency plasma vapor phase synthesis method for quartz glass. The present invention comprises the steps that continuous plasma arcs are introduced as a heat source of a production furnace; oxygen and silicon tetrachloride gas are mixed and are put onto the top of the internal target surface of the production furnace in a continuous and steady flow rate; silicon oxide particles are produced and are deposited onto the target surface to form glass. The present invention uses pure plasma as the heat source, no outside impurities are introduced, the produced quartz glass has better representation in the aspect of total spectrum transmittance, and the transmittance is higher with the spectrum of 2730 nm, wherein the content of hydroxyl is equal to or even lower than 5 ppm. The quartz glass also has the advantages of high purity, high glass optical uniformity, etc. The quartz glass can satisfy the requirements for high-quality quartz pendulum slices and special type optical materials.
Description
Technical field
The present invention relates to the preparation of silica glass, particularly a kind of method for preparing the high-performance special silica glass.
Background technology
Transparency silica glass has than multi-usage industrial.Silica glass and preparation thereof generally have following three kinds of main types:
The I class: with mineral crystal or quartz sand is raw material, the transparency silica glass of founding with electric heating process.The atmosphere of founding has inert atmosphere, hydrogen atmosphere, also can be vacuum.(OH) content is lower than 5ppm (ppm=1 * 10 to hydroxyl in the silica glass of founding under vacuum or inert atmosphere
-4%); Hydroxy radical content can reach 150ppm in the silica glass of founding under hydrogen atmosphere.The foreign matter content height of this type of silica glass, Al content are 30～100ppm, alkali metal content 5～10ppm.Be mainly used in electric light source, also be applied to industries such as metallurgy, chemical industry, semi-conductor.
II class: the transparency silica glass that the mineral crystal raw material is founded in hydrogen one oxygen flame.Hydroxy radical content reaches 180～250ppm in this type of silica glass.Metals content impurity is low, and Al content is less than 20ppm, and alkali metal content is lower than 5ppm, and softening temperature is than low 50 ℃ of I quartz-like glass.Be mainly used in semi-conductor, the light source industry also is used for industries such as chemical industry, metallurgy.
III class: the hydrolysis in hydrogen-oxygen flame of silicon tetrachloride gas raw material, found into silica glass.The metals content impurity of this type of silica glass is lower than 1ppm, but hydroxy radical content surpasses 1000ppm, and contains the above Cl of 100ppm.The softening temperature of III quartz-like glass is than low 50～100 ℃ of preceding two quartz-like glass, but foreign matter content is low, and optics is even, saturating ultraviolet, and anti-x ray irradiation x is applicable to optical material.
Along with the development in sophisticated technology fields such as space technology and photoconductive fiber, have higher requirement for the special optical material of high-performance (photopermeability is good), i.e. IV quartz-like glass.Foreign matter content should be lower than 1ppm in this quartz-like glass, and hydroxy radical content can be controlled to and is lower than 5ppm, Cl content 200ppm.The optical homogeneity height of glass sees through light wavelength wide ranges (0.18～3.5 μ m), is applicable to high quality quartz pendulous reed and special optical material, as space technology laser reflecting prism and photoconductive fiber.The production method of research IV quartz-like glass all is in confidential state at present, does not have the pertinent literature report.
The innovation and creation content
The object of the present invention is to provide a kind of method of the IV of preparation class high-performance special silica glass, the silica glass of preparation can be used as the special optical material.
The method of a kind of high frequency plasma gas phase synthetic quartz glass of the present invention, comprise that the plasma arc introducing that will continue is as the thermal source of producing stove, oxygen and silicon tetrachloride gas mixed and, generate silicon dioxide microparticle and also be deposited into the step that forms glass on the target surface with the continual and steady flow target surface top in the stove of putting into production.
In the aforesaid method, the numerical value of the arc body length of described plasma arc between 20～40cm, the numerical value of arc body terminal temperature between 2000～3000 ℃, and in the entire method temperature fluctuation range within 5%.
In the aforesaid method, oxygen and silicon tetrachloride mixed gas flow in the described stove that puts into production are 0.08～0.20m
3A numerical value the between/h, and in the whole input process flow rate fluctuation scope within 5%.
In the aforesaid method, oxygen and silicon tetrachloride gas blended concrete steps are:
1) will feed the bubbling bottle bottom that Sheng is loaded with the liquid silicon tetrachloride with material oxygen, the bubbling bottle keeps 40 ℃ temperature;
2) gas that will collect from bubbling bottle top feeds a gasification bottle bottom, and the gasification bottle keeps 80 ℃ temperature;
3) gas that will collect from gasification bottle top feeds flow control bottle, feeds in this flow control bottle simultaneously
Auxiliary oxygen with flow valve control auxiliary oxygen flow, is drawn oxygen from the outlet of this flow control bottle then
Gas and the silicon tetrachloride mixed gas stove that puts into production.
In the aforesaid method, described band material oxygen flow is controlled at 0.06～0.15m
3/ h, the auxiliary oxygen flow is controlled at 0.08～0.20m
3A numerical value the between/h; The arc body length of preferred plasma arc is 25cm, and arc body terminal temperature is 2000 ℃, and band material oxygen flow is controlled at 0.08m
3/ h, the auxiliary oxygen flow is controlled at 0.12m
3/ h.
The present invention with purified plasma body as thermal source, there is not the introducing of introduced contaminants, the silica glass of producing is having performance preferably aspect the full spectral transmittance, and the spectral transmittance at 2730nm is higher, wherein hydroxy radical content is only below 5ppm, using under the situation of pure raw material even can reach about 2ppm, this silica glass also has the optical homogeneity advantages of higher of purity height, glass, satisfies the requirement that is used for high quality quartz pendulous reed and special optical material.
Description of drawings
Fig. 1 is preparation technology's flow process of the present invention.
Fig. 2 produces synoptic diagram for silica glass of the present invention.
Fig. 3 is that mixed gas forms synoptic diagram in the inventive method.
Fig. 4-1 detects collection of illustrative plates for the silica glass transmitance that the inventive method obtains.
Fig. 4-2 is that four kinds of silica glass transmitances detect the contrast collection of illustrative plates.
Embodiment
The inventive method be with the silicon tetrachloride be raw material in the flame passes of no hydrogen high temperature oxidation, found into silica glass.Preparation technology's flow process is referring to Fig. 1.
Among the present invention, use no hydrogen flame passes as high temperature heat source, chemical reaction takes place and generates silicon dioxide microparticle in the silicon tetrachloride G﹠O in enough thermal environments, deposits on the target surface and further vitrifying and form the quartz glass block of required quality.
No hydrogen flame passes produces by the plasma radio-frequency generator.The generation of high frequency plasma is the high-frequency current that produces the 4M hertz by AC transformer to step-up transformer then by triode self-sustained oscillation, in light fixture, pass to specific air-flow then, thereby produce the plasma arc body, arc body center top temperature can reach about 10000K, and arc body periphery can reach about 2000～4000K.Among the present invention, require the plasma arc body length at 20～40cm, arc body terminal temperature is at 2000～3000 ℃, and requires the plasma jet continous-stable, to guarantee the stable of technological process.The present invention can select any plasma generator that satisfies above-mentioned condition, the high-frequency plasma generator that preferred Liaoning Electronic Equipment Factory produces.
The present invention utilizes high frequency plasma as thermal source direct production silica glass.Its reaction formula is:
The production of chemical reaction and silica glass is finished existing quartzy production in the stove, and referring to shown in Figure 2, the plasma arc body is introduced into quartzy production in the stove as thermal source, makes the vertical about 5～20cm of deposition target surface that places in the arc body end-to-end distance stove; Treat that the target surface temperature rises to more than 1600 ℃, introduce and use O
2The SiCl that carries
4(material) gas stream adds to apart from about 5～10cm place, target surface top air-flow; O
2And SiCl
4Reaction at high temperature obtains nano level SiO
2Particulate directly is deposited on the target surface under the effect of air-flow and gravity, and forms silica glass of the present invention through the vitrified process at target surface.
In the production process, reasonably the flow control of cutting mode and gas stream also is the successful key of invention.During blanking of the present invention only with O
2As carrier gas, do not introduce other components, gas flow is controlled at 0.08～0.20m when feeding intake in producing stove
3/ h.Following method and apparatus can be used as an embodiment of control blanking air flow rate.
Referring to Fig. 3, blanking device comprises bubbling device 1, gasification installation 2 and flow rate control device 3, and wherein, bubbling device 1 is made up of first water bath 11 and the bubbling bottle 12 that is placed in one, the bath temperature of first water bath 11 is controlled at about 40 ℃, adds SiCl in the bubbling bottle 12
4Raw material, first inlet pipe 13 that has variable valve 15 is led to the bottom of bubbling bottle 12, and other has one first escape pipe 14 to draw from the top of bubbling bottle 12, leads in the gasification installation 2; Gasification installation 2 is made up of second water bath 21 and gasification bottle 22, the bath temperature of second water bath 21 is controlled at about 80 ℃, the bottom that first escape pipe 14 of drawing from bubbling bottle 12 tops feeds gasification bottle 22 forms second inlet pipe 23, second escape pipe 24 is established on top at gasification bottle 22, and this second escape pipe 24 feeds in the flow rate control device 3; Flow rate control device 3 is a control bottle, second escape pipe 24 of drawing from gasification bottle 22 tops feeds this control bottle and forms the 3rd inlet pipe 33, introduce a carrier gas inlet pipe 36 from source of oxygen in addition, installing flowrate control valve 35 on this carrier gas inlet pipe 36, the exit end of flow control bottle 3 is established the 3rd escape pipe 34, the three escape pipes 34 and is fed quartzy production in the stove.During use, from first inlet pipe 13, feed purity oxygen earlier, by variable valve 15 control band material O
2Flow is at 0.06～0.15m
3/ h, oxygen feeds the liquid Si Cl in the bubbling bottle 12
4Middle beginning bubbling carries SiCl
4Enter gasification bottle 22 from first escape pipe 14, the gasification back enters in the flow control bottle 3 by second escape pipe 24 in gasification bottle 22; Feed pure oxygen gas in another inlet pipe 36 of flow control bottle 3, by the auxiliary O of flowrate control valve 35 controls
2Flow is at 0.08～0.20m
3/ h, band material O
2, SiCl
4With auxiliary O
2The mixing back is introduced into to produce in the stove by the flow of setting by the 3rd escape pipe 34 and participates in chemical reaction in flow control bottle 3.
Add SiCl owing to simple with adding the oxygen belt material in the operation
4, its flow velocity is not enough to the SiO after pyroreaction
2Guide to target surface and deposit vitreous, so increase auxiliary O
2Inlet pipe increases the blanking flow velocity to guarantee reaction product SiO under the high temperature
2Can be in target surface deposition and vitreous smoothly.SiCl
4Be to introduce by bubbling bottle, vaporization bottle, drawing material by two-stage also is in order to guarantee the uniform and stable of blanking, thereby guarantees the stable of technology.
Silica glass production process of the present invention can adopt following operation: the power supply of connecting high-frequency plasma generator; wait to boost to logical argon gas about 8kv by the operation instructions of high-frequency plasma generator; connect shielding gas after the starting the arc at once; argon gas switches to working gas (oxygen), and the working gas flow is 2～6m
3/ h, shield gas flow rate are 4～10m
3/ h; Monitoring deposition targets surface temperature, when the surface temperature that sticks together rises to more than 1600 ℃ (arc body temperature degree is at 2000～3000 ℃), accommodation zone material O
2Flow and auxiliary O
2Flow (band material O
2Flow is at 0.12m
3About/h, auxiliary O
2Flow is at 0.16m
3About/h), the beginning blanking continues 20～40 hours, closes blanking channel, cuts off the power supply of high-frequency plasma generator, is cooled to room temperature naturally, takes out the glass that is deposited on the target surface and promptly obtains silica glass of the present invention.
The silica glass diameter that this example obtains can reach 15 centimetres, and thickness reaches 5 centimetres, and this silica glass entire body is sparkling and crystal-clear transparent, and the quality homogeneous only has indivedual bubbles at the edge, and main part does not have bubble.Carry out following performance test with this silica glass:
One, purity test
Method: atomic absorption and atomic emissions, adopt the GB/T3284-1993 standard
Result: referring to table 1.
| Element | Analytical results (ppm) |
| Aluminium | 0.25 |
| Calcium | 0.23 |
| Magnesium | 0.09 |
| Titanium | 0.02 |
| Sodium | 0.03 |
| Potassium | 0.04 |
| Iron | 0.17 |
| Copper | 0.08 |
| Cobalt | 0.01 |
| Manganese | 0.01 |
| Nickel | 0.01 |
| Lithium | 0.01 |
| Boron | 0.01 |
| Cl | 200 |
Numerical value can see that content of impurities is lower than 1ppm in the silica glass of the present invention from table, and total content is 0.92ppm, Cl content 200ppm.
Two, glass optical performance test
Method: specimen is: (10 * 30 * 50mm), 10mm is a thickness to the polishing both surfaces silica glass
Testing tool is: UV, visible light near infrared spectrometer, working conditions are 20 ℃ ± 5 ℃.
Result: Fig. 4-1 detects collection of illustrative plates for silica glass transmitance of the present invention, and Fig. 4-2 is that four kinds of (I～IV class) silica glass transmitances detect the contrast collection of illustrative plates.
The result can see among Fig. 4-1, and sample of the present invention does not all have tangible absorption peak at 200～2700nm place, illustrates near ultraviolet-visible light-near infrared transmitance all to have surpassed 80%, sees through the light wavelength scope at 0.2～3.2 μ m.
In addition, from contrast spectrogram (Fig. 4-2) as can be seen, preceding I, II class sample is on the low side in the transmitance at ultraviolet place, and III class sample 1480,2200, all there is the hydroxyl absorption peak at the 2730nm place, even if sample of the present invention also only has a very little absorption peak at the 2730nm place, illustrate that hydroxy radical content seldom (can reach below the 5ppm) in this sample.
Hydroxy radical content of the present invention, available following experimental formula estimation:
Hydroxy radical content (ppm)=96.5 ÷ thickness of sample (cm) * log (vertex transmitance ÷ lower-most point transmitance)
Wherein: transmitance is the maximum and the Schwellenwert of 2730nm place absorption peak.
Calculate with above-mentioned formula, the hydroxy radical content in the sample of the present invention is about 5ppm, and calculates with same formula, and I quartz-like glass hydroxy radical content is at 30～100ppm, and the II class is at 180～250ppm, and the III class is more than 1000ppm.
The present invention high-purity alpha-SiC l
4Repeat the preparation process and the testing process of above-mentioned silica glass as raw material, wherein the arc body length of plasma arc is controlled to be 25cm, and arc body terminal temperature is 2000 ℃, and band material oxygen flow is controlled at 0.08m
3/ h, the auxiliary oxygen flow is controlled at 0.12m
3/ h.The silica glass that the result is more optimized, and resulting silica glass hydroxy radical content can reach below the 2ppm.
The present invention also just is the pure of it with plasma body as the major cause of thermal source, does not have the introducing of introduced contaminants substantially.And the method for oxyhydrogen flame synthetic quartz glass in the past, its reaction formula is:
Can introduce a large amount of OH with oxyhydrogen flame as the production process of thermal source
-(hydroxy radical content generally can reach 1000ppm), thereby cause the glass of production very big absorption peak to be arranged at 2730nm, and the silica glass hydroxy radical content that the present invention produces as thermal source with plasma body is at 5ppm even lower, therefore its spectral transmittance at 2730nm is higher, simultaneously because its purity fundamental sum oxyhydrogen flame is synthetic similar, therefore in that performance is preferably all arranged aspect the full spectral transmittance, satisfy the requirement that is used for high quality quartz pendulous reed and special optical material.
Claims (4)
1, a kind of method of high frequency plasma gas phase synthetic quartz glass, comprise that the plasma arc introducing that will continue is as the thermal source of producing stove, oxygen and silicon tetrachloride gas mixed and, generate silicon dioxide microparticle and also be deposited into the step that forms glass on the target surface with the continual and steady flow target surface top in the stove of putting into production; Wherein, the numerical value of the arc body length of described plasma arc between 20～40cm, the numerical value of arc body terminal temperature between 2000～3000 ℃, and in the entire method temperature fluctuation range within 5%; Oxygen and silicon tetrachloride mixed gas flow in the described stove that puts into production are 0.08～0.20m
3A numerical value the between/h, and in the whole input process flow rate fluctuation scope within 5%.
2, method according to claim 1 is characterized in that, oxygen and silicon tetrachloride gas blended concrete steps are:
1) will feed the bubbling bottle bottom that Sheng is loaded with the liquid silicon tetrachloride with material oxygen, the bubbling bottle keeps 40 ℃ temperature;
2) gas that will collect from bubbling bottle top feeds a gasification bottle bottom, and the gasification bottle keeps 80 ℃ temperature;
3) gas that will collect from gasification bottle top feeds flow control bottle, simultaneously in this flow control bottle, feed auxiliary oxygen, with flow valve control auxiliary oxygen flow, draw oxygen and the silicon tetrachloride mixed gas stove that puts into production from the outlet of this flow control bottle then.
3, method according to claim 2 is characterized in that, described band material oxygen flow is controlled at 0.06～0.15m
3/ h, the auxiliary oxygen flow is controlled at 0.08～0.20m
3A numerical value the between/h.
4, method according to claim 3 is characterized in that, concrete controlled variable is: the arc body length of plasma arc is 25cm, and arc body terminal temperature is 2000 ℃, and band material oxygen flow is controlled at 0.08m
3/ h, the auxiliary oxygen flow is controlled at 0.12m
3/ h.
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| CNB2005100766134A CN1314608C (en) | 2005-06-10 | 2005-06-10 | High-frequency plasma vapor phase synthesis method for quartz glass |
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|---|---|---|---|
| CNB2005100766134A CN1314608C (en) | 2005-06-10 | 2005-06-10 | High-frequency plasma vapor phase synthesis method for quartz glass |
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| CN1314608C true CN1314608C (en) | 2007-05-09 |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102092954B (en) * | 2010-11-09 | 2012-09-05 | 杭州电子科技大学 | Quartz pendulum sheet matrix arranged chemical corrosion device and method |
| CN105502897B (en) * | 2016-01-12 | 2018-08-24 | 中国建筑材料科学研究总院 | The preparation method of super pure silica 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 |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0247415B2 (en) * | 1984-07-03 | 1990-10-19 | Hitachi Cable | HIKARIFUAIBABOZAINOSEIZOHOHO |
| CN1252778A (en) * | 1997-12-19 | 2000-05-10 | 纤维管有限公司 | Method of making a tubular member for optical fiber production using plasma outside vapor deposition |
| DE10054270A1 (en) * | 2000-11-02 | 2002-05-16 | Schott Glas | Production of photomask substrates, used for semiconductor lithography, comprises plasma-promoted deposition of quartz glass from reaction gases, doping quartz glass with hydrogen, and processing into photomask substrate plates |
| CN1396131A (en) * | 2002-07-09 | 2003-02-12 | 长飞光纤光缆有限公司 | Process for preparing quartz optical fibre core |
| CN1458097A (en) * | 2003-04-23 | 2003-11-26 | 中国建筑材料科学研究院 | Process for synthesizing guartz glass by vertical silicon tetrachloride vapor deposition |
| CN1490267A (en) * | 2003-07-14 | 2004-04-21 | 烽火通信科技股份有限公司 | Method for manufacturing rare earth extended fibre-optical prefabricated bar |
-
2005
- 2005-06-10 CN CNB2005100766134A patent/CN1314608C/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0247415B2 (en) * | 1984-07-03 | 1990-10-19 | Hitachi Cable | HIKARIFUAIBABOZAINOSEIZOHOHO |
| CN1252778A (en) * | 1997-12-19 | 2000-05-10 | 纤维管有限公司 | Method of making a tubular member for optical fiber production using plasma outside vapor deposition |
| DE10054270A1 (en) * | 2000-11-02 | 2002-05-16 | Schott Glas | Production of photomask substrates, used for semiconductor lithography, comprises plasma-promoted deposition of quartz glass from reaction gases, doping quartz glass with hydrogen, and processing into photomask substrate plates |
| CN1396131A (en) * | 2002-07-09 | 2003-02-12 | 长飞光纤光缆有限公司 | Process for preparing quartz optical fibre core |
| CN1458097A (en) * | 2003-04-23 | 2003-11-26 | 中国建筑材料科学研究院 | Process for synthesizing guartz glass by vertical silicon tetrachloride vapor deposition |
| CN1490267A (en) * | 2003-07-14 | 2004-04-21 | 烽火通信科技股份有限公司 | Method for manufacturing rare earth extended fibre-optical prefabricated bar |
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