CN104326646B - Quartz glass of Doped with Titanium and preparation method thereof, preparation facilities - Google Patents

Quartz glass of Doped with Titanium and preparation method thereof, preparation facilities Download PDF

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Publication number
CN104326646B
CN104326646B CN201410571933.6A CN201410571933A CN104326646B CN 104326646 B CN104326646 B CN 104326646B CN 201410571933 A CN201410571933 A CN 201410571933A CN 104326646 B CN104326646 B CN 104326646B
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quartz glass
burner
preparation
titanium
control system
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CN104326646A (en
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邵竹锋
饶传东
向在奎
符博
聂兰舰
王宏杰
王慧
王蕾
刘飞翔
王玉芬
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China Building Materials Academy CBMA
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    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C3/00—Glass compositions
    • C03C3/04—Glass compositions containing silica
    • C03C3/06—Glass compositions containing silica with more than 90% silica by weight, e.g. quartz
    • 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
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2201/00—Glass compositions
    • C03C2201/06—Doped silica-based glasses
    • C03C2201/30—Doped silica-based glasses containing metals
    • C03C2201/40—Doped silica-based glasses containing metals containing transition metals other than rare earth metals, e.g. Zr, Nb, Ta or Zn
    • C03C2201/42—Doped silica-based glasses containing metals containing transition metals other than rare earth metals, e.g. Zr, Nb, Ta or Zn containing titanium
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2203/00—Production processes
    • C03C2203/40—Gas-phase processes
    • C03C2203/42—Gas-phase processes using silicon halides as starting materials
    • C03C2203/44—Gas-phase processes using silicon halides as starting materials chlorine containing

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Glass Melting And Manufacturing (AREA)
  • Glass Compositions (AREA)

Abstract

The invention discloses a kind of quartz glass of Doped with Titanium and preparation method thereof, preparation facilities, the preparation method includes：During silicon-containing material and titaniferous materials are put into using oxyhydrogen flame as the burner of the reaction energy, low-expansion quartz glass stone roller is prepared using vertical chemical vapour deposition technique, quartz glass stone roller is fitted into homogenizing in high temperature homogenizing furnace to handle, then passes through the quartz glass that cold working prepares Doped with Titanium.The preparation facilities includes, silicon tetrachloride control system and titanium tetrachloride control system connect mixing bottle respectively, mixing bottle hydrogen control system and oxygen control system connect burner respectively, burner is located in the burner hearth of combustion furnace, basic rod one end is provided with pallet, and pallet is located in burner hearth, the basic rod other end connection traversing mechanism, rotating mechanism connects jacking system, burner hearth connection chimney.The present invention can be accurately controlled doping quantity, therefore, it is possible to the coefficient of expansion of accurate control quartz glass.

Description

Quartz glass of Doped with Titanium and preparation method thereof, preparation facilities
Technical field
The present invention relates to a kind of low-expansion quartz glass of large scale, more particularly to a kind of quartz glass of Doped with Titanium And preparation method thereof, preparation facilities.
Background technology
In recent years, due to the specific demand of different field, the constituent of quartz glass is also constantly changing.In stone Adulterate different types of rare earth or metallic element in the basic constituent silica of English glass, thus it is possible to vary quartz glass exists Characteristic in terms of the coefficient of expansion, intensity, stability, light transmittance, resistance to irradiation.Reflected light is required in Aero-Space and astronomical field Learning element both has very high weight reduction rate, has extremely low thermal coefficient of expansion again to ensure optical element energy in temperature fluctuation Enough keep its surface figure accuracy.Large scale low-expansion quartz glass both has good weldability energy, can make cellular light Quantizing structure, while there is extremely low thermal coefficient of expansion again, and very high resistance to deformation intensity, it is the desired light for reflecting optical field Learn material.
At present, the preparation technology of domestic large scale quartz glass has four kinds, but quartz glass prepared by these techniques The coefficient of expansion is 10-7/ DEG C, phenomenon can be burst after lightweight is welded, and thermal stability is poor.
The content of the invention
In order to solve problem of the prior art, uniform doping is realized the embodiments of the invention provide one kind, doping is controllable Doped with Titanium quartz glass preparation method.
To achieve these goals, the present invention is adopted the technical scheme that：
A kind of preparation method of the quartz glass of Doped with Titanium, comprises the following steps：
During silicon-containing material and titaniferous materials are put into using oxyhydrogen flame as the burner of the reaction energy, using vertical chemical gas Phase sedimentation prepares low-expansion quartz glass stone roller, and quartz glass stone roller is fitted into homogenizing in high temperature homogenizing furnace is handled, then is added through supercooling Work prepares the quartz glass of Doped with Titanium.
Further, following steps are specifically included：
(1) hydrogen and oxygen are passed through in burner, combustion reaction forms redox reaction atmosphere；
(2) by silicon-containing material and the titaniferous materials vaporization under Material control respectively, after uniform mixing device, Is reacted under the drive of material containing gas in feeding burner, the quality for controlling titaniferous materials be silicon-containing material quality 3%~ 10%；The SiO generated after reaction2And TiO2Particle is deposited on the pallet in combustion furnace, at a high temperature of 1300~2000 DEG C by Layer sintering forms low-expansion coefficient quartz glass stone roller；Pallet is under the rotation of basic rod, descending at slow speed, and quartz glass stone roller is gradually long Greatly；
(3) quartz glass stone roller is ultimately formed into the quartz glass of Doped with Titanium by homogenizing and follow-up cold working.
The silicon-containing material is silicon tetrachloride, and/or, the titaniferous materials are titanium tetrachloride.
The speed of the deposition is 100~500 Grams Per Hours.
In the high temperature homogenizing furnace, programming rate is 200~700 DEG C/h, and maximum temperature is 1700~1900 DEG C；Institute High temperature homogenizing furnace is stated for closed structure, vacuum or insufflation gas are kept during work in stove, the gas is inert gas or gone back Originality gas.
The flow of the silicon-containing material is 800~1500g/h, and the flow of the titaniferous materials is 24~150g/h.
The present invention also provides a kind of quartz glass of Doped with Titanium, is prepared according to above-mentioned preparation method.
The present invention provides a kind of preparation facilities of the quartz glass of Doped with Titanium, including hydrogen control system, Oxygen control again System, silicon tetrachloride control system, titanium tetrachloride control system and basic rod, the silicon tetrachloride control system and titanium tetrachloride Control system connects mixing bottle respectively, and the mixing bottle connects burner, the hydrogen control system and oxygen control system point Burner is not connected, and the burner is located in the burner hearth of combustion furnace, and described basic rod one end is provided with pallet, and the pallet is located at In the burner hearth, the basic rod other end connection traversing mechanism, the rotating mechanism connects jacking system, the burner hearth connection Chimney.
The burner is that multilayer wraps up tubular structure, and the material of described burner is exotic material.
The combustion furnace is vertical shaft furnace, and the burner is positioned over the position more than middle part of burner hearth, the burning The port of device is against the position of burner hearth inner pallet.
Compared with prior art, the beneficial effects of the invention are as follows：
A certain amount of titanium dioxide of the invention that adulterated in quartz glass can substantially reduce the coefficient of expansion of quartz glass, And titanium dioxide can be uniformly mixed in quartz glass substrate, and can accurately controlled using vertical chemical vapour deposition technique System doping quantity, therefore, it is possible to the coefficient of expansion of accurate control quartz glass.
Brief description of the drawings
Technical scheme in order to illustrate the embodiments of the present invention more clearly, makes required in being described below to embodiment Accompanying drawing is briefly described, it should be apparent that, drawings in the following description are only some embodiments of the present invention, for For those of ordinary skill in the art, on the premise of not paying creative work, other can also be obtained according to these accompanying drawings Accompanying drawing.
Fig. 1 is the structural representation of the preparation facilities of the quartz glass for the Doped with Titanium that the present invention is provided.
In figure:1 hydrogen control system, 2 oxygen control systems, 3 silicon tetrachloride control systems, 4 titanium tetrachloride control systems, 5 mixing bottles, 6 burners, 7 burner hearths, 8 low-expansion quartz glasses stone roller, 9 chimneys, 10 jacking systems, 11 basic rods, 12 rotating mechanisms.
Embodiment
To make the object, technical solutions and advantages of the present invention clearer, below in conjunction with accompanying drawing to embodiment party of the present invention Formula is described in further detail.
Referring to Fig. 1, a kind of preparation facilities of the quartz glass of Doped with Titanium, including hydrogen control system 1, oxygen control system 2nd, silicon tetrachloride control system 3, titanium tetrachloride control system 4 and basic rod 11, silicon tetrachloride control system 3 and titanium tetrachloride control System 4 processed connects mixing bottle 5 respectively, and mixing bottle 5 connects burner 6, and hydrogen control system 1 and oxygen control system 2 connect respectively Burner 6 is connect, burner 6 is located in the burner hearth 7 of combustion furnace, it is preferable that burner 6 is positioned over the position more than middle part of burner hearth 7, The port of burner 6 is against the position of the inner pallet 13 of burner hearth 7, and the one end of basic rod 11 is provided with pallet 13, and pallet 13 is located at burner hearth 7 It is interior, the other end connection traversing mechanism 12 of basic rod 11, the connection jacking system 10 of rotating mechanism 12, the connection chimney 9 of burner hearth 7.
Preferably, burner 6 is that multilayer wraps up tubular structure, and the material of burner 6 is exotic material.It is preferred that quartzy glass Glass.
The combustion furnace of the present invention is vertical shaft furnace.Suitable for chemical vapor deposition method.
Using the device of the present invention, adulterate a certain amount of titanium dioxide in quartz glass substrate, uniform doping, doping Controllable, quartz glass prepared by the present invention thermal expansion change within the scope of larger temperature is smaller, under the conditions of suitable temperature very Zero thermal expansion can extremely be realized.
The present invention also provides a kind of preparation method of the quartz glass of Doped with Titanium, comprises the following steps：
During silicon-containing material and titaniferous materials are put into using oxyhydrogen flame as the burner of the reaction energy, using vertical chemical gas Phase sedimentation prepares low-expansion quartz glass stone roller, and quartz glass stone roller is fitted into homogenizing in high temperature homogenizing furnace is handled, then is added through supercooling Work prepares the quartz glass of Doped with Titanium.
In order to prevent internal flaw from influenceing the physical property of final finished, also for production cost is saved, the present invention is provided Be used for prepare titania-doped quartz glass technique be chemical vapor deposition method.
Further, following steps are specifically included：
(1) hydrogen and oxygen are passed through in burner, combustion reaction forms redox reaction atmosphere；
(2) by silicon-containing material and the titaniferous materials vaporization under Material control respectively, after uniform mixing device, Is reacted under the drive of material containing gas in feeding burner, the quality for controlling titaniferous materials be silicon-containing material quality 3%~ 10%；The SiO generated after reaction2And TiO2Particle is deposited on the pallet in combustion furnace, at a high temperature of 1300~2000 DEG C by Layer sintering forms low-expansion coefficient quartz glass stone roller；Pallet is under the rotation of basic rod, descending at slow speed, and quartz glass stone roller is gradually long Greatly；
(3) quartz glass stone roller is ultimately formed into the quartzy glass of the Doped with Titanium of certain specification by homogenizing and follow-up cold working Glass.
The silicon-containing material is silicon tetrachloride, and/or, the titaniferous materials are titanium tetrachloride.
The speed of the deposition is 100~500 Grams Per Hours, preferably 300 Grams Per Hours.
In the high temperature homogenizing furnace, programming rate is 200~700 DEG C/h, and preferably 500 DEG C/h, maximum temperature is 1700~1900 DEG C, preferably 1800 DEG C；The high temperature homogenizing furnace is closed structure, keeps vacuum in stove during work or is filled with gas Body, the gas is inert gas or reducibility gas.
The flow of the silicon-containing material is 800~1500g/h, preferably 1200g/h, and the flow of the titaniferous materials is tetrachloro The 3%~10% of SiClx flow, preferably 7%.
The material containing gas is one kind in hydrogen, oxygen, argon gas, or it is other do not enter the gas of glass structure, and contain Silicon raw material material containing gas flow is 2-6L/min, and the flow of the titaniferous materials is 24~150g/h.
The present invention also provides a kind of large scale low-expansion coefficient quartz glass, the i.e. quartz glass of Doped with Titanium, existing to overcome The problem of some quartz glass coefficients of expansion is high.Prepared according to above-mentioned preparation method, the main component of the quartz glass Including TiO2And SiO2, TiO2Weight/mass percentage composition be SiO23%~10%, its coefficient of expansion be 10-8/ DEG C, even more It is low.The quartz glass can be welded into cellular lightweight structure, can be worked into very high optical flat degree, and in optics Stability is high in system, will not change its surface face shape with the fluctuation of temperature.Its preparation method is main with silicon tetrachloride For raw material, low-expansion quartz glass of Doped with Titanium is manufactured using chemical vapor deposition method (CVD).The present invention is provided Quartz glass relatively low thermal expansion can be achieved within the scope of one relatively wide in range temperature, or even under suitable temperature conditionss Zero thermal expansion can be achieved.Available for high-tech areas such as Aero-Space, optics, communications.The quartzy glass of the large scale low bulk of the present invention Glass, its profile can be the shape of any requirement, and its maximum gauge can reach 2 meters.Its coefficient of expansion is better than 5 × 10-7/℃。
The technological reaction principle of the present invention：
1) hydrogen and oxygen burn in the burner generation water vapour after it is anti-with gaseous silicon in burner tremie pipe Silica micro-particle should be generated；
2) hydrogen and oxygen burn in the burner generation vapor after it is anti-with gaseous titanium tetrachloride in burner tremie pipe Titanium dioxide microparticle should be generated；
3) silica and titanium dioxide microparticle are reunited in flame, are grown to serve as bigger particle, and in flame Moved under drive towards depositing base.
4) silica and titanium dioxide granule reach fused silica glass matrix and are adsorbed, in the effect of thermal-flame Issue heat migration.Meanwhile, the gas molecule being mingled with particle diffuses to surface, leaves crystallizing field, is discharged with air-flow.
Below by specific embodiment, the present invention is described further：
Embodiment 1 (referring to Fig. 1)
1) silicon tetrachloride control system 3：(purity reaches high purity silicon tetrachloride material liquid in silicon tetrachloride head tank More than 99.999%), tetrachloro is imported via binder gas (high pure nitrogen being used in the present embodiment, purity is up to more than 99.999%) In SiClx vaporizes kettle, because the boiling point of silicon tetrachloride material liquid is 57.6 DEG C, the temperature of vaporizes kettle is adjusted to 40~50 DEG C in advance, this Embodiment selects 45 DEG C, and material containing gas (uses high-purity argon gas, purity is up to more than 99.999%, material containing gas stream in the present embodiment Measure as 4L/min) flow through drier remove vapor after enter vaporizes kettle in, and kettle it is atomization after silicon tetrachloride vapor then by Material containing gas be carried through after mixing bottle 5 enter oxyhydrogen flame burner 6, the silicon tetrachloride flow carried out be 800~ 1500g/h, preferably 1200g/h, silicon tetrachloride gas and the mixed gas that material containing gas is constituted after vaporizing are silicon tetrachloride Unstripped gas.
2) titanium tetrachloride control system 4：(purity reaches high-purity titanium tetrachloride material liquid in titanium tetrachloride head tank More than 99.99%), (high pure nitrogen is used in the present embodiment, purity is up to more than 99.999%, material containing gas via binder gas Flow is 0.2L/min) import in titanium tetrachloride vaporizes kettle, because the boiling point of titanium tetrachloride material liquid is 136.4 DEG C, it will vaporize The temperature of kettle is adjusted to 110~125 DEG C in advance, and the present embodiment selects 120 DEG C, and material containing gas is (pure using high-purity argon gas in the present embodiment Degree is up to more than 99.999%) flow through drier and remove and enter after vapor in vaporizes kettle, and the titanium tetrachloride after kettle is atomization steams Vapour is then carried through after mixing bottle 5 entering oxyhydrogen flame burner 6 by material containing gas, and the titanium tetrachloride flow carried out is 24- 150g/h, the present embodiment selects 90g/h, and the titanium tetrachloride gases after vaporizing are tetrachloro with the mixed gas that material containing gas is constituted Change titanium material gas.
3) hydrogen (purity up to more than 99.999%) and oxygen (purity is up to more than 99.999%) are respectively through hydrogen control Oxyhydrogen flame burner 6 is passed through after the flow control of system 1 and oxygen control system 2 simultaneously to be burnt, hydrogen flowing quantity control In 300L/min~500L/min and oxygen flux control in 100L/min~200L/min.The present embodiment selects hydrogen flowing quantity 400L/min and oxygen flow 150L/min, when oxyhydrogen flame temperature reaches 800~1300 DEG C, the present embodiment selects 1000 DEG C, silicon tetrachloride unstripped gas and titanium tetrachloride unstripped gas are reacted in burner hearth 7 simultaneously, and silica and dioxy are generated respectively Change titanium particle, mixed deposit is on the basic rod 11 in combustion furnace after high-temperature fusion, and the speed of deposition is 300 Grams Per Hours, Low-expansion quartz glass stone roller 8 is made by high temperature sintering again, the waste gas of generation is discharged by the negative pressure of chimney 9.Basic rod 11 exists Rotating speed is 200r/min~500r/min under control of rotating mechanism 12, and the present embodiment selects 400r/min, in descending mechanism 10 Control under reduction of speed be 0.2mm/h~0.5mm/h, the present embodiment selects 0.4mm/h.
4) the titania-doped quartz glass stone roller 8 that deposition is formed is cooled down after 32h, is taken out in combustion furnace, by quartz Glass stone roller is fitted into homogenizing in high temperature homogenizing furnace and handled, then passes through the component of quartz glass that cold working prepares Doped with Titanium, high temperature Homogenizing furnace is that vacuum is kept in closed structure, stove, and the programming rate of high temperature homogenizing furnace is 500 DEG C/h, is warming up to 1800 DEG C.
Embodiment 2
1) silicon tetrachloride unstripped gas is prepared：With the step 1 of embodiment 1) it is identical, except that：By the temperature of vaporizes kettle 40 DEG C are adjusted in advance, the silicon tetrachloride flow carried out is 1500g/h, material containing gas is hydrogen, and material containing gas flow is 2L/min.
2) titanium tetrachloride unstripped gas is prepared：With the step 2 of embodiment 1) it is identical, except that：The temperature of vaporizes kettle is pre- 125 DEG C are adjusted to, the titanium tetrachloride flow carried out is 24g/h, material containing gas is oxygen, and material containing gas flow is 0.2L/min.
3) generation silica and titanium dioxide granule：With the step 3 of embodiment 1) it is identical, except that：Hydrogen stream Amount control is in 500L/min and oxygen flux control in 200L/min；Oxyhydrogen flame temperature reaches 800 DEG C；Basic rod 11 is in rotation Rotating speed is 200r/min under control of mechanism 12, and reduction of speed is 0.5mm/h under control of descending mechanism 10, and the speed of deposition is 500 Grams Per Hours.
4) component of quartz glass is made：After the titania-doped quartz glass stone roller cooling 24h that deposition is formed, by burning Taken out in stove, quartz glass stone roller is fitted into homogenizing in high temperature homogenizing furnace is handled, then passes through the stone that cold working prepares Doped with Titanium English glass elements, high temperature homogenizing furnace is closed structure, keeps vacuum in stove, the programming rate of high temperature homogenizing furnace for 700 DEG C/it is small When, it is warming up to 1700 DEG C.
Embodiment 3
1) silicon tetrachloride unstripped gas is prepared：With the step 1 of embodiment 1) it is identical, except that：By the temperature of vaporizes kettle 50 DEG C are adjusted in advance, the silicon tetrachloride flow carried out is 800g/h, material containing gas flow is 6L/min；
2) titanium tetrachloride unstripped gas is prepared：With the step 2 of embodiment 1) it is identical, except that：The temperature of vaporizes kettle is pre- 110 DEG C are adjusted to, the titanium tetrachloride flow carried out is 150g/h, material containing gas flow is 0.18L/min；
3) generation silica and titanium dioxide granule：With the step 2 of embodiment 1) it is identical, except that：Hydrogen stream Amount control is in 300L/min and oxygen flux control in 100L/min；Oxyhydrogen flame temperature reaches 1300 DEG C；Basic rod 11 is in rotation Rotating speed is 500r/min under control of rotation mechanism 12, and reduction of speed is 0.2mm/h under control of descending mechanism 10, and the speed of deposition is 100 Grams Per Hours,.
4) component of quartz glass is made：After the titania-doped quartz glass stone roller cooling 36h that deposition is formed, by burning Taken out in stove, quartz glass stone roller is fitted into homogenizing in high temperature homogenizing furnace is handled, then passes through the stone that cold working prepares Doped with Titanium English glass elements, high temperature homogenizing furnace is closed structure, keeps vacuum in stove, the programming rate of high temperature homogenizing furnace for 200 DEG C/it is small When, it is warming up to 1900 DEG C.
The present invention uses above-mentioned technical proposal, and its advantage is as follows：
1) silicon tetrachloride and titanium tetrachloride adulterate under vapor state, can realize uniform doping, and doping is controllable.
2) low-expansion quartz glass is prepared using layer by layer deposition synthetic method, without defects such as macroscopical bubble, miscellaneous points.
3) vertical chemical gaseous phase depositing process is used, is conducive to preparing large scale quartz glass stone roller.
The foregoing is only presently preferred embodiments of the present invention, be not intended to limit the invention, it is all the present invention spirit and Within principle, any modification, equivalent substitution and improvements made etc. should be included in the scope of the protection.

Claims (8)

1. a kind of preparation method of the quartz glass of Doped with Titanium, it is characterised in that including：
In being put into after silicon-containing material and titaniferous materials uniformly mixing using oxyhydrogen flame as the burner of the reaction energy, using vertical Chemical vapour deposition technique prepares low-expansion quartz glass stone roller, and quartz glass stone roller is fitted into homogenizing in high temperature homogenizing furnace is handled, then is passed through Cross the quartz glass that cold working prepares Doped with Titanium；
It specifically includes following steps：
(1) hydrogen and oxygen are passed through in burner, combustion reaction forms redox reaction atmosphere；
(2) by silicon-containing material and the titaniferous materials vaporization under Material control respectively, after uniform mixing device, in material containing Reacted under the drive of gas in feeding burner, the quality for controlling titaniferous materials is the 3%~10% of silicon-containing material quality； The SiO generated after reaction2And TiO2Particle is deposited on the pallet in combustion furnace, is successively burnt at a high temperature of 1300~2000 DEG C Knot forms low-expansion coefficient quartz glass stone roller；Pallet 200r/min~500r/min of basic rod rotating speed rotation under, with 0.2mm/h~0.5mm/h speed descending at slow speed, quartz glass stone roller is gradually grown up；
(3) quartz glass stone roller is passed through in homogenizing and follow-up cold working, the high temperature homogenizing furnace, programming rate is 200~700 DEG C/h, 1700~1900 DEG C are warming up to, the quartz glass of Doped with Titanium is ultimately formed.
2. preparation method according to claim 1, it is characterised in that the silicon-containing material is silicon tetrachloride, the titaniferous Raw material is titanium tetrachloride.
3. preparation method according to claim 1, it is characterised in that the speed of the deposition is 100~500 Grams Per Hours.
4. preparation method according to claim 1, it is characterised in that the high temperature homogenizing furnace is closed structure, during work Vacuum or insufflation gas are kept in stove, the gas is inert gas or reducibility gas.
5. preparation method according to claim 1, it is characterised in that the flow of the silicon-containing material is 800~1500g/ H, the flow of the titaniferous materials is 24~150g/h.
6. preparation method according to claim 5, it is characterised in that the material containing gas is hydrogen, oxygen or argon gas, institute Silicon-containing material material containing gas flow is stated for 2-6L/min, the titaniferous materials material containing gas flow is silicon-containing material material containing gas stream The 3%~10% of amount.
7. preparation method according to claim 1, it is characterised in that the quartz glass preparation facilities of Doped with Titanium includes hydrogen Control system, oxygen control system, silicon tetrachloride control system, titanium tetrachloride control system and basic rod, the silicon tetrachloride Control system and titanium tetrachloride control system connect mixing bottle respectively, and the mixing bottle connects burner, the hydrogen control system System and oxygen control system connect burner respectively, and the burner is located in the burner hearth of vertical shaft furnace, the basic rod one End is provided with pallet, and the pallet is located in the burner hearth, and the basic rod other end connection traversing mechanism, the rotating mechanism connects Jacking system is connect, the burner hearth connects chimney.
8. preparation method according to claim 1, it is characterised in that the burner is that multilayer wraps up tubular structure, institute The material for the burner stated is exotic material；The burner is positioned over the position more than middle part of burner hearth, the burner Port against the position of burner hearth inner pallet.
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JP6241276B2 (en) * 2013-01-22 2017-12-06 信越化学工業株式会社 Method for manufacturing member for EUV lithography

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