CN106430947A - Preparation method of quartz glass and quartz glass - Google Patents
Preparation method of quartz glass and quartz glass Download PDFInfo
- Publication number
- CN106430947A CN106430947A CN201610809509.XA CN201610809509A CN106430947A CN 106430947 A CN106430947 A CN 106430947A CN 201610809509 A CN201610809509 A CN 201610809509A CN 106430947 A CN106430947 A CN 106430947A
- Authority
- CN
- China
- Prior art keywords
- quartz glass
- silicon dioxide
- doping
- dioxide powder
- chloride
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- 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
- 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
- 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
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
- C03C1/02—Pretreated ingredients
-
- 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
-
- 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
- C03C2201/34—Doped silica-based glasses containing metals containing rare earth metals
- C03C2201/3405—Scandium
-
- 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
- C03C2201/34—Doped silica-based glasses containing metals containing rare earth metals
- C03C2201/3411—Yttrium
-
- 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
- C03C2201/34—Doped silica-based glasses containing metals containing rare earth metals
- C03C2201/3417—Lanthanum
-
- 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
- C03C2201/34—Doped silica-based glasses containing metals containing rare earth metals
- C03C2201/36—Doped silica-based glasses containing metals containing rare earth metals containing rare earth metals and aluminium, e.g. Er-Al co-doped
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Glass Compositions (AREA)
Abstract
The invention relates to a preparation method of quartz glass and the quartz glass, relates to the technical field of quartz glass manufacturing, and mainly aims at improving corrosion resistance of a finished quartz glass product in hydrofluoric acid, fluorine F2 and other fluorine-containing environments. The method comprises the steps that a first doped compound and a second doped compound are dissolved through a solvent and mixed to form a doped mixed solution, wherein the first doped compound is an aluminum-containing compound; the doped mixed solution and water are mixed and then react with a silicon tetrachloride liquid phase to obtain doped silicon dioxide gel; the doped silicon dioxide gel is fired to be a finished quartz glass product through a firing technology, and the finished quartz glass product comprises Al2O3 formed through conversion after being fired with the doped mixed solution and at least one of ZrO2, Y2O3, La2O3, Sc2O3, ThO2, V2O5 and TiO2 which are formed through conversion after being fired with the doped mixed solution. Holes of a SiO2 tetrahedral network structure are filled with Al2O3, ZrO2, Y2O3, La2O3, Sc2O3, ThO2, V2O5 and TiO2 which are in a network intermediate or network outer body mode, and the quartz glass is resistant to acid corrosion.
Description
Technical field
The present invention relates to quartz glass manufacturing technology field, more particularly to a kind of preparation method of quartz glass and quartz
Glass.
Background technology
Quartz glass is the amorphous material using silicon dioxide as main component, and its microstructure is a kind of by titanium dioxide
The flat network of silicon four sides structure construction unit composition, because Si-O chemistry bond energy is very big, structure is very tight, so quartzy glass
Glass has the performance of uniqueness, such as high temperature resistant, that the coefficient of expansion is low, resistance to heat shocks, chemical stability high and electrical insulation capability is good etc. is excellent
Point.
Due to the special performance of quartz glass, it is that the irreplaceable ideal of semiconductor integrated circuit manufacture process is supporting auxiliary
Material, carves including in quartz glass tube, quartz glass plate, quartz glass ring, quartz glass plate, quartz glass flange, quartz glass
The devices such as groove boat, quartz glass rinse bath, are widely used.
At present, the preparation technology of quartz glass is broadly divided into direct method preparation technology and indirect method preparation technology, direct
In method preparation technology, quartz glass crystal, Silicon stone, silicon-containing compound are raw material, through high temperature melting or chemical vapor deposition
Become, melting method has electric smelting method (as vacuum electric fusion process), gas refining fusion process, high-frequency plasma fusion process, continuous melting method
Deng chemical vapour deposition technique has chemical vapor deposition CVD and PCVD PCVD etc..In indirect method preparation technology
In, with silicon-containing material, the silicon dioxide loosening body with a large amount of pores is obtained through low temperature chemical vapor deposition synthesis, then by two
Silicon oxide loosening body is sintered in normal pressure or direct draught, so that the gas in pore in silicon dioxide loosening body is discharged, thus obtaining
Obtain high-quality quartz glass finished product.
In realizing process of the present invention, inventor finds that in prior art, at least there are the following problems:
Si-O chemical bond is easy to be corroded by Fluohydric acid., through measuring and calculating, under hydrofluoric acid environment, all with Si-O chemical bond structure
The quartz glass becoming, the speed of corrosion has reached 150 μm/h, and the corrosion rate under hydrofluoric acid environment of existing quartz glass is relatively
Soon it is impossible to meet the application requirement of the semiconductor etching under hydrofluoric acid environment.
Content of the invention
In view of this, the present invention provides a kind of preparation method of quartz glass and quartz glass, and main purpose is to improve
Quartz glass finished product is in the corrosion resistance under hydrofluoric acid environment.
For reaching above-mentioned purpose, present invention generally provides following technical scheme:
On the one hand, embodiments of the invention provide a kind of preparation method of quartz glass, including:
First doped compound, the second doped compound dissolving are mixed to form by doping mixed solution, institute by lytic agent
Stating the first doped compound is aluminum contained compound, and described second doped compound includes compound containing Zr, compound containing Y, contains La
At least one in compound, compound containing Sc, compound containing Th, compound containing V, compound containing Ti;
By parts by volume L1Doping mixed solution, parts by volume L2Water mixing after, with Silicon chloride. liquid phase reactor obtain doping
Silica dioxide gel;
Described doping silicon dioxide gel is fired as quartz glass finished product, wherein, described quartz glass through burning process
Include in glass finished product and fire, through the Part I in described doping mixed solution, the Al being transformed2O3, through described doping mixing
Part II in solution fires the ZrO being transformed2、Y2O3、La2O3、Sc2O3、ThO2、V2O5、TiO2In at least one.
The object of the invention to solve the technical problems also can be applied to the following technical measures to achieve further.
Optionally, the preparation method of aforesaid quartz glass, wherein L1、L2Ratio 1:5~200.
Optionally, the preparation method of aforesaid quartz glass, the reaction rate of wherein said Silicon chloride. 20~
500ml/min.
Optionally, the preparation method of aforesaid quartz glass, wherein said by parts by volume L1Doping mixed solution, volume
Part L2Water mixing after, with Silicon chloride. liquid phase reactor obtain doping silicon dioxide gel, specifically include:
During Silicon chloride. is gradually added doping mixed solution and the mixed mixed liquor of water, and to described mixing
Liquid is stirred, and obtains doping silicon dioxide gel;Or,
Described by parts by volume L1Doping mixed solution, parts by volume L2Water mixing after, with Silicon chloride. liquid phase reactor obtain
Doping silicon dioxide gel, specifically includes:
After Silicon chloride., doping mixed solution and the mixed mixed liquor of water are atomized respectively, it is passed through in reative cell simultaneously
Carry out phase reaction and obtain doping silicon dioxide gel.
Optionally, the preparation method of aforesaid quartz glass, wherein said by parts by volume L1Doping mixed solution, volume
Part L2Water mixing after, with Silicon chloride. liquid phase reactor obtain doping silicon dioxide gel, specifically include:
Mixed doping mixed solution, the mixed liquor of water are obtained with Silicon chloride. liquid phase reactor under 10~100 degrees Celsius
Obtain doping silicon dioxide gel.
Optionally, the preparation method of aforesaid quartz glass, wherein said lytic agent includes mixing for dissolving described first
First lytic agent of heterocompound, described first lytic agent includes methanol, ethanol, acetic acid, hydrochloric acid, nitric acid, distilled water, hydrogen peroxide
In at least one;
Described first doped compound includes nitric hydrate aluminum Al (NO3)3·H2O, ANN aluminium nitrate nonahydrate Al (NO3)3·
9H2O, six hydration aluminium chlorate Al (ClO3)3·6H2O, aluminum chloride AlCl3In at least one.
Optionally, the preparation method of aforesaid quartz glass, wherein said lytic agent includes mixing for dissolving described second
Second lytic agent of heterocompound, described second lytic agent includes methanol, ethanol, acetic acid, hydrochloric acid, nitric acid, distilled water, hydrogen peroxide
In at least one;
Described compound containing Zr includes zirconium nitrate Zr (NO3)4·5H2O, zirconium carbonate ammonium ZrO (CO3)2(NH4)2·nH2O, carbon
Sour zirconium ZrOCO3·nH2O, eight water oxygen zirconium chloride ZrOCl2·8(H2O), zirconium chloride ZrCl4, eight water basic zirconium chloride ZrOCl2·
8H2At least one in O;
Described compound containing Y includes yttrium oxalate Y2(C2O4)3·10H2O, Yttrium trinitrate Y (NO3)3·6H2O, hydration Yttrium carbonate (Y2(CO3)3) Y2
(CO3)3·3H2O, Yttrium chloride(Y2Cl6) six water YCl3·6H2O, chloride hydrate yttrium YCl3H2At least one in O;
Described compound containing La includes lanthanum chloride LaCl3, Lanthanum trichloride hexahydrate. LaCl3·6H2O, Lanthanum (III) nitrate La (NO3)3·
6H2O, lanthanum carbonate La2(CO3)3.8H2At least one in O;
Described compound containing Sc includes six water Scium chloride (Sc4Cl12) ScCl3·6H2O, Scium chloride (Sc4Cl12) ScCl3, Scium nitrate(Sc(NO3)3) Sc (NO3)3·
3H2O, Scium nitrate(Sc(NO3)3) Sc (NO3)3·4H2O, Scium nitrate(Sc(NO3)3) Sc (NO3)3·5H2O, Scium nitrate(Sc(NO3)3) Sc (NO3)3·6H2O, six pasture and water acid scandium Sc2
(C2O4)3·6H2At least one in O;
Described compound containing Th includes thorium nitrate Th (NO3)4·4H2O, thhorium oxalate Th (C2O4)2, thorium tetrachloride ThCl4, high
Chloric acid thorium Th (ClO4)4In at least one;
Described compound containing V includes vanadium chloride VCl3, nitric acid vanadium acyl VO2NO3In at least one;
Described compound containing Ti includes Titanium Nitrate Ti (NO3)4.
Optionally, the preparation method of aforesaid quartz glass, wherein said Al2O3With SiO in described quartz glass finished product2
Weight than 0.5~10%;
ZrO2、Y2O3、La2O3、Sc2O3、ThO2、V2O5、TiO2With SiO in described quartz glass finished product2Weight ratio divide equally
Not 0.5~5%.
Optionally, the preparation method of aforesaid quartz glass, wherein said by described doping silicon dioxide gel through burning
Technique processed is fired as quartz glass finished product, specifically includes:
In T1At a temperature of to described doping silicon dioxide gel drying, obtain amorphous doping silicon dioxide powder, T1?
100~1000 degrees Celsius;
In T2At a temperature of to described doping silicon dioxide powder calcine, make described doping silicon dioxide powder be changed into crystallization
The doping silicon dioxide powder of state, T2At 1000~1500 degrees Celsius;
Described quartz glass finished product prepared by the doping silicon dioxide powder of crystallized state.
Optionally, the preparation method of aforesaid quartz glass, wherein said in T1At a temperature of to described doping silicon dioxide
Gel drying, specifically includes:
The hothouse that described doping silicon dioxide gel is dried is passed through atmosphere is dried, the wherein said atmosphere that is dried includes sky
Gas, oxygen O2, chlorine Cl2, dichloride oxygen sulfur SOCl2In at least one.
Optionally, the preparation method of aforesaid quartz glass, the doping silicon dioxide powder system of wherein said crystallized state
For going out described quartz glass finished product, specially:
Grinding is carried out to the doping silicon dioxide powder of described crystalline state, and to the doping silicon dioxide Powder screen after grinding
Point, obtain the silicon dioxide powder after screening, the silicon dioxide powder after screening is adopted melting technology, takes the photograph 1000~2500
Under family name's degree, it is melting into described quartz glass finished product.
Optionally, the preparation method of aforesaid quartz glass, the wherein said doping silicon dioxide powder to described crystalline state
Material carries out grinding, and to the doping silicon dioxide powder screening after grinding, obtains the silicon dioxide powder after screening, after sieving
Silicon dioxide powder adopt melting technology, under 1000~2500 degrees Celsius, be melting into described quartz glass finished product, specifically
For:
To the doping silicon dioxide powder screening after grinding, obtain the doping silicon dioxide powder in 20~200 mesh for the granule,
The doping silicon dioxide powder of 20~200 mesh is melting into described quartz glass finished product using vacuum electric process of smelting;Or,
To the doping silicon dioxide powder screening after grinding, obtain the doping silicon dioxide powder in 40~300 mesh for the granule,
The doping silicon dioxide powder of 40~300 mesh is melting into described quartz glass finished product using high-frequency plasma melting technology;
Or,
To the doping silicon dioxide powder screening after grinding, obtain the doping silicon dioxide powder in 40~300 mesh for the granule,
The doping silicon dioxide powder of 40~300 mesh is melting into described quartz glass finished product using gas refining melting technology;Or,
To the doping silicon dioxide powder screening after grinding, obtain the doping silicon dioxide powder in 40~300 mesh for the granule,
The doping silicon dioxide powder of 40~300 mesh is melting into described quartz glass finished product using continuous melting technique.
On the other hand, embodiments of the invention provide a kind of quartz glass, including:
Quartz glass finished product, described quartz glass finished product is prepared from using the preparation method of above-mentioned quartz glass,
Al2O3And ZrO2、Y2O3、La2O3、Sc2O3、ThO2、V2O5、TiO2In at least one with network intermediate or network outer body form
It is filled in SiO2In the hole of tetrahedral network structure.
The object of the invention to solve the technical problems also can be applied to the following technical measures to achieve further.
Optionally, aforesaid quartz glass, wherein said quartz glass finished product is quartz glass stone roller, quartz glass bar, stone
English glass tubing, quartz glass plate, quartz glass ring, quartz glass plate, quartz glass flange, quartz glass cutting boat or quartzy glass
Glass rinse bath.
The preparation method of quartz glass providing by technique scheme, technical solution of the present invention and quartz glass are at least
There are following advantages:
In technical scheme provided in an embodiment of the present invention, from aluminum contained compound as the first doped compound, select and contain
In Zr compound, compound containing Y, compound containing La, compound containing Sc, compound containing Th, compound containing V, compound containing Ti
First doped compound, the second doped compound dissolving, as the second doped compound, are mixed by least one by lytic agent
Form doping mixed solution, from parts by volume L1Doping mixed solution, parts by volume L2Water mixing after, with Silicon chloride. liquid phase
Reaction obtains doping silicon dioxide gel;Finally, described doping silicon dioxide gel is fired as quartzy glass through burning process
Glass finished product, wherein, include in described quartz glass finished product through described doping mixed solution in Part I fire conversion and
The Al becoming2O3, through described doping mixed solution in Part II fire the ZrO being transformed2、Y2O3、La2O3、Sc2O3、
ThO2、V2O5、TiO2In at least one.In the quartz glass finished product that the present invention provides, Al2O3、ZrO2、Y2O3、La2O3、
Sc2O3、ThO2、V2O5、TiO2SiO is filled in network intermediate or network outer body form2In the hole of tetrahedral network structure,
Make quartz glass of the present invention finer and close;Meanwhile, Al2O3、ZrO2、Y2O3、La2O3、Sc2O3、ThO2、V2O5、TiO2Resolution
Valency compares SiO2Height, that is, compared with SiO2Resistant to hydrogen fluoric acid corrosivity strong, it is possible to decrease quartz glass is in acid solution or sour gas
The corrosion rate of (as hydrofluoric acid environment), and then improve the acid-resisting corrosive nature of quartz glass.Improve quartz glass
Product are in Fluohydric acid. and fluorine gas F2Etc. the corrosion resistance under fluorine-containing environment.
Meanwhile, in technical scheme provided in an embodiment of the present invention, simultaneously as Al2O3Quartz glass is formed with network
Presented in body or network intermediate, can effectively adjust the network structure in quartz glass, it is to avoid be doped with ZrO2、Y2O3、
La2O3、Sc2O3、ThO2、V2O5Or TiO2Powder in melting process, crystallize or cluster occur.
Described above is only the general introduction of technical solution of the present invention, in order to better understand the technological means of the present invention,
And can be practiced according to the content of description, below with presently preferred embodiments of the present invention and coordinate accompanying drawing describe in detail as after.
Brief description
By reading the detailed description of hereafter preferred implementation, various other advantages and benefit are common for this area
Technical staff will be clear from understanding.Accompanying drawing is only used for illustrating the purpose of preferred implementation, and is not considered as to the present invention
Restriction.And in whole accompanying drawing, it is denoted by the same reference numerals identical part.In the accompanying drawings:
Fig. 1 is a kind of schematic flow sheet of the preparation method of quartz glass that embodiments of the invention provide;
Fig. 2 is the schematic flow sheet of the preparation method of a kind of specific quartz glass that embodiments of the invention provide.
Specific embodiment
For further illustrating that the present invention is to reach technological means and effect that predetermined goal of the invention is taken, below in conjunction with
Accompanying drawing and preferred embodiment, to according to the preparation method of quartz glass proposed by the present invention and its specific embodiment party of quartz glass
Formula, structure, feature and its effect, after describing in detail such as.In the following description, different " embodiment " or " embodiment " refers to
It is not necessarily same embodiment.Additionally, special characteristic in one or more embodiments, structure or feature can be by any suitable shapes
Formula combines.
The terms "and/or", only a kind of incidence relation of description affiliated partner, represents there may be three kinds of passes
System, for example, A and/or B, specifically it is interpreted as:A and B can be included simultaneously, can be with individualism A it is also possible to individualism
B, can possess above-mentioned three kinds of any one situations.
As shown in figure 1, a kind of preparation method of quartz glass of one embodiment of the present of invention proposition, it includes:
Step 10, by lytic agent by the first doped compound, second doped compound dissolving being mixed to form doping mixing
Solution, described first doped compound is aluminum contained compound, and described second doped compound includes compound containing Zr, chemical combination containing Y
At least one in thing, compound containing La, compound containing Sc, compound containing Th, compound containing V, compound containing Ti;
Wherein, lytic agent can be a kind of lytic agent, can simultaneously to the first doped compound, the second doped compound
Dissolved;Or, lytic agent can include two kinds of lytic agents, and a kind of lytic agent is used for dissolving the first doped compound, another
Plant lytic agent and be used for dissolving the second doped compound, forming doping mixed solution can be saline solution;In specific mixing, can be first right
First doped compound carries out dissolving and obtains the first mixed solution, the second doped compound is carried out with dissolving acquisition second mixing molten
Then first mixed solution, the second mixed solution are mixed to form doping mixed solution by liquid;Or, by the first doped compound,
Second doped compound first mixes, being dissolved to the first doped compound, the second doped compound using lytic agent simultaneously,
Form doping mixed solution;
Step 20, by parts by volume L1Doping mixed solution, parts by volume L2Water mixing after, with Silicon chloride. liquid phase reactor
Obtain doping silicon dioxide gel;
Specifically, water can adopt distilled water;Gel refers to:Colloidal particle in colloidal sol or solution or macromolecule are in certain bar
Interconnect under part, form space net structure, be filled with the liquid as disperse medium in structural void, such a is special
Dispersion claim, there is no a mobility, internal often contain big quantity of fluid.Wherein, L1、L2Ratio can 1:5~200.As 1:
20,1:50,1:100,1:150,1:160,1:180 etc..Wherein, liquid phase reactor can be reaction progressively, described Silicon chloride.
Reaction rate controls in 20~500ml/min.As 100ml/min, 200ml/min, 300ml/min, 400ml/min.
Step 30, described doping silicon dioxide gel is fired as quartz glass finished product through burning process, wherein, described
Include in quartz glass finished product and fire, through the Part I in described doping mixed solution, the Al being transformed2O3, mix through described
Part II in miscellaneous mixed solution fires the ZrO being transformed2、Y2O3、La2O3、Sc2O3、ThO2、V2O5、TiO2In at least
A kind of.
Wherein, Part I is the part that the first doped compound and lytic agent react generation, and Part II is the
Two doped compounds and lytic agent react the part generating, and what such as the second doped compound was selected is compound containing Zr, then warp
Part II in described doping mixed solution fires the ZrO being transformed2, what such as the second doped compound was selected is containing Yization
Compound, then through described doping mixed solution in Part II fire be transformed have Y2O3, the such as second doped compound choosing
It is compound containing Sc and compound containing Th, then fire through the Part II in described doping mixed solution and be transformed
There is Sc2O3And ThO2, what such as the second doped compound was selected is compound containing Y, then through second in described doping mixed solution
Part fire be transformed have Y2O3, etc..
In the prior art, as quartz glass reaction chamber using process due to constantly being corroded by Fluohydric acid., surface produce
White atomizing effect, and then affect radio frequency power source glow discharge;Reaction lumen wall be corroded position can drastically thinning occur little
Pinprick, or the pressure differential between vacuum and atmospheric pressure can not be born and cause explosion etc. because tube wall is corroded thinning, all
Vacuum leak can be led to, cause the radio frequency power source can not normal build-up of luminance;Quartz glass samples support is also can be progressively using process
Corroded by Fluohydric acid., and need to often change.Not only increase semiconductor manufacturing cost it is often more important that have impact on the etching of silicon chip
Efficiency, seriality and quality stability etc., thus integrated circuit etching process must use corrosion resistance silica glass material and
Product, improves the technical problem that its hydrofluoric acid corrosion resistance is that those skilled in the art are badly in need of solving.
In technical scheme provided in an embodiment of the present invention, from aluminum contained compound as the first doped compound, select and contain
In Zr compound, compound containing Y, compound containing La, compound containing Sc, compound containing Th, compound containing V, compound containing Ti
First doped compound, the second doped compound dissolving, as the second doped compound, are mixed by least one by lytic agent
Form doping mixed solution, from parts by volume L1Doping mixed solution, parts by volume L2Water mixing after, with Silicon chloride. liquid phase
Reaction obtains doping silicon dioxide gel;Finally, described doping silicon dioxide gel is fired as quartzy glass through burning process
Glass finished product, wherein, include in described quartz glass finished product through described doping mixed solution in Part I fire conversion and
The Al becoming2O3, through described doping mixed solution in Part II fire the ZrO being transformed2、Y2O3、La2O3、Sc2O3、
ThO2、V2O5、TiO2In at least one.In the quartz glass finished product that the present invention provides, Al2O3、ZrO2、Y2O3、La2O3、
Sc2O3、ThO2、V2O5、TiO2SiO is filled in network intermediate or network outer body form2In the hole of tetrahedral network structure,
Make quartz glass of the present invention finer and close;Meanwhile, Al2O3、ZrO2、Y2O3、La2O3、Sc2O3、ThO2、V2O5、TiO2Resolution
Valency compares SiO2Height, that is, compared with SiO2Resistant to hydrogen fluoric acid corrosivity strong, it is possible to decrease quartz glass is in acid solution or sour gas
The corrosion rate of (as hydrofluoric acid environment), and then improve the acid-resisting corrosive nature of quartz glass.
Meanwhile, in technical scheme provided in an embodiment of the present invention, simultaneously as Al2O3Quartz glass is formed with network
Presented in body or network intermediate, can effectively adjust the network structure in quartz glass, it is to avoid be doped with ZrO2、Y2O3、
La2O3、Sc2O3、ThO2、V2O5Or TiO2Powder in melting process, crystallize or cluster occur.
In the middle of specific enforcement, the liquid phase reactor with Silicon chloride., can be carried out by number of ways, specifically can be found in as
Under type, as shown in Fig. 2
First, the preparation method of above-mentioned quartz glass, described by parts by volume L1Doping mixed solution, parts by volume L2Water
After mixing, obtain doping silicon dioxide gel with Silicon chloride. liquid phase reactor, specifically include:
Step 21, during Silicon chloride. is gradually added doping mixed solution and the mixed mixed liquor of water, and right
Described mixed liquor is stirred, and obtains doping silicon dioxide gel.
In operation, can be by Silicon chloride. addition mixed liquor drop by drop, the speed of addition is directly proportional to stir speed (S.S.).
After treating that the reactant reaction in mixed liquor is finished by Silicon chloride., stop adding Silicon chloride..Wherein, the mode of stirring can be adopted
With manual stirring, or machine stirring.
Or,
2nd, the preparation method of above-mentioned quartz glass, described by parts by volume L1Doping mixed solution, parts by volume L2Water
After mixing, obtain doping silicon dioxide gel with Silicon chloride. liquid phase reactor, specifically include:
Step 22, Silicon chloride., doping mixed solution and the mixed mixed liquor of water are atomized respectively after, be passed through instead simultaneously
Answer and in room, carry out phase reaction acquisition doping silicon dioxide gel.
By the way of atomization, Silicon chloride. can be made fully to react with mixed liquor, and react contact comparatively fast, production efficiency is relatively
High.
Wherein, described by parts by volume L1Doping mixed solution, parts by volume L2Water mixing after, anti-with Silicon chloride. liquid phase
Doping silicon dioxide gel should be obtained, specifically include:
Mixed doping mixed solution, the mixed liquor of water are obtained with Silicon chloride. liquid phase reactor under 10~100 degrees Celsius
Obtain doping silicon dioxide gel.
That is, specific reaction environment can be carried out at normal temperatures it is not necessary to heat;Or reaction environment can be heated,
As being heated to 60~90 degrees Celsius, reaction rate can be improved.
In the specific preparation method implementing central, above-mentioned quartz glass,
Described lytic agent includes the first lytic agent for dissolving described first doped compound, described first lytic agent bag
Include methanol, ethanol, acetic acid, hydrochloric acid, nitric acid, distilled water, at least one in hydrogen peroxide;
Described first doped compound includes nitric hydrate aluminum Al (NO3)3·H2O, ANN aluminium nitrate nonahydrate Al (NO3)3·
9H2O, six hydration aluminium chlorate Al (ClO3)3·6H2O, aluminum chloride AlCl3In at least one.The first selected doped compound
It is mutually matched with the first lytic agent of described selection, so that the first doped compound is mutually dissolved with the first lytic agent.Described
First lytic agent, a described doped compound all can adopt single or multiple combination.
In the specific preparation method implementing central, above-mentioned quartz glass,
Described lytic agent includes the second lytic agent for dissolving described second doped compound, described second lytic agent bag
Include methanol, ethanol, acetic acid, hydrochloric acid, nitric acid, distilled water, at least one in hydrogen peroxide;
Described compound containing Zr includes zirconium nitrate Zr (NO3)4·5H2O, zirconium carbonate ammonium ZrO (CO3)2(NH4)2·nH2O, carbon
Sour zirconium ZrOCO3·nH2O, eight water oxygen zirconium chloride ZrOCl2·8(H2O), zirconium chloride ZrCl4, eight water basic zirconium chloride ZrOCl2·
8H2At least one in O;
Described compound containing Y includes yttrium oxalate Y2(C2O4)3·10H2O, Yttrium trinitrate Y (NO3)3·6H2O, hydration Yttrium carbonate (Y2(CO3)3) Y2
(CO3)3·3H2O, Yttrium chloride(Y2Cl6) six water YCl3·6H2O, chloride hydrate yttrium YCl3H2At least one in O;
Described compound containing La includes lanthanum chloride LaCl3, Lanthanum trichloride hexahydrate. LaCl3·6H2O, Lanthanum (III) nitrate La (NO3)3·
6H2O, lanthanum carbonate La2(CO3)3.8H2At least one in O;
Described compound containing Sc includes six water Scium chloride (Sc4Cl12) ScCl3·6H2O, Scium chloride (Sc4Cl12) ScCl3, Scium nitrate(Sc(NO3)3) Sc (NO3)3·
3H2O, Scium nitrate(Sc(NO3)3) Sc (NO3)3·4H2O, Scium nitrate(Sc(NO3)3) Sc (NO3)3·5H2O, Scium nitrate(Sc(NO3)3) Sc (NO3)3·6H2O, six pasture and water acid scandium Sc2
(C2O4)3·6H2At least one in O;
Described compound containing Th includes thorium nitrate Th (NO3)4·4H2O, thhorium oxalate Th (C2O4)2, thorium tetrachloride ThCl4, high
Chloric acid thorium Th (ClO4)4In at least one;
Described compound containing V includes vanadium chloride VCl3, nitric acid vanadium acyl VO2NO3In at least one;
Described compound containing Ti includes Titanium Nitrate Ti (NO3)4.
The second selected doped compound is mutually matched with the second lytic agent of described selection, makes the second doped compound
Can be mutually dissolved with the second lytic agent.Described second lytic agent, described two doped compounds all can be using single or multiple groups
Close.
In the quartz glass finished product that the preparation method through above-mentioned quartz glass is obtained, Al2O3And ZrO2、Y2O3、La2O3、
Sc2O3、ThO2、V2O5、TiO2In at least one shared proportion, determine the corrosion resistance of quartz glass finished product, in order to
When get both the script quality of glass and corrosion resistance, described Al2O3With SiO in described quartz glass finished product2Weight ratio can be
0.5~10%;As 1%, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9% preferably, can be ZrO2、Y2O3、La2O3、Sc2O3、
ThO2、V2O5、TiO2In the more firm support of at least one offer.
In order to reach above-mentioned weight proportion, specially:Choose the Silicon chloride. of m weight portion, according to described Al2O3With institute
State SiO in quartz glass finished product2Weight ratio meter calculate the weight of the first doped compound.The concrete weight of the first doped compound
Depending on amount is according to the concrete material selected.
In addition, ZrO2、Y2O3、La2O3、Sc2O3、ThO2、V2O5、TiO2In at least one with described quartz glass finished product in
SiO2Weight than 0.5~5%.Be greatly improved, the corrosion resistance of quartz glass finished product.
According to described ZrO2、Y2O3、La2O3、Sc2O3、ThO2、V2O5、TiO2In at least one and described quartz glass become
SiO in product2Weight ratio meter calculate the weight of the second doped compound.The concrete weight of the second doped compound is according to selection
Depending on concrete material.
In the middle of specific enforcement, the preparation method of above-mentioned quartz glass, described by described doping silicon dioxide gel
Fire as quartz glass finished product through burning process, specifically include:
Step 31, in T1At a temperature of to described doping silicon dioxide gel drying, obtain amorphous doping silicon dioxide
Powder, T1At 100~1000 degrees Celsius;
Amorphous doping silicon dioxide powder macroscopically shows as isotropism, no obvious fusing point during melting, simply
Gradually soften with the rising of temperature, viscosity reduces, and is gradually transitions liquid.Amorphous state, also known as glassy state, can be regarded as
The very big subcooled liquid of viscosity.
Step 32, in T2At a temperature of to described doping silicon dioxide powder calcine, so that described doping silicon dioxide powder is turned
It is changed into the doping silicon dioxide powder of crystalline state, T2At 1000~1500 degrees Celsius;
The doping silicon dioxide powder of crystalline state refers to the prevailing form that solid body exists.
Described quartz glass finished product prepared by the doping silicon dioxide powder of crystallized state.
Further, the preparation method of above-mentioned quartz glass, described in T1At a temperature of to described doping silicon dioxide coagulate
Glue is dried, and specifically includes:
The hothouse that described doping silicon dioxide gel is dried is passed through atmosphere is dried, the wherein said atmosphere that is dried includes sky
Gas, oxygen O2, chlorine Cl2, dichloride oxygen sulfur SOCl2In at least one.
In drying, remaining carbon, moisture or hydroxyl in removable doping silicon dioxide gel.
In order to obtain high-quality quartz glass finished product, the preparation method of above-mentioned quartz glass, described crystallized state
Described quartz glass finished product prepared by doping silicon dioxide powder, specially:
Step 33, the doping silicon dioxide powder to described crystalline state carry out grinding, and to the doping titanium dioxide after grinding
Silica flour material screen divides, and obtains the silicon dioxide powder after screening, the silicon dioxide powder after screening is adopted melting technology, 1000
Under~2500 degrees Celsius, it is melting into described quartz glass finished product.
Using in different melting technologies, needing to screen out the doping batch of corresponding particle size, specifically can be found in
Following embodiments:
First, vacuum electric process of smelting fusion process:
The described doping silicon dioxide powder to described crystalline state carries out grinding, and to the doping silicon dioxide powder after grinding
Material screen divides, and obtains the silicon dioxide powder after screening, and the silicon dioxide powder after screening is adopted melting technology, 1000~
Under 2500 degrees Celsius, it is melting into described quartz glass finished product, specially:
To the doping silicon dioxide powder screening after grinding, obtain the doping silicon dioxide powder in 20~200 mesh for the granule,
The doping silicon dioxide powder of 20~200 mesh is melting into described quartz glass finished product using vacuum electric process of smelting.
2nd, high-frequency plasma melting technology fusion process:
The described doping silicon dioxide powder to described crystalline state carries out grinding, and to the doping silicon dioxide powder after grinding
Material screen divides, and obtains the silicon dioxide powder after screening, and the silicon dioxide powder after screening is adopted melting technology, 1000~
Under 2500 degrees Celsius, it is melting into described quartz glass finished product, specially:
To the doping silicon dioxide powder screening after grinding, obtain the doping silicon dioxide powder in 40~300 mesh for the granule,
The doping silicon dioxide powder of 40~300 mesh is melting into described quartz glass finished product using high-frequency plasma melting technology.
3rd, gas refining melting technology fusion process:
The described doping silicon dioxide powder to described crystalline state carries out grinding, and to the doping silicon dioxide powder after grinding
Material screen divides, and obtains the silicon dioxide powder after screening, and the silicon dioxide powder after screening is adopted melting technology, 1000~
Under 2500 degrees Celsius, it is melting into described quartz glass finished product, specially:
To the doping silicon dioxide powder screening after grinding, obtain the doping silicon dioxide powder in 40~300 mesh for the granule,
The doping silicon dioxide powder of 40~300 mesh is melting into described quartz glass finished product using gas refining melting technology.
4th, continuous melting technique fusion process:
The described doping silicon dioxide powder to described crystalline state carries out grinding, and to the doping silicon dioxide powder after grinding
Material screen divides, and obtains the silicon dioxide powder after screening, and the silicon dioxide powder after screening is adopted melting technology, 1000~
Under 2500 degrees Celsius, it is melting into described quartz glass finished product, specially:
To the doping silicon dioxide powder screening after grinding, obtain the doping silicon dioxide powder in 40~300 mesh for the granule,
The doping silicon dioxide powder of 40~300 mesh is melting into described quartz glass finished product using continuous melting technique.
The invention provides the preparation method of the quartz glass of several samples, referring specifically to table 1:
The quartz glass that above-mentioned 3 samples obtain in etching condition is:
40 DEG C of temperature, top pure grade HF and volume ratio=9 analyzing pure acetic acid:Corroded in 4 solution, the present invention obtains
Quartz glass corrosion rate be respectively less than 26 μm/h, existing pure quartz glass under above-mentioned etching condition corrosion rate be 60 μ
m/h;
40 DEG C of temperature, F2In in corroded, the present invention obtain quartz glass corrosion rate be 65 μm/h, existing height
Pure quartz glass corrosion rate under above-mentioned etching condition is 150 μm/h;
Understand through above-mentioned experiment, under above-mentioned etching condition, corrosion rate is respectively 60 μm/h with existing pure quartz glass
Compare with 150 μm/h, the quartz glass that the present invention obtains substantially increases the decay resistance of quartz glass.Inventive embodiments system
The quartz glass obtaining belongs to high-quality quartz glass, can be applied to the application demand in the fields such as semiconductor manufacturing.
Embodiment two
A kind of quartz glass that one embodiment of the present of invention proposes, including:
Quartz glass finished product, the preparation method of described quartz glass finished product quartz glass is prepared from;
The preparation method of described quartz glass, including:
First doped compound, the second doped compound dissolving are mixed to form by doping mixed solution, institute by lytic agent
Stating the first doped compound is aluminum contained compound, and described second doped compound includes compound containing Zr, compound containing Y, contains La
At least one in compound, compound containing Sc, compound containing Th, compound containing V, compound containing Ti;
By parts by volume L1Doping mixed solution, parts by volume L2Water mixing after, with Silicon chloride. liquid phase reactor obtain doping
Silica dioxide gel;
Described doping silicon dioxide gel is fired as quartz glass finished product, wherein, described quartz glass through burning process
Include in glass finished product and fire, through the Part I in described doping mixed solution, the Al being transformed2O3, through described doping mixing
Part II in solution fires the ZrO being transformed2、Y2O3、La2O3、Sc2O3、ThO2、V2O5、TiO2In at least one;
Al2O3And ZrO2、Y2O3、La2O3、Sc2O3、ThO2、V2O5、TiO2In at least one with network intermediate or network
Ectosome form is filled in SiO2In the hole of tetrahedral network structure.
In the quartz glass finished product that the present invention provides, Al2O3、ZrO2、Y2O3、La2O3、Sc2O3、ThO2、V2O5、TiO2With net
Network intermediate or network outer body form are filled in SiO2In the hole of tetrahedral network structure, quartz glass of the present invention is made more to cause
Close;Meanwhile, Al2O3、ZrO2、Y2O3、La2O3、Sc2O3、ThO2、V2O5、TiO2Resolution valency compare SiO2Height, that is, compared with SiO2Anti-
The corrosivity of Fluohydric acid. are strong, it is possible to decrease quartz glass corrosion of (as hydrofluoric acid environment) in acid solution or sour gas is fast
Rate, and then improve the acid-resisting corrosive nature of quartz glass.
Specifically, the preparation method of the quartz glass described in the present embodiment two can directly be provided using above-described embodiment one
Described quartz glass preparation method, concrete implementation structure can be found in the related content described in above-described embodiment one, this
Place repeats no more.
Wherein, quartz glass finished product can burn out product of different shapes according to using different grinding tools.Described quartz glass
Glass finished product can prop up for quartz glass stone roller, quartz glass bar, quartz glass tube, quartz glass plate, quartz glass ring, quartz glass
Frame, quartz glass plate, quartz glass flange, quartz glass cutting boat or quartz glass rinse bath.
In the above-described embodiments, the description to each embodiment all emphasizes particularly on different fields, and does not have the portion described in detail in certain embodiment
Point, may refer to the associated description of other embodiment.
It is understood that the correlated characteristic in said apparatus can mutually reference.In addition, in above-described embodiment " the
One ", " second " etc. is for distinguishing each embodiment, and does not represent the quality of each embodiment.
In description mentioned herein, illustrate a large amount of details.It is to be appreciated, however, that the enforcement of the present invention
Example can be put into practice in the case of not having these details.In some instances, known structure and skill are not been shown in detail
Art, so as not to obscure the understanding of this description.
Similarly it will be appreciated that in order to simplify the disclosure and help understand one or more of each inventive aspect,
Above in the description to the exemplary embodiment of the present invention, each feature of the present invention is grouped together into single enforcement sometimes
In example, figure or descriptions thereof.However, the device of the disclosure should be construed to reflect following intention:I.e. required guarantor
The application claims of shield more features than the feature being expressly recited in each claim.More precisely, it is such as following
Claims reflected as, inventive aspect is all features less than single embodiment disclosed above.Therefore,
The claims following specific embodiment are thus expressly incorporated in this specific embodiment, wherein each claim itself
All as the separate embodiments of the present invention.
Those skilled in the art are appreciated that and the part in the device in embodiment can be carried out adaptively
Change and they are arranged in one or more devices different from this embodiment.Can be the unit construction in embodiment
Become a part, and multiple subassemblies can be divided in addition.Except at least some of such feature is mutual
Outside repulsion, can be using any combinations to the institute disclosed in this specification (including adjoint claim, summary and accompanying drawing)
Feature and all parts of so disclosed any device are had to be combined.Unless expressly stated otherwise, this specification (includes
Adjoint claim, summary and accompanying drawing) disclosed in each feature can be by the replacement providing identical, equivalent or similar purpose
Feature is replacing.
Although additionally, it will be appreciated by those of skill in the art that some embodiments described herein include other embodiments
In included some features rather than further feature, but the combination of the feature of different embodiment means to be in the present invention's
Within the scope of and form different embodiments.For example, in the following claims, embodiment required for protection appoint
One of meaning can in any combination mode using.The all parts embodiment of the present invention can be realized with hardware, or
Realized with combinations thereof.
It should be noted that above-described embodiment the present invention will be described rather than limits the invention, and ability
Field technique personnel can design alternative embodiment without departing from the scope of the appended claims.In the claims,
Any reference markss between bracket should not be configured to limitations on claims.Word "comprising" does not exclude the presence of not
Part listed in the claims or assembly.Word "a" or "an" before part or assembly does not exclude the presence of multiple
Such part or assembly.The present invention can be realized by means of the device including some difference parts.Some listing
In the claim of part, several in these parts can be embodied by same part item.Word first,
Second and the use of third class do not indicate that any order.These words can be construed to title.
The above, be only presently preferred embodiments of the present invention, and not the present invention is made with any pro forma restriction, according to
Any simple modification, equivalent variations and modification above example made according to the technical spirit of the present invention, all still falls within this
In the range of bright technical scheme.
Claims (14)
1. a kind of preparation method of quartz glass is it is characterised in that include:
First doped compound, the second doped compound dissolving are mixed to form by doping mixed solution by lytic agent, described the
One doped compound is aluminum contained compound, and described second doped compound includes compound containing Zr, compound containing Y, chemical combination containing La
At least one in thing, compound containing Sc, compound containing Th, compound containing V, compound containing Ti;
By parts by volume L1Doping mixed solution, parts by volume L2Water mixing after, with Silicon chloride. liquid phase reactor obtain doping dioxy
SiClx gel;
Described doping silicon dioxide gel is fired as quartz glass finished product, wherein, described quartz glass one-tenth through burning process
Include in product and fire, through the Part I in described doping mixed solution, the Al being transformed2O3, through described doping mixed solution
In Part II fire the ZrO being transformed2、Y2O3、La2O3、Sc2O3、ThO2、V2O5、TiO2In at least one.
2. quartz glass according to claim 1 preparation method it is characterised in that
L1、L2Ratio 1:5~200.
3. quartz glass according to claim 1 preparation method it is characterised in that
The reaction rate of described Silicon chloride. is in 20~500ml/min.
4. quartz glass according to claim 1 preparation method it is characterised in that
Described by parts by volume L1Doping mixed solution, parts by volume L2Water mixing after, with Silicon chloride. liquid phase reactor obtain doping
Silica dioxide gel, specifically includes:
During Silicon chloride. is gradually added doping mixed solution and the mixed mixed liquor of water, and described mixed liquor is entered
Row stirring, obtains doping silicon dioxide gel;Or,
Described by parts by volume L1Doping mixed solution, parts by volume L2Water mixing after, with Silicon chloride. liquid phase reactor obtain doping
Silica dioxide gel, specifically includes:
After Silicon chloride., doping mixed solution and the mixed mixed liquor of water are atomized respectively, it is passed through in reative cell simultaneously and carries out
Phase reaction obtains doping silicon dioxide gel.
5. quartz glass according to claim 1 preparation method it is characterised in that
Described by parts by volume L1Doping mixed solution, parts by volume L2Water mixing after, with Silicon chloride. liquid phase reactor obtain doping
Silica dioxide gel, specifically includes:
Mixed doping mixed solution, the mixed liquor of water are obtained with Silicon chloride. liquid phase reactor under 10~100 degrees Celsius and mix
Miscellaneous silica dioxide gel.
6. quartz glass according to claim 1 preparation method it is characterised in that
Described lytic agent includes the first lytic agent for dissolving described first doped compound, and described first lytic agent includes first
At least one in alcohol, ethanol, acetic acid, hydrochloric acid, nitric acid, distilled water, hydrogen peroxide;
Described first doped compound includes nitric hydrate aluminum Al (NO3)3·H2O, ANN aluminium nitrate nonahydrate Al (NO3)3·9H2O, six
Hydration aluminium chlorate Al (ClO3)3·6H2O, aluminum chloride AlCl3In at least one.
7. quartz glass according to claim 1 preparation method it is characterised in that
Described lytic agent includes the second lytic agent for dissolving described second doped compound, and described second lytic agent includes first
At least one in alcohol, ethanol, acetic acid, hydrochloric acid, nitric acid, distilled water, hydrogen peroxide;
Described compound containing Zr includes zirconium nitrate Zr (NO3)4·5H2O, zirconium carbonate ammonium ZrO (CO3)2(NH4)2·nH2O, zirconium carbonate
ZrOCO3·nH2O, eight water oxygen zirconium chloride ZrOCl2·8(H2O), zirconium chloride ZrCl4, eight water basic zirconium chloride ZrOCl2·8H2O
In at least one;
Described compound containing Y includes yttrium oxalate Y2(C2O4)3·10H2O, Yttrium trinitrate Y (NO3)3·6H2O, hydration Yttrium carbonate (Y2(CO3)3) Y2
(CO3)3·3H2O, Yttrium chloride(Y2Cl6) six water YCl3·6H2O, chloride hydrate yttrium YCl3H2At least one in O;
Described compound containing La includes lanthanum chloride LaCl3, Lanthanum trichloride hexahydrate. LaCl3·6H2O, Lanthanum (III) nitrate La (NO3)3·6H2O、
Lanthanum carbonate La2(CO3)3.8H2At least one in O;
Described compound containing Sc includes six water Scium chloride (Sc4Cl12) ScCl3·6H2O, Scium chloride (Sc4Cl12) ScCl3, Scium nitrate(Sc(NO3)3) Sc (NO3)3·3H2O, nitre
Sour scandium Sc (NO3)3·4H2O, Scium nitrate(Sc(NO3)3) Sc (NO3)3·5H2O, Scium nitrate(Sc(NO3)3) Sc (NO3)3·6H2O, six pasture and water acid scandium Sc2
(C2O4)3·6H2At least one in O;
Described compound containing Th includes thorium nitrate Th (NO3)4·4H2O, thhorium oxalate Th (C2O4)2, thorium tetrachloride ThCl4, perchloric acid
Thorium Th (ClO4)4In at least one;
Described compound containing V includes vanadium chloride VCl3, nitric acid vanadium acyl VO2NO3In at least one;
Described compound containing Ti includes Titanium Nitrate Ti (NO3)4.
8. quartz glass according to claim 1 preparation method it is characterised in that
Described Al2O3With SiO in described quartz glass finished product2Weight than 0.5~10%;
ZrO2、Y2O3、La2O3、Sc2O3、ThO2、V2O5、TiO2With SiO in described quartz glass finished product2Weight ratio respectively exist
0.5~5%.
9. the preparation method according to described quartz glass arbitrary in claim 1~8 it is characterised in that
Described described doping silicon dioxide gel is fired as quartz glass finished product through burning process, specifically include:
In T1At a temperature of to described doping silicon dioxide gel drying, obtain amorphous doping silicon dioxide powder, T1100
~1000 degrees Celsius;
In T2At a temperature of to described doping silicon dioxide powder calcine, make described doping silicon dioxide powder be changed into crystalline state
Doping silicon dioxide powder, T2At 1000~1500 degrees Celsius;
Described quartz glass finished product prepared by the doping silicon dioxide powder of crystallized state.
10. quartz glass according to claim 9 preparation method it is characterised in that
Described in T1At a temperature of to described doping silicon dioxide gel drying, specifically include:
The hothouse that described doping silicon dioxide gel is dried is passed through atmosphere is dried, wherein said be dried atmosphere include air,
Oxygen O2, chlorine Cl2, dichloride oxygen sulfur SOCl2In at least one.
The preparation method of 11. quartz glasss according to claim 9 it is characterised in that
Described quartz glass finished product prepared by the doping silicon dioxide powder of described crystallized state, specially:
Grinding is carried out to the doping silicon dioxide powder of described crystalline state, and to the doping silicon dioxide powder screening after grinding,
Obtain the silicon dioxide powder after screening, the silicon dioxide powder after screening is adopted melting technology, Celsius 1000~2500
Under degree, it is melting into described quartz glass finished product.
The preparation method of 12. quartz glasss according to claim 11 it is characterised in that
The described doping silicon dioxide powder to described crystalline state carries out grinding, and to the doping silicon dioxide Powder screen after grinding
Point, obtain the silicon dioxide powder after screening, the silicon dioxide powder after screening is adopted melting technology, takes the photograph 1000~2500
Under family name's degree, it is melting into described quartz glass finished product, specially:
To the doping silicon dioxide powder screening after grinding, obtain the doping silicon dioxide powder in 20~200 mesh for the granule, by 20
The doping silicon dioxide powder of~200 mesh is melting into described quartz glass finished product using vacuum electric process of smelting;Or,
To the doping silicon dioxide powder screening after grinding, obtain the doping silicon dioxide powder in 40~300 mesh for the granule, by 40
The doping silicon dioxide powder of~300 mesh is melting into described quartz glass finished product using high-frequency plasma melting technology;Or,
To the doping silicon dioxide powder screening after grinding, obtain the doping silicon dioxide powder in 40~300 mesh for the granule, by 40
The doping silicon dioxide powder of~300 mesh is melting into described quartz glass finished product using gas refining melting technology;Or,
To the doping silicon dioxide powder screening after grinding, obtain the doping silicon dioxide powder in 40~300 mesh for the granule, by 40
The doping silicon dioxide powder of~300 mesh is melting into described quartz glass finished product using continuous melting technique.
A kind of 13. quartz glasss are it is characterised in that include:
Quartz glass finished product, described quartz glass finished product adopts the system of arbitrary described quartz glass in the claims 1-12
Preparation Method is prepared from.
14. quartz glasss according to claim 13 it is characterised in that
Described quartz glass finished product is quartz glass stone roller, quartz glass bar, quartz glass tube, quartz glass plate, quartz glass ring,
Quartz glass support, quartz glass plate, quartz glass flange, quartz glass cutting boat or quartz glass rinse bath.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201610809509.XA CN106430947B (en) | 2016-09-07 | 2016-09-07 | The preparation method and quartz glass of quartz glass |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201610809509.XA CN106430947B (en) | 2016-09-07 | 2016-09-07 | The preparation method and quartz glass of quartz glass |
Publications (2)
Publication Number | Publication Date |
---|---|
CN106430947A true CN106430947A (en) | 2017-02-22 |
CN106430947B CN106430947B (en) | 2019-02-19 |
Family
ID=58165188
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201610809509.XA Active CN106430947B (en) | 2016-09-07 | 2016-09-07 | The preparation method and quartz glass of quartz glass |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN106430947B (en) |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1974447A (en) * | 2005-08-10 | 2007-06-06 | 德古萨诺瓦拉科技股份公司 | Sol-gel process |
CN103864292A (en) * | 2014-02-28 | 2014-06-18 | 中国科学院上海光学精密机械研究所 | Preparation method for fluorine-containing low-refractivity Yb<3+>-doped quartz glass |
CN105481246A (en) * | 2015-12-01 | 2016-04-13 | 中国科学院上海光学精密机械研究所 | Rare earth, lanthanum and aluminum codoped quartz glass and preparation method thereof |
-
2016
- 2016-09-07 CN CN201610809509.XA patent/CN106430947B/en active Active
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1974447A (en) * | 2005-08-10 | 2007-06-06 | 德古萨诺瓦拉科技股份公司 | Sol-gel process |
CN103864292A (en) * | 2014-02-28 | 2014-06-18 | 中国科学院上海光学精密机械研究所 | Preparation method for fluorine-containing low-refractivity Yb<3+>-doped quartz glass |
CN105481246A (en) * | 2015-12-01 | 2016-04-13 | 中国科学院上海光学精密机械研究所 | Rare earth, lanthanum and aluminum codoped quartz glass and preparation method thereof |
Non-Patent Citations (3)
Title |
---|
YU FEN WANG ET AL.: "Preparation of High Purity Low Hydroxyl Synthetic Fused Silica Glass", 《ADVANCED MATERIALS RESEARCH》 * |
徐平坤等: "《耐火材料新工艺技术》", 31 January 2005, 冶金工业出版社 * |
王超: "《水解工艺Yb3+/Al3+共掺石英玻璃的研制及特性表征》", 《光电子·激光》 * |
Also Published As
Publication number | Publication date |
---|---|
CN106430947B (en) | 2019-02-19 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
US11952303B2 (en) | Increase in silicon content in the preparation of quartz glass | |
TW201731781A (en) | Preparation of a quartz glass body in a standing sinter crucible | |
US11299417B2 (en) | Preparation of a quartz glass body in a melting crucible of refractory metal | |
US11053152B2 (en) | Spray granulation of silicon dioxide in the preparation of quartz glass | |
TW201736288A (en) | Preparation of a quartz glass body in a hanging sinter crucible | |
TW201733930A (en) | Ammonia treatment of silicon dioxide powder in the preparation of quartz glass | |
TW201738188A (en) | Preparation of quartz glass bodies with dew point monitoring in the melting oven | |
US20190062193A1 (en) | Preparation of a quartz glass body in a multi-chamber oven | |
TW201736290A (en) | Preparation and post-treatment of a quartz glass body | |
TW201731767A (en) | Preparation of quartz glass bodies from silicon dioxide powder | |
CN1215708A (en) | Method for producing corrosion resistant refractories | |
TW201731780A (en) | Preparation of a quartz glass body in a hanging metal sheet crucible | |
KR20180095879A (en) | Treating the carbon-doped silica granules at elevated temperatures to reduce the alkaline earth metal content of the silica granules | |
TW201733929A (en) | Preparation of an opaque quartz glass body | |
TW201736287A (en) | Gas flushing for melting ovens and process for preparation of quartz glass | |
CN106430912A (en) | Preparation method of low-hydroxyl quartz glass and quartz glass | |
CN105271649B (en) | For producing the method for doped silica glass | |
CN103556224A (en) | Method for preparing zirconium silicate whisker by employing non-hydrolytic sol-gel technology combined with molten-salt growth method | |
CN106116122A (en) | Prepare sintering equipment and the system of quartz glass | |
CN106365438A (en) | Quartz glass and preparation method thereof | |
CN106430947A (en) | Preparation method of quartz glass and quartz glass | |
CN106380072B (en) | The preparation method and quartz glass of quartz glass | |
CN106396350A (en) | Sintering method for preparing silica glass and silica glass | |
CN106430920B (en) | The preparation method and quartz glass of quartz glass | |
WO2020195721A1 (en) | Spinel powder |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
C06 | Publication | ||
PB01 | Publication | ||
C10 | Entry into substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
GR01 | Patent grant | ||
GR01 | Patent grant |