CN116969669A - Preparation device and method for large-size infrared synthetic quartz material - Google Patents
Preparation device and method for large-size infrared synthetic quartz material Download PDFInfo
- Publication number
- CN116969669A CN116969669A CN202310985729.8A CN202310985729A CN116969669A CN 116969669 A CN116969669 A CN 116969669A CN 202310985729 A CN202310985729 A CN 202310985729A CN 116969669 A CN116969669 A CN 116969669A
- Authority
- CN
- China
- Prior art keywords
- deposition
- deposition crucible
- production
- synthetic quartz
- burner
- 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.)
- Pending
Links
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 165
- 239000010453 quartz Substances 0.000 title claims abstract description 99
- 239000000463 material Substances 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title claims description 58
- 230000008021 deposition Effects 0.000 claims abstract description 139
- 238000006243 chemical reaction Methods 0.000 claims abstract description 106
- 238000004519 manufacturing process Methods 0.000 claims abstract description 86
- 239000010936 titanium Substances 0.000 claims abstract description 71
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 71
- 238000005906 dihydroxylation reaction Methods 0.000 claims abstract description 52
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 51
- 238000007872 degassing Methods 0.000 claims abstract description 41
- 150000004820 halides Chemical class 0.000 claims abstract description 39
- 239000002912 waste gas Substances 0.000 claims abstract description 20
- 238000000151 deposition Methods 0.000 claims description 139
- 235000012239 silicon dioxide Nutrition 0.000 claims description 123
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 52
- 239000007789 gas Substances 0.000 claims description 50
- 239000000377 silicon dioxide Substances 0.000 claims description 33
- 230000008569 process Effects 0.000 claims description 28
- 229910052786 argon Inorganic materials 0.000 claims description 26
- 239000002994 raw material Substances 0.000 claims description 25
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 22
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 20
- 239000001307 helium Substances 0.000 claims description 20
- 229910052734 helium Inorganic materials 0.000 claims description 20
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 20
- 239000001257 hydrogen Substances 0.000 claims description 20
- 229910052739 hydrogen Inorganic materials 0.000 claims description 20
- 239000001301 oxygen Substances 0.000 claims description 20
- 229910052760 oxygen Inorganic materials 0.000 claims description 20
- 230000001502 supplementing effect Effects 0.000 claims description 20
- -1 titanium halide Chemical class 0.000 claims description 20
- 239000011261 inert gas Substances 0.000 claims description 18
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 claims description 17
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 17
- 239000000460 chlorine Substances 0.000 claims description 17
- 229910052801 chlorine Inorganic materials 0.000 claims description 17
- 239000005049 silicon tetrachloride Substances 0.000 claims description 17
- 238000005245 sintering Methods 0.000 claims description 16
- 239000000919 ceramic Substances 0.000 claims description 5
- 238000002485 combustion reaction Methods 0.000 claims description 4
- 239000002657 fibrous material Substances 0.000 claims description 4
- 238000002203 pretreatment Methods 0.000 claims description 4
- 238000004017 vitrification Methods 0.000 claims description 4
- 229910010293 ceramic material Inorganic materials 0.000 claims description 3
- 230000003247 decreasing effect Effects 0.000 claims description 3
- 238000006460 hydrolysis reaction Methods 0.000 claims description 2
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 claims 1
- 239000000203 mixture Substances 0.000 claims 1
- 230000007547 defect Effects 0.000 abstract description 5
- 239000000843 powder Substances 0.000 description 12
- 238000007740 vapor deposition Methods 0.000 description 11
- 230000003287 optical effect Effects 0.000 description 9
- 239000012535 impurity Substances 0.000 description 8
- 238000009826 distribution Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 5
- 230000033001 locomotion Effects 0.000 description 5
- 238000002834 transmittance Methods 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 238000005137 deposition process Methods 0.000 description 4
- 230000031700 light absorption Effects 0.000 description 4
- 230000001360 synchronised effect Effects 0.000 description 4
- 239000000872 buffer Substances 0.000 description 3
- 230000006866 deterioration Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000002210 silicon-based material Substances 0.000 description 3
- 238000009423 ventilation Methods 0.000 description 3
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 2
- 229910003074 TiCl4 Inorganic materials 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 238000009825 accumulation Methods 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 238000004891 communication Methods 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 230000018044 dehydration Effects 0.000 description 2
- 238000006297 dehydration reaction Methods 0.000 description 2
- 229910001882 dioxygen Inorganic materials 0.000 description 2
- 230000005484 gravity Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 230000010355 oscillation Effects 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 150000003609 titanium compounds Chemical class 0.000 description 2
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 2
- 238000009827 uniform distribution Methods 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 229910010386 TiI4 Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000000429 assembly Methods 0.000 description 1
- 230000000712 assembly Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000001459 lithography Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 239000013307 optical fiber Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- NLLZTRMHNHVXJJ-UHFFFAOYSA-J titanium tetraiodide Chemical compound I[Ti](I)(I)I NLLZTRMHNHVXJJ-UHFFFAOYSA-J 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B37/00—Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
- C03B37/01—Manufacture of glass fibres or filaments
- C03B37/012—Manufacture of preforms for drawing fibres or filaments
- C03B37/014—Manufacture of preforms for drawing fibres or filaments made entirely or partially by chemical means, e.g. vapour phase deposition of bulk porous glass either by outside vapour deposition [OVD], or by outside vapour phase oxidation [OVPO] or by vapour axial deposition [VAD]
- C03B37/018—Manufacture of preforms for drawing fibres or filaments made entirely or partially by chemical means, e.g. vapour phase deposition of bulk porous glass either by outside vapour deposition [OVD], or by outside vapour phase oxidation [OVPO] or by vapour axial deposition [VAD] by glass deposition on a glass substrate, e.g. by inside-, modified-, plasma-, or plasma modified- chemical vapour deposition [ICVD, MCVD, PCVD, PMCVD], i.e. by thin layer coating on the inside or outside of a glass tube or on a glass rod
- C03B37/01807—Reactant delivery systems, e.g. reactant deposition burners
- C03B37/01815—Reactant deposition burners or deposition heating means
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B37/00—Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
- C03B37/01—Manufacture of glass fibres or filaments
- C03B37/012—Manufacture of preforms for drawing fibres or filaments
- C03B37/014—Manufacture of preforms for drawing fibres or filaments made entirely or partially by chemical means, e.g. vapour phase deposition of bulk porous glass either by outside vapour deposition [OVD], or by outside vapour phase oxidation [OVPO] or by vapour axial deposition [VAD]
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B37/00—Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
- C03B37/01—Manufacture of glass fibres or filaments
- C03B37/012—Manufacture of preforms for drawing fibres or filaments
- C03B37/014—Manufacture of preforms for drawing fibres or filaments made entirely or partially by chemical means, e.g. vapour phase deposition of bulk porous glass either by outside vapour deposition [OVD], or by outside vapour phase oxidation [OVPO] or by vapour axial deposition [VAD]
- C03B37/018—Manufacture of preforms for drawing fibres or filaments made entirely or partially by chemical means, e.g. vapour phase deposition of bulk porous glass either by outside vapour deposition [OVD], or by outside vapour phase oxidation [OVPO] or by vapour axial deposition [VAD] by glass deposition on a glass substrate, e.g. by inside-, modified-, plasma-, or plasma modified- chemical vapour deposition [ICVD, MCVD, PCVD, PMCVD], i.e. by thin layer coating on the inside or outside of a glass tube or on a glass rod
- C03B37/01807—Reactant delivery systems, e.g. reactant deposition burners
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention relates to a preparation device of a large-size infrared synthetic quartz material, which comprises a furnace body, a bottom cover arranged below the furnace body, a supporting system which is arranged at the center of the bottom cover and can be rotated and lifted under the drive of a power device, and a deposition crucible connected with the supporting system. The furnace body and the bottom cover jointly form a working cavity, the deposition crucible is fixedly arranged at the top of the supporting system, the supporting system can also transversely move under the drive of the power device, the bottom cover is provided with a furnace bottom opening baffle for separating the reaction cavity and the waste gas cavity, and the furnace bottom opening baffle is provided with an air draft micropore and can transversely move under the drive of the supporting system. A blast lamp component is arranged above the deposition crucible, and the blast lamp component is a component comprising a production blast lamp, a dehydroxylation pre-degassing blast lamp and a titanium-containing halide blast lamp. The invention solves the technical problems that the loose body has weak strength and is not easy to burn through due to the defects of small density, air holes and the like in the loose body in the prior art, and the infrared synthetic quartz is not suitable to be oversized.
Description
Technical Field
The invention relates to the technical field of infrared synthetic quartz material preparation, in particular to a preparation device and a preparation method of a large-size infrared synthetic quartz material.
Background
Synthetic quartz is a key substrate material for communication optical fiber preforms, LCD photomasks and semiconductor photomasks, and is also an important optical element material in aerospace, high-energy laser systems and lithography systems. The infrared synthetic quartz is synthetic quartz with higher application rate, and has the characteristics of high ultraviolet transmittance, high optical uniformity, high internal quality, high laser damage resistance, low absorption coefficient and the like.
The infrared synthetic quartz is synthesized by chemical reaction mainly taking silicon-containing compounds as raw materials, and the main preparation methods comprise a Plasma Chemical Vapor Deposition (PCVD) method and a VAD (vapor deposition) process method. The PCVD method directly deposits the silicon-containing compound in a plasma flame anhydrous environment to obtain the infrared synthetic quartz, so that the preparation cost is high, and the industrial mass is difficult to realize. The VAD process uses oxyhydrogen flame to replace plasma flame, namely, firstly, silicon-containing compounds are subjected to deposition reaction in oxyhydrogen flame environment to generate loose bodies, then, the loose bodies are sintered to form infrared synthetic quartz, and the quartz product prepared by the VAD process is extremely low in impurity content, controllable in hydroxyl content and low in preparation cost, so that the VAD process gradually becomes a mainstream preparation method of the infrared synthetic quartz.
However, the existing VAD process has the following problems due to the limitations of the preparation apparatus and method, although it has low cost: as the existing VAD process adopts a downward growth method, namely, in a device for implementing the VAD process, a deposition seed rod is positioned at the bottom of a supporting system and can rise along with the rotation of the supporting system in the deposition production process, and meanwhile, raw materials are sprayed onto the seed rod from bottom to top to perform deposition to form a loose body, and the loose body is gradually formed from top to bottom in the process, which is called downward growth. The density of the loose body generated by the device is small, and defects such as air holes exist in the loose body, so that the problems of cracking and falling, incapability of burning and air bubble defects can occur when the diameter of the burned loose body is large. Therefore, the diameter of the infrared synthetic quartz manufactured by the VAD process implemented by the prior device is generally controlled to be about 300mm, and when a large-caliber element is required to be manufactured, the quartz rod needs to be processed after primary or secondary groove sinking and shaping, so that the utilization rate of materials is reduced, and the materials have great scrapping risks in the groove sinking process, which limits the application of the infrared synthetic quartz manufactured by the prior device and method to the large-caliber element.
Disclosure of Invention
Therefore, the technical problem to be solved by the invention is to overcome the defects that the density of a loose body prepared by the existing device and method is small, pores exist in the loose body, and the like, so that the loose body is weak in strength and is not easy to burn through, and the technical problem that the size of infrared synthetic quartz is not suitable to be excessively large is solved.
In order to solve the technical problems, the invention provides a preparation device of a large-size infrared synthetic quartz material, which comprises a furnace body, a bottom cover arranged below the furnace body, a supporting system which is arranged at the center of the bottom cover and can be rotated and lifted under the drive of a power device, and a deposition crucible connected with the supporting system. The furnace body and the bottom cover jointly form a working cavity, and the deposition crucible is fixedly arranged at the top of the supporting system; the supporting system can transversely move under the drive of the power device. The bottom cover is provided with a furnace bottom opening baffle plate which can transversely move under the drive of the supporting system, and the working cavity is divided into a reaction cavity and a waste gas cavity. The baffle plate at the bottom of the furnace is provided with an exhaust micropore, and a blast lamp component (6) is arranged above the deposition crucible.
In one embodiment of the invention, the furnace body is made of ceramic fiber material, and a quartz lining is arranged on the inner side.
In one embodiment of the invention, at least one air supplementing channel with an included angle R smaller than 180 degrees with the side wall of the furnace body is arranged at the top of the reaction cavity and is used for introducing inert gas, and an exhaust channel for exhausting exhaust gas is arranged at one side of the exhaust cavity.
In one embodiment of the invention, a burner assembly comprises a production burner, a dehydroxylation pre-degas burner, and a titanium-containing halide burner. The number of the production torches, the dehydroxylation pre-degassing torches and the titanium-containing halide torches is at least one. The production burner, the dehydroxylation pre-degassing burner and the titanium-containing halide burner are uniformly arranged.
In one embodiment of the invention, the inner diameter of the deposition crucible is not less than 1100mm and the depth is not less than 600mm, and the material of the deposition crucible is ceramic material.
The invention also provides a preparation method of the large-size infrared synthetic quartz material, which comprises the following production steps:
step S1: introducing hydrogen and oxygen into the reaction cavity through the production blowtorch, and forming oxyhydrogen flame after ignition, so that the reaction cavity is heated and preheated;
step S2: when the temperature in the reaction cavity reaches 800 ℃, argon is continuously introduced into the reaction cavity through a production blowlamp;
step S3: raising the support system to a deposition reaction position, wherein the lower end of the blast lamp assembly is positioned at 300-500mm above the inner bottom of the deposition crucible;
step S4: when the temperature in the reaction cavity is stabilized at 800-1000 ℃, introducing gaseous silicon tetrachloride raw material into the deposition crucible through a production blowtorch, and producing nano-scale silicon dioxide after the silicon tetrachloride undergoes hydrolysis reaction in the oxyhydrogen combustion process, wherein the nano-scale silicon dioxide is accumulated in the deposition crucible to form a loose quartz ingot; while carrying out deposition production, introducing a chlorine and helium mixed gas into a deposition crucible by a dehydroxylation pre-degassing blast lamp, and carrying out dehydroxylation pre-treatment on a loose quartz ingot; simultaneously, a titanium halide blast lamp is used for introducing titanium halide into the deposition crucible, and titanium doping treatment is carried out on the loose quartz ingot;
Step S5: in the deposition production process, the supporting system and the deposition crucible are driven by the power device to repeatedly move transversely while rotating downwards, and the bottom baffle of the furnace is driven by the supporting system to repeatedly move transversely; the distance between the lower end of the blast lamp component and the top of the loose quartz ingot is always controlled to be 300-500mm; high-cleanness inert gas is introduced into the reaction cavity through the air supplementing channel, and the air speed range of air supplementing is 2-10m/s; exhausting air through the air exhausting channel, wherein waste gas and silicon dioxide in the reaction cavity enter the waste gas cavity through the air exhausting micropore in the deposition production process, and then are exhausted through the air exhausting channel, and the air speed range of air exhausting is 2-10m/s;
step S6: after deposition production for 50-80 hours, loose quartz ingots with the weight not less than 250kg are obtained, and then the process ending and stopping operation is carried out. And transferring the loose quartz ingot into a sintering furnace for vitrification sintering to finally obtain the infrared synthetic quartz rod with the diameter of 600 mm.
In one embodiment of the present invention, in step S1, the hydrogen and oxygen are high purity gases with a purity of 5N or more; the flow rate of hydrogen ranges from 75L/min to 230L/min, and the flow rate of oxygen ranges from 50L/min to 150L/min.
In one embodiment of the present invention, in step S2, argon is a high purity gas with a purity of 5N, and the flow rate of argon is in the range of 20-80L/min.
In one embodiment of the invention, in the step S4, the flow rate of the gaseous silicon tetrachloride raw material ranges from 20L/min to 40L/min; chlorine and helium are high-purity gases with the purity of more than 5N, and the molar ratio of the mixed gases of the chlorine and the helium is 1:0.75, wherein the flow range of the mixed gas is 5-20L/min; the flow rate of the titanium halide is in the range of 3-20L/min.
In one embodiment of the invention, in the step S5, the rotating speed of the deposition crucible is 15-50rpm, the traversing speed is 0.1-5m/S, the interval is +/-200 mm, and the curve that the central speed is maximum and gradually decreases towards the edge is changed into the accelerating movement; when the deposition crucible moves transversely, the projection below the blast lamp component does not exceed the inner bottom of the deposition crucible.
Compared with the prior art, the technical scheme of the invention has the following advantages:
the invention relates to a preparation device of a large-size infrared synthetic quartz material, which comprises a furnace body, a bottom cover arranged below the furnace body, a supporting system which is arranged at the center of the bottom cover and can be rotated and lifted under the drive of a power device, and a deposition crucible connected with the supporting system. The furnace body and the bottom cover together form a working cavity. In the invention, the deposition crucible is arranged at the top of the supporting system, compared with the situation that the deposition crucible adopted in the prior art is arranged at the bottom of the supporting system, the invention adopts an upward growth method, namely, in the deposition crucible, loose bodies are gradually formed from bottom to top, and compared with the prior art, the upward growth method has the advantages that the density of the loose bodies is increased, the strength is higher, the loose bodies are not easy to crack and fall off under the action of gravity, and the defects of few or no air holes and the like exist in the inside. In addition, the deposition crucible provided by the invention can be repeatedly transversely moved while being driven by the supporting system to rotate and descend, so that the density distribution of silicon dioxide deposited in the deposition crucible is more uniform. The bottom cover is provided with a bottom baffle plate, the bottom baffle plate divides the working cavity into a reaction cavity and a waste gas cavity, and a loose body is formed in the reaction cavity. The bottom baffle is provided with exhaust micropores, so that waste gas and silicon dioxide in the reaction chamber are uniformly led out through the exhaust micropores, and the stability and consistency of a flow field in the reaction chamber are ensured. The bottom baffle plate can transversely move under the drive of the support system, so that loose powder obtained by deposition is repeatedly shaken, and the density of the loose powder is higher and the growth process is more uniform.
The invention installs the blast lamp assembly above the deposition crucible, the blast lamp assembly is the assembly comprising at least one production blast lamp, at least one dehydroxylation pre-degassing blast lamp and at least one titanium-containing halide blast lamp, the quantity of the three blast lamps is the same and the three blast lamps are evenly arranged ， The dehydroxylation treatment and the titanium doping treatment are more uniform, so that the loose quartz ingot is thoroughly dehydroxylated, and the optical performance of the sintered infrared synthetic quartz is more excellent. In the upward production method, gaseous silicon tetrachloride raw materials are introduced into a deposition crucible through a production blast lamp to carry out deposition reaction to produce loose powder, a microlayer loose powder is produced through deposition, meanwhile, chlorine and helium mixed gas is introduced into the deposition crucible through a dehydroxylation pre-degassing blast lamp to carry out dehydroxylation pretreatment on the produced loose powder, meanwhile, titanium halide is introduced into the deposition crucible through a titanium-containing halide blast lamp to carry out titanium doping treatment on the produced loose powder, synchronous deposition and synchronous process treatment are realized, the problem that the hydroxyl content is gradually reduced from a core part to an edge due to dehydration in the sintering process is solved, uniform distribution and stable doping of titanium compounds are realized, and the optical uniformity of materials is improved. Because the upward growth method implemented by the preparation device of the large-size infrared synthetic quartz material of the invention is adopted, the density of loose bodies is increased and the distribution is more uniform Even, the intensity of the loose body is increased and the sintering is easier, so the upward growth method implemented by the preparation device of the large-size infrared synthetic quartz material can obviously increase the size of the obtained loose body, and further the infrared synthetic quartz with larger size can be obtained by sintering.
Furthermore, the furnace body is made of heat-insulating ceramic fiber materials, so that the temperature of the external environment is isolated, and the smooth reaction is ensured. The quartz lining is arranged on the inner side of the furnace body, so that the problems of low purity of the loose body, poor material transmittance, and deterioration of key indexes such as light absorption and laser damage resistance threshold value caused by metal impurities in the cavity are avoided.
Furthermore, at least one air supplementing channel with an included angle R smaller than 180 degrees is arranged at the top of the working cavity, and the included angle R is smaller than 180 degrees, so that the influence on deposition reaction during air supplementing is avoided. One side of the waste gas cavity is provided with an exhaust channel for exhausting waste gas. High-cleanness inert gas is introduced into the reaction cavity through the air supplementing channel, the air supplementing speed ranges from 2 m/s to 10m/s, the air supplementing speed is ensured to be not less than the air exhausting speed of the air exhausting micropore, and the positive pressure in the reaction cavity is maintained 。 Exhausting and exhausting are carried out through the exhaust channel, waste gas and silicon dioxide in the deposition production process enter the waste gas cavity through the exhaust micropores, and then are exhausted through the exhaust channel, the air speed range of exhaust is 2-10m/s, and the negative pressure of the waste gas cavity is kept. In the prior art, the atmosphere in the reaction chamber is maintained by using air which is efficiently filtered as clean air, but various impurities are easily introduced in the ventilation process, so that various optical indexes of the material are deteriorated. Therefore, in the embodiment of the present invention, highly clean inert gas having a purity of 5N or more may be used as clean wind instead of efficiently filtered air, and the circulation flow of the gas in the chamber may be maintained while maintaining the atmosphere in the reaction chamber.
In addition, the invention also provides a preparation method of the large-size infrared synthetic quartz material, which utilizes the preparation device of the large-size infrared synthetic quartz material, and the preparation method is an upward growth method, so that the technical problems that the prepared loose body is weak in strength and difficult to burn through due to the fact that the density of the loose body is small and pores exist in the loose body in the existing downward growth method are well solved, and the size of the infrared synthetic quartz is not suitable to be excessively large are solved.
In conclusion, the invention well solves the problems existing in the prior art and realizes the beneficial effect of obtaining the large-size infrared synthetic quartz.
Drawings
In order that the invention may be more readily understood, a more particular description of the invention will be rendered by reference to specific embodiments thereof that are illustrated in the appended drawings.
FIG. 1 is a schematic diagram of a device for preparing an embodiment of a device and method for preparing a large-size infrared synthetic quartz material according to the present invention;
FIG. 2 is a schematic diagram showing a uniform arrangement of burner assemblies according to an embodiment of an apparatus and method for manufacturing a large-sized infrared synthetic quartz material according to the present invention;
FIG. 3 is a schematic diagram of a torch assembly of an embodiment of an apparatus and method for producing a large-sized infrared synthetic quartz material according to the present invention, which is uniformly distributed along concentric circles;
Description of the specification reference numerals: 1. a furnace body; 11. a quartz liner; 2. a bottom cover; 21. a furnace bottom opening baffle; 211. exhausting micropores; 22. a positioning block; 23. a return spring; 24. a bearing; 25. a groove; 3. a support system; 4. a working chamber; 41. a reaction chamber; 411. an air supplementing channel; 42. a waste gas chamber; 421. an air draft channel; 5. a deposition crucible; 6. a torch assembly; 60. a mounting plate; 61. producing a blast lamp; 62. a dehydroxylation pre-degassing torch; 63. titanium-containing halide torches; 7. loosening the quartz ingot.
Detailed Description
The present invention will be further described with reference to the accompanying drawings and specific examples, which are not intended to be limiting, so that those skilled in the art will better understand the invention and practice it.
Referring to fig. 1, a large-sized infrared synthetic quartz material preparing apparatus of the present invention is hereinafter simply referred to as "the present preparing apparatus". The preparation device comprises a furnace body 1, a bottom cover 2 arranged below the furnace body 1, a supporting system 3 which is arranged at the center of the bottom cover 2 and can be rotationally lifted under the drive of a power device, and a deposition crucible 5 fixedly arranged at the top of the supporting system 3. The furnace body 1 and the bottom cover 2 together form a working cavity 4, and the supporting system 3 can also transversely move under the drive of the power device. The power device can adopt any known form, and only needs to meet the requirement that the support system 3 can repeatedly move transversely while rotating and lifting, and is not repeated here. In this embodiment, the power device includes three stepper motors, wherein an output end of one stepper motor is fixedly connected with the support system 3, and is used for driving the support system 3 to perform rotational movement; the output ends of the other two stepping motors are connected with gears which are meshed with racks to respectively drive the supporting system 3 to lift and move transversely. Compared with the prior art, the deposition crucible 5 is fixedly arranged at the top of the supporting system 3, so that the preparation device can be used for implementing an upward growth method, namely, the raw materials in the deposition crucible 5 are deposited from bottom to top to form loose bodies, and compared with the downward growth method adopted in the prior art, the upward growth method implemented by using the preparation device can enable the loose bodies to have the advantages of increased density, higher strength, difficult cracking and falling under the action of gravity, and meanwhile, only a small amount of or even no air holes exist in the loose bodies. The bottom cover 2 of the present invention is provided with a bottom mouth baffle plate 21, and the bottom mouth baffle plate 21 divides the working chamber 4 into a reaction chamber 41 and an exhaust gas chamber 42. The furnace bottom opening baffle 21, the deposition crucible 5 and the support system 3 are synchronously moved transversely. The repeated traversing of the deposition crucible 5 causes the deposited loose powder to be repeatedly dithered, so that the loose powder density is greater and the growth process is more uniform. The bottom baffle 21 is provided with an exhaust micropore 211, and exhaust gas and silicon dioxide in the reaction cavity 41 are uniformly led out through the exhaust micropore 211, so that the stability and consistency of a flow field in the reaction cavity 41 are ensured. The burner assembly 6 is installed above the furnace body 1, the burner assembly 6 is an assembly comprising at least one production burner 61, at least one dehydroxylation pre-degassing burner 62 and at least one titanium-containing halide burner 63, the production burner 61, the dehydroxylation pre-degassing burner 62 and the titanium-containing halide burner 63 are arranged on the mounting plate 60, and the three burners are the same in number and are uniformly arranged with each other. As used herein, "uniformly aligned with each other" means that:
When the production burner 61, the dehydroxylation pre-degassing burner 62, and the titanium-containing halide burner 63 are all one:
mode one: the production burner 61, the pre-dehydroxylation degassing burner 62, and the titanium-containing halide burner 63 may be aligned in a straight line, i.e., the centers of the production burner 61, the pre-dehydroxylation degassing burner 62, and the titanium-containing halide burner 63 are on the same straight line, and the distances between the centers of adjacent ones of the production burner 61, the pre-dehydroxylation degassing burner 62, and the titanium-containing halide burner 63 are equal.
Mode 2: the production burner 61, the dehydroxylation pre-degassing burner 62, and the titanium-containing halide burner 63 may be arranged in a triangle, i.e., the center lines of the production burner 61, the dehydroxylation pre-degassing burner 62, and the titanium-containing halide burner 63 are equilateral triangles.
When the production burner 61, the dehydroxylation pre-degassing burner 62, and the titanium-containing halide burner 63 are all plural:
three production torches 61, dehydroxylation pre-degassing torches 62 and titanium-containing halide torches 63 are taken as examples.
Mode one: referring to fig. 2, three production torches 61 are one production torch group, and centers of the three production torches 61 are on the same straight line, and at the same time, distances between centers of adjacent two production torches 61 are equal; the three dehydroxylation pre-degassing blast lamps 62 are a dehydroxylation pre-degassing blast lamp set, the centers of the three dehydroxylation pre-degassing blast lamps 62 are on the same straight line, and meanwhile, the distances between the centers of two adjacent dehydroxylation pre-degassing blast lamps 62 are equal; the three titanium-containing halide lamps 63 are one titanium-containing halide lamp group, and the centers of the three titanium-containing halide lamps 63 are on the same straight line, and at the same time, the distances between the centers of two adjacent titanium-containing halide lamps 63 are equal.
The three rows of production burner groups, dehydroxylation pre-degassing burner groups and titanium-containing halide burner groups are arranged correspondingly, namely for example: the three production torches 61 correspond to three dehydroxylation pre-degassing torches 62, the three dehydroxylation pre-degassing torches 62 correspond to three titanium-containing halide torches 63, in which case the distance of the center of the three production torches 61 from the center of the three dehydroxylation pre-degassing torches 62 is equal to the distance of the center of the three dehydroxylation pre-degassing torches 62 from the center of the three titanium-containing halide torches 63.
Mode two: referring to fig. 3, three production torches 61 are one production torch group, and centers of the three production torches 61 are on the same straight line, and at the same time, distances between centers of adjacent two production torches 61 are equal; the three dehydroxylation pre-degassing blast lamps 62 are a dehydroxylation pre-degassing blast lamp set, the centers of the three dehydroxylation pre-degassing blast lamps 62 are on the same straight line, and meanwhile, the distances between the centers of two adjacent dehydroxylation pre-degassing blast lamps 62 are equal; the three titanium-containing halide lamps 63 are one titanium-containing halide lamp group, and the centers of the three titanium-containing halide lamps 63 are on the same straight line, and at the same time, the distances between the centers of two adjacent titanium-containing halide lamps 63 are equal.
The straight line formed by the center lines of the three production torches 61, the straight line formed by the center lines of the three pre-dehydroxylation degassing torches 62, and the straight line formed by the center lines of the three titanium-containing halide torches 63 intersect at the same point, which is called an intersection point, which is equal to the distance from its nearest production torch 61 to the connected two production torches 61, which is equal to the distance from its nearest pre-dehydroxylation degassing torch 62 to the adjacent two pre-dehydroxylation degassing torches 62, which is equal to the distance from its nearest titanium-containing halide torch 63 to the connected two titanium-containing halide torches 63.
The gaseous silicon tetrachloride raw material is introduced into the reaction cavity 41 through the production blast lamp 61 for deposition production, the chlorine and helium mixed gas is introduced into the reaction cavity 41 through the dehydroxylation pre-degassing blast lamp 62 for dehydroxylation pretreatment, and the titanium-containing halide blast lamp 63 is introduced into the reaction cavity 41 for titanium doping treatment, so that the dehydroxylation and the titanium doping treatment can be simultaneously carried out in the deposition production process, the purposes of synchronous deposition and synchronous process treatment are realized, the problem that the hydroxyl content gradually decreases from the core part to the edge due to dehydration in the sintering process is solved, the purposes of uniform distribution and stable doping of the titanium compound are realized, and the optical uniformity of the material is also improved.
Production burner 61, dehydroxylation pre-degassing burner 62, and titanium-containing halide burner 63
Specifically, the installation of the furnace body 1 and the bottom cover 2 can adopt any known form, and only the joints can be sealed by meeting the requirement, which is not repeated here. In the embodiment, the furnace body 1 and the bottom cover 2 are connected through bolts, and a sealing gasket is arranged at the joint. The deposition crucible 5 may be mounted on top of the support system 3 in any known manner, provided that the mounting strength is ensured at high temperature, for example: welding, screwing, etc., the deposition crucible 5 in this embodiment is welded on top of the support system 3. In addition, a groove 25 is provided in the bottom cover 2 at a position where the bottom mouth baffle 21 is arranged, both ends of the bottom mouth baffle 21 extend into the groove 25, and both ends of the bottom mouth baffle 21 and the bottom D of the groove 25 form a moving gap so that both ends of the bottom mouth baffle 21 can be laterally moved in the groove XX. In order to ensure smooth movement of the hearth opening baffle 21, the thickness H of the hearth opening baffle 21 may be slightly smaller than the height L of the groove 25, and the specific dimensions are such that the hearth opening baffle 21 can move smoothly. Further, the end part of the furnace bottom opening baffle 21 extending into the groove 25 can be provided with a positioning block 22, the thickness M of the positioning block 22 is larger than the thickness H of the furnace bottom opening baffle 21, the furnace bottom opening baffle 21 is arranged in the middle of the positioning block 22, and the upper surface and the lower surface of the furnace bottom opening baffle 21 are not contacted with the inner wall of the groove 25, so that the furnace bottom opening baffle 21 has the functions of: in the process that the furnace bottom opening baffle 21 transversely moves under the drive of the support system 3, only the positioning block 22 is always in contact with the inner wall of the groove 25, and the purpose of reducing friction force can be realized by reducing the contact area of the positioning block 22 and the inner wall of the groove 25 as much as possible by adjusting the size of the positioning block 22, for example: the bottom area of the positioning block 22 can be reduced to reduce the contact area between the bottom surface of the positioning block 22 and the inner wall of the bottom of the groove 25, so as to realize the effect of reducing friction force. That is, the positioning block 22 achieves the purpose of reducing friction while ensuring the lateral movement stability of the furnace bottom opening baffle 21. In addition, in order to avoid the impact of the positioning block 22 on the bottom D of the groove 25, a buffer device may be installed between the positioning block 22 and the bottom D of the groove 25, and the buffer device may take any one of the conventional known forms, which only needs to satisfy the requirement of high temperature resistance while slowing down the impact of the positioning block 22 on the bottom D of the groove 25. In this embodiment, the return spring 23 is selectively installed between the positioning block 22 and the bottom D of the groove 25, and when the bottom baffle 21 is driven by the support system 3 to move toward the bottom D of the groove 25, the return spring 23 is compressed, and the return spring 23 buffers the impact of the positioning block 22 to the bottom D of the groove 25. When the furnace bottom baffle 21 moves away from the bottom D of the groove 25 under the drive of the support system 3, the return spring 23 stretches and returns. Because the supporting system 3 drives the furnace bottom baffle plate 21 to repeatedly move transversely and also has rotary lifting motion relative to the furnace bottom baffle plate 21, a bearing 24 can be arranged on one side of the furnace bottom baffle plate 21, which is close to the supporting system 3, so that the connection position can form a closed working environment and simultaneously friction resistance is reduced.
Optionally, the material of the furnace body 1 can be a ceramic fiber material for heat preservation and heat insulation so as to isolate the temperature of the external environment and ensure that the reaction is smoothly carried out. In addition, the inner side of the furnace body 1 can be provided with a quartz lining 11 to avoid the problems of loose body purity reduction, material transmittance deterioration, light absorption, laser damage resistance threshold and other key indexes deterioration caused by metal impurities in the cavity. The quartz liner 11 may be installed in any known manner, and it is only necessary to form a clean reaction chamber 41 while being resistant to high temperatures. In this embodiment, the quartz lining 11 is in interference fit with the furnace body 1, and is inlaid inside the furnace body 1.
Optionally, at least one air compensating channel 411 with an included angle R smaller than 180 degrees with the side wall of the furnace body 1 is arranged at the top of the working cavity 4, and a plurality of air compensating channels 411 can be optionally arranged. An exhaust channel 421 for exhausting exhaust gas may be further provided at one side of the exhaust chamber 42. The included angle R between the air supplementing channel 411 and the side wall of the furnace body 1 is smaller than 180 degrees, so that the influence on the deposition reaction during air supplementing is avoided. In the deposition process, the gas maintaining the atmosphere in the reaction chamber 41 enters the reaction chamber 41 through the air supplementing channel 411, so that the waste gas and silicon dioxide in the deposition process are driven to enter the waste gas chamber 42 through the air exhausting micropores 211, and then are exhausted through the air exhausting channel 421. During the deposition production process, air in the reaction cavity 41 is discharged into the waste air cavity 42 through the air draft micropores 211 while supplementing air, and the air speed range of the air supplement is 2-10m/s, so that the continuous positive pressure in the reaction cavity 41 is required to be satisfied. When the air pressure in the reaction chamber 41 is small, the wind speed of the air supply is appropriately increased in the wind speed range of the air supply, and when the air pressure in the reaction chamber 41 is large, the wind speed of the air supply is appropriately decreased in the wind speed range of the air supply. In the deposition production process, after the gas in the reaction cavity 41 is discharged into the exhaust cavity 42 through the exhaust micropores 211, the gas is discharged through the exhaust channel 421, and the exhaust wind speed range is 2-10m/s, so that the continuous negative pressure in the exhaust cavity 42 is required to be satisfied. When the negative pressure in the exhaust chamber 42 is small, the wind-drawing wind speed is appropriately increased in the wind-drawing wind speed range, and when the negative pressure in the reaction chamber 41 is large, the wind-drawing wind speed is appropriately decreased in the wind-supplementing wind speed range.
Alternatively, the inner diameter of the deposition crucible 5 may be not less than 1100mm and the depth may be not less than 600mm. The material of the deposition crucible 5 may be any one of high-purity, high-temperature-resistant ceramic materials having a total content of metallic impurities of not more than 500ppm and a melting point higher than 1500 deg.c, and the size of the deposition crucible 5 is determined according to the number of three torches and the required diameter of the loose body. In this example, the inner diameter of the deposition crucible 5 is 1100mm, the depth is 600mm, and the material is zirconia ceramics with high cleanness and high temperature resistance.
The second aspect of the embodiment of the present invention also provides a method for preparing a large-size infrared synthetic quartz material, which is applied to the preparation device in the above embodiment, and specific embodiments are as follows:
example 1:
step S1: hydrogen and oxygen are introduced into the reaction chamber 41 through the production torch 61, and the hydrogen and the oxygen are combusted to form oxyhydrogen flame, so that the reaction chamber 41 is heated and preheated;
optionally, in step S1, the hydrogen and oxygen are high-purity gases with a purity of 5N or more; the flow rate of hydrogen ranges from 75L/min to 230L/min, and the flow rate of oxygen ranges from 50L/min to 150L/min. In this embodiment, in step S1, the flow rate of hydrogen is 75L/min and the flow rate of oxygen is 50L/min. The hydrogen and oxygen are introduced into the reaction chamber 41 by the production burner 61 and then ignited to form oxyhydrogen flame, and meanwhile, the temperature in the reaction chamber 41 is increased, so that the effect of heating and preheating is achieved.
Step S2: argon is introduced into the reaction chamber 41 through the production blowlamp 61 when the temperature in the reaction chamber 41 reaches 800 ℃;
optionally, in step S2, argon is high-purity gas with purity of 5N, and the flow rate of the argon is 20-80L/min. In this embodiment, in step S2, the flow rate range of argon is 20L/min. The bulk deposition reaction needs to be carried out at 800 ℃ or higher, but the temperature in the reaction chamber 41 is not preferably too high due to the limitation of the preparation apparatus. Therefore, when the temperature in the reaction chamber 41 reaches 800 ℃, the hydrogen gas and the oxygen gas are introduced into the reaction chamber 41 through the production torch 61, and the argon gas is introduced into the reaction chamber 41 through the production torch 61. Argon is a typical inert gas, and the concentration of hydrogen and oxygen is reduced while maintaining the atmosphere in the reaction chamber 41 by introducing argon, so that the combustion reaction is suppressed and the temperature is prevented from being greatly increased in a short time.
Step S3: raising the support system 3 to a deposition reaction position, wherein the lower end of the blast lamp assembly 6 is positioned 300-500mm above the inner bottom of the deposition crucible 5;
specifically, the deposition reaction is essentially performed by charging the raw material into the deposition crucible 5 of the reaction chamber 41 by the production torch 61 to form silica, and depositing and growing the silica on the deposition crucible 5 to form a loose body. Since the blast lamp has a certain speed when spraying the raw material, and the raw material reaction also needs a certain time, the distance between the lower end of the blast lamp assembly 6 and the bottom of the deposition crucible 5 should not be too small, and in this embodiment, the lower end of the blast lamp assembly 6 is located 300mm above the bottom of the deposition crucible 5.
Step S4: when the temperature in the reaction chamber 41 is lower than 900 ℃, stopping introducing argon into the reaction chamber 41; when the temperature in the reaction chamber 41 is higher than 900 ℃, argon gas is continuously introduced into the reaction chamber 41. When the temperature in the reaction cavity 41 is stabilized at 800-1000 ℃, the gaseous silicon tetrachloride raw material is introduced into the deposition crucible 5 through the production blowlamp 61 for deposition production to generate loose powder, and the loose powder is piled up in the deposition crucible 5 to form a loose quartz ingot 7. At the same time of deposition production, a dehydroxylation pre-degassing blast lamp 62 is used for introducing a mixed gas of chlorine and helium into the deposition crucible 5 and carrying out dehydroxylation pre-treatment on the loose quartz ingot 7. Simultaneously, a titanium halide-containing blast lamp 63 introduces titanium halide into the deposition crucible 5, and the bulk quartz ingot 7 is subjected to titanium doping treatment. The usual titanium halides are TiCl 4 、TiCl 3 、TiCl 2 、TiOCl 2 TiOCl and TiI 4 The present example uses TiCl 4 The bulk quartz ingot 7 was subjected to a titanium doping treatment as a titanium halide.
Optionally, in the step S4, the flow rate of the gaseous silicon tetrachloride raw material ranges from 20L/min to 40L/min. Chlorine and helium are high-purity gases with the purity of more than 5N, and the molar ratio of the mixed gases of the chlorine and the helium is 1: and 0.75, wherein the flow rate of the mixed gas is 5-20L/min. The flow rate of the titanium halide is in the range of 3-20L/min. In the embodiment, in the step S4, the flow range of the gaseous silicon tetrachloride raw material is 20L/min; the flow range of the mixed gas of chlorine and helium is 5L/min; the flow rate of the titanium halide was in the range of 3L/min. The production torch 61 introduces a gaseous silicon tetrachloride raw material into the reaction chamber 41, and oxidizes the raw material in an oxyhydrogen flame atmosphere to form SiO 2 The silicon dioxide is deposited at the bottom of the deposition crucible 5 in a rotary descending state to form a loose body rod which grows upwards in the axial direction, and the loose body rod continuously rotates along with the deposition crucible 5 to descend and repeatedly transversely move, so that a loose body quartz ingot 7 with high and uniform density is formed. After the mixed gas of chlorine and helium is introduced into the reaction cavity 41, the hydroxyl groups in the loose body are removed, so that the problem of uneven dehydroxylation effect in the subsequent sintering process is avoided. The titanium-containing halide torch 63 introduces titanium halide into the reaction chamber 41 to perform titanium doping treatment, and improves the optical performance of the infrared synthetic quartz after sintering.
Step S5: in the deposition production process, the supporting system 3 and the deposition crucible 5 are driven by the power device to repeatedly move transversely while rotating downwards, and the furnace bottom baffle 21 is driven by the supporting system 3 to repeatedly move transversely. The distance between the lower end of the blast lamp component 6 and the top of the loose quartz ingot 7 is always controlled to be 300-500mm;
alternatively, in step S5, the rotation speed of the deposition crucible 5 is 15-50rpm and the traversing frequency is 60-300S/time, i.e., 60-300S are required for each oscillation of the deposition crucible 5. Meanwhile, when the deposition crucible 5 moves transversely, the projection below the blast lamp assembly 6 does not exceed the inner bottom of the deposition crucible 5. In this embodiment, in step S5, the rotation speed of the support system 3 is 15rpm and the traversing frequency is 60S/time. In the deposition production process, silicon dioxide is accumulated at the bottom of the deposition crucible 5, and the deposition crucible 5 always rotates at a certain speed, so that the distribution of the silicon dioxide at the bottom of the deposition crucible 5 is mainly concentric circles, and the silicon dioxide in a part of concentric circle areas is accumulated and raised, and the silicon dioxide in a part of concentric circle areas is accumulated and recessed, so that the density of the prepared loose body is uneven. In the invention, under the drive of the power device, the support system 3 can drive the deposition crucible 5 to repeatedly move transversely while rotating downwards, so that the silicon dioxide accumulated in the deposition crucible 5 is repeatedly shaken, and the silicon dioxide accumulation is more compact and even, thus a loose quartz ingot 7 with larger density and more even distribution can be prepared. The distance between the lower end of the blast lamp component 6 and the top of the loose quartz ingot 7 is consistent with that in the step S3, and is always controlled at 300mm. Because the loose quartz ingot 7 is continuously grown, the height of the deposition crucible 5 needs to be adjusted at any time through the support system 3, and therefore, the distance between the lower end of the blast lamp assembly 6 and the top of the loose quartz ingot 7 allows an error, and the error range is controlled to be 2mm. High-clean inert gas is introduced into the reaction cavity 41 through the air supplementing channel 411, the air supplementing speed ranges from 2 m/s to 10m/s, and the positive pressure in the reaction cavity 41 is maintained. Exhaust is performed through the exhaust passage 421 so that exhaust gas and silica in the deposition process enter the exhaust chamber 42 through the exhaust micro holes 211 and are then discharged through the exhaust passage 421. The wind speed of the draft is in the range of 2-10m/s, and the negative pressure in the exhaust cavity 42 is maintained.
In the prior art, the atmosphere in the reaction chamber 41 is maintained by the air which is efficiently filtered as clean air, and impurities are easily introduced during the air ventilation process, so that key indexes such as the transmittance, the light absorption characteristic, the laser damage resistance threshold and the like of the material are deteriorated. In this embodiment, highly clean inert gas is used as clean air instead of efficiently filtered air, and the circulation flow of the gas in the chamber is ensured while maintaining the atmosphere of the working space. The inert gases include helium, argon and nitrogen, and any known inert gas can be selected as the inert gas with high purity in the embodiment, and the purity is not less than 3N.
Step S6: after depositing for 80 hours, loose quartz ingots 7 with the weight not less than 250kg are obtained, then the process ending, material stopping and gas stopping operations are carried out, and the waste gas in the production process is discharged into a professional waste gas treatment device; and transferring the loose quartz ingot 7 into a sintering furnace for vitrification sintering to finally obtain the infrared synthetic quartz rod with the diameter of 600 mm.
Example 2:
step S1: hydrogen and oxygen are introduced into the reaction chamber 41 through the production torch 61, and the hydrogen and the oxygen are combusted to form oxyhydrogen flame, so that the reaction chamber 41 is heated and preheated;
Optionally, in step S1, the hydrogen and oxygen are high-purity gases with a purity of 5N or more; the flow rate of hydrogen ranges from 75L/min to 230L/min, and the flow rate of oxygen ranges from 50L/min to 150L/min. In this embodiment, in step S1, the flow rate range of hydrogen is 230L/min, and the flow rate range of oxygen is 150L/min. The hydrogen and oxygen are introduced into the reaction chamber 41 by the production burner 61 and then ignited to form oxyhydrogen flame, and meanwhile, the temperature in the reaction chamber 41 is increased, so that the effect of heating and preheating is achieved.
Step S2: argon is introduced into the reaction chamber 41 through the production blowlamp 61 when the temperature in the reaction chamber 41 reaches 800 ℃;
optionally, in step S2, argon is high-purity gas with purity of 5N, and the flow rate of the argon is 20-80L/min. In this embodiment, in step S2, the flow rate range of argon is 80L/min. The bulk deposition reaction needs to be carried out at 800 ℃ or higher, but the temperature in the reaction chamber 41 is not preferably too high due to the limitation of the preparation apparatus. Therefore, when the temperature in the reaction chamber 41 reaches 800 ℃, the hydrogen gas and the oxygen gas are introduced into the reaction chamber 41 through the production torch 61, and the argon gas is introduced into the reaction chamber 41 through the production torch 61. Argon is a typical inert gas, and the concentration of hydrogen and oxygen is reduced while maintaining the atmosphere in the reaction chamber 41 by introducing argon, so that the combustion reaction is suppressed and the temperature is prevented from being greatly increased in a short time.
Step S3: raising the support system 3 to a deposition reaction position, wherein the lower end of the blast lamp assembly 6 is positioned 300-500mm above the inner bottom of the deposition crucible 5;
specifically, the deposition reaction is essentially performed by charging the raw material into the deposition crucible 5 of the reaction chamber 41 by the production torch 61 to form silica, and depositing and growing the silica on the deposition crucible 5 to form a loose body. Since the blast lamp has a certain speed when spraying the raw material, and the raw material reaction also needs a certain time, the distance between the lower end of the blast lamp assembly 6 and the bottom of the deposition crucible 5 should not be too small, and in this embodiment, the lower end of the blast lamp assembly 6 is located above the bottom of the deposition crucible 5 by 500 mm.
Step S4: when the temperature in the reaction chamber 41 is lower than 900 ℃, stopping introducing argon into the reaction chamber 41; when the temperature in the reaction chamber 41 is higher than 900 ℃, argon gas is continuously introduced into the reaction chamber 41. When the temperature in the reaction cavity 41 is stabilized at 800-1000 ℃, the gaseous silicon tetrachloride raw material is introduced into the deposition crucible 5 through the production blowlamp 61 for deposition production to generate loose powder, and the loose powder is piled up in the deposition crucible 5 to form a loose quartz ingot 7. At the same time of deposition production, a dehydroxylation pre-degassing blast lamp 62 is used for introducing a mixed gas of chlorine and helium into the deposition crucible 5 and carrying out dehydroxylation pre-treatment on the loose quartz ingot 7. Simultaneously, a titanium halide-containing blast lamp 63 introduces titanium halide into the deposition crucible 5, and the bulk quartz ingot 7 is subjected to titanium doping treatment. Typical titanium halides are TiCl4, tiCl3, tiCl2, tiOCl and TiI4, and this example uses TiCl4 as the titanium halide to titanium dope the bulk quartz ingot 7.
Optionally, in the step S4, the flow rate of the gaseous silicon tetrachloride raw material ranges from 20L/min to 40L/min. Chlorine and helium are high-purity gases with the purity of more than 5N, and the molar ratio of the mixed gases of the chlorine and the helium is 1: and 0.75, wherein the flow rate of the mixed gas is 5-20L/min. The flow rate of the titanium halide is in the range of 3-20L/min. In the embodiment, in the step S4, the flow range of the gaseous silicon tetrachloride raw material is 40L/min; the flow range of the mixed gas of chlorine and helium is 20L/min; the flow rate of the titanium halide was in the range of 20L/min. The production blowlamp 61 is filled with gaseous silicon tetrachloride raw material into the reaction cavity 41, the gaseous silicon tetrachloride raw material is oxidized in oxyhydrogen flame atmosphere to form SiO2 silicon dioxide, the silicon dioxide is deposited at the bottom of the deposition crucible 5 in a rotary descending state to form a loose body rod which grows upwards in the axial direction, and the loose body rod continuously rotates, descends along with the deposition crucible 5 and repeatedly moves transversely to form a loose body quartz ingot 7 with high and uniform density. After the mixed gas of chlorine and helium is introduced into the reaction cavity 41, the hydroxyl groups in the loose body are removed, so that the problem of uneven dehydroxylation effect in the subsequent sintering process is avoided. The titanium-containing halide torch 63 introduces titanium halide into the reaction chamber 41 to perform titanium doping treatment, and improves the optical performance of the infrared synthetic quartz after sintering.
Step S5: in the deposition production process, the supporting system 3 and the deposition crucible 5 are driven by the power device to repeatedly move transversely while rotating downwards, and the furnace bottom baffle 21 is driven by the supporting system 3 to repeatedly move transversely. The distance between the lower end of the blast lamp component 6 and the top of the loose quartz ingot 7 is always controlled to be 300-500mm;
alternatively, in step S5, the rotation speed of the deposition crucible 5 is 15-50rpm and the traversing frequency is 60-300S/time, i.e., 60-300S are required for each oscillation of the deposition crucible 5. Meanwhile, when the deposition crucible 5 moves transversely, the projection below the blast lamp assembly 6 does not exceed the inner bottom of the deposition crucible 5. In this embodiment, in step S5, the rotation speed of the support system 3 is 50rpm and the traversing frequency is 300S/time. In the deposition production process, silicon dioxide is accumulated at the bottom of the deposition crucible 5, and the deposition crucible 5 always rotates at a certain speed, so that the distribution of the silicon dioxide at the bottom of the deposition crucible 5 is mainly concentric circles, and the silicon dioxide in a part of concentric circle areas is accumulated and raised, and the silicon dioxide in a part of concentric circle areas is accumulated and recessed, so that the density of the prepared loose body is uneven. In the invention, under the drive of the power device, the support system 3 can drive the deposition crucible 5 to repeatedly move transversely while rotating downwards, so that the silicon dioxide accumulated in the deposition crucible 5 is repeatedly shaken, and the silicon dioxide accumulation is more compact and even, thus a loose quartz ingot 7 with larger density and more even distribution can be prepared. The distance between the lower end of the blast lamp component 6 and the top of the loose quartz ingot 7 is consistent with the distance in the step S3, and is always controlled to be 500mm. Because the loose quartz ingot 7 is continuously grown, the height of the deposition crucible 5 needs to be adjusted at any time through the support system 3, and therefore, the distance between the lower end of the blast lamp assembly 6 and the top of the loose quartz ingot 7 allows an error, and the error range is controlled to be 2mm. High-clean inert gas is introduced into the reaction cavity 41 through the air supplementing channel 411, the air supplementing speed ranges from 2 m/s to 10m/s, and the positive pressure in the reaction cavity 41 is maintained. Exhaust is performed through the exhaust passage 421 so that exhaust gas and silica in the deposition process enter the exhaust chamber 42 through the exhaust micro holes 211 and are then discharged through the exhaust passage 421. The wind speed of the draft is in the range of 2-10m/s, and the negative pressure in the exhaust cavity 42 is maintained.
In the prior art, the atmosphere in the reaction chamber 41 is maintained by the air which is efficiently filtered as clean air, and impurities are easily introduced during the air ventilation process, so that key indexes such as the transmittance, the light absorption characteristic, the laser damage resistance threshold and the like of the material are deteriorated. In this embodiment, highly clean inert gas is used as clean air instead of efficiently filtered air, and the circulation flow of the gas in the chamber is ensured while maintaining the atmosphere of the working space. The inert gases include helium, argon and nitrogen, and any known inert gas can be selected as the inert gas with high purity in the embodiment, and the purity is not less than 3N.
Step S6: after 50 hours of deposition, loose quartz ingots 7 with the weight not less than 250kg are obtained, then the process ending, material stopping and gas stopping operations are carried out, and the waste gas in the production process is discharged into a professional waste gas treatment device; and transferring the loose quartz ingot 7 into a sintering furnace for vitrification sintering to finally obtain the infrared synthetic quartz rod with the diameter of 600 mm.
The efficiency of the existing VAD process and the loose body prepared by the embodiment of the invention and the performance of the prepared infrared synthetic quartz are shown in the following table:
As can be seen from the above table, compared with the existing VAD process, the method provided by the invention can be used for preparing the infrared synthetic quartz with the diameter of 600 mm. Meanwhile, the deposition efficiency of the loose body is greatly improved, the metal impurities are reduced by ten times, the expansion coefficient of the infrared synthetic quartz is reduced, the optical performance is obviously improved, and the application requirements of the photoelectric technical field can be further met.
In the present invention, unless explicitly specified and limited otherwise, the terms "mounted," "connected," "secured," and the like are to be construed broadly and include, for example, either fixedly attached, detachably attached, or integrally formed; can be mechanically or electrically connected; can be directly connected or indirectly connected through an intermediate medium; may be a communication between two elements or an interaction between two elements. The specific meaning of the above terms in the present invention can be understood by those of ordinary skill in the art according to the specific circumstances.
In the present invention, unless expressly stated or limited otherwise, a first feature is "on" or "under" a second feature, which may be in direct contact with the first and second features, or in indirect contact with the first and second features via an intervening medium. Moreover, a first feature "above," "over" and "on" a second feature may be a first feature directly above or obliquely above the second feature, or simply indicate that the first feature is higher in level than the second feature. The first feature being "under", "below" and "beneath" the second feature may be the first feature being directly under or obliquely below the second feature, or simply indicating that the first feature is level lower than the second feature.
It is apparent that the above examples are given by way of illustration only and are not limiting of the embodiments. Other variations and modifications of the present invention will be apparent to those of ordinary skill in the art in light of the foregoing description. It is not necessary here nor is it exhaustive of all embodiments. And obvious variations or modifications thereof are contemplated as falling within the scope of the present invention.
Claims (10)
1. The preparation device of the large-size infrared synthetic quartz material comprises a furnace body (1), a bottom cover (2) arranged below the furnace body (1), a supporting system (3) which is arranged at the center of the bottom cover (2) and can be rotated and lifted under the drive of a power device, and a deposition crucible (5) connected with the supporting system (3); the furnace body (1) and the bottom cover (2) jointly form a working cavity (4), and the furnace is characterized in that: the deposition crucible (5) is fixedly arranged at the top of the supporting system (3); the supporting system (3) can transversely move under the drive of the power device; the bottom cover (2) is provided with a furnace bottom opening baffle plate (21) which can transversely move under the drive of the supporting system (3) to divide the working cavity (4) into a reaction cavity (41) and an exhaust gas cavity (42); the furnace bottom opening baffle (21) is provided with an air draft micropore (211); a blast lamp component (6) is arranged above the deposition crucible (5).
2. The apparatus for producing a large-size infrared synthetic quartz material according to claim 1, wherein: the furnace body (1) is made of ceramic fiber materials, and a quartz lining (11) is arranged on the inner side of the furnace body.
3. The apparatus for producing a large-size infrared synthetic quartz material according to claim 2, wherein: at least one air supplementing channel (411) with an included angle R smaller than 180 degrees with the side wall of the furnace body (1) is arranged at the top of the reaction cavity (41) and is used for introducing inert gas; one side of the waste gas cavity (42) is provided with an exhaust channel (421) for exhausting waste gas.
4. A device for preparing a large-size infrared synthetic quartz material according to claim 3, wherein: the burner assembly (6) comprises a production burner (61), a dehydroxylation pre-degassing burner (62) and a titanium-containing halide burner (63); the production burner (61), the dehydroxylation pre-degassing burner (62) and the titanium-containing halide burner (63) are all in the same number, at least one; the production burner (61), the dehydroxylation pre-degassing burner (62) and the titanium-containing halide burner (63) are uniformly arranged therebetween.
5. The device for preparing the large-size infrared synthetic quartz material according to claim 4, wherein the device comprises: the inner diameter of the deposition crucible (5) is not smaller than 1100mm, the depth is not smaller than 600mm, and the material of the deposition crucible (5) is ceramic material.
6. A preparation method of a large-size infrared synthetic quartz material is characterized by comprising the following steps of: which is carried out with a device for the preparation of large-size infrared synthetic quartz material according to claim 4 or 5, comprising the following production steps:
step S1: introducing hydrogen and oxygen into the reaction cavity (41) through the production blowtorch (61), and forming oxyhydrogen flame after ignition so as to heat and preheat the reaction cavity (41);
step S2: when the temperature in the reaction cavity (41) reaches 800 ℃, argon is continuously introduced into the reaction cavity (41) through the production blowlamp (61);
step S3: lifting the support system (3) to a deposition reaction position, wherein the lower end of the blowtorch assembly (6) is positioned at a position 300-500mm above the inner bottom of the deposition crucible (5);
step S4: when the temperature in the reaction cavity (41) is stabilized at 800-1000 ℃, introducing gaseous silicon tetrachloride raw material into the deposition crucible (5) through the production blowlamp (61), and producing nano-scale silicon dioxide after the silicon tetrachloride undergoes hydrolysis reaction in the oxyhydrogen combustion process, wherein the nano-scale silicon dioxide is accumulated in the deposition crucible (5) to form a loose quartz ingot (7); while carrying out deposition production, introducing a chlorine gas and helium gas mixture into the deposition crucible (5) by the dehydroxylation pre-degassing blast lamp (62) to carry out dehydroxylation pre-treatment on the loose quartz ingot (7); simultaneously, the titanium-containing halide blast lamp (63) is used for introducing titanium halide into the deposition crucible (5) and carrying out titanium doping treatment on the loose quartz ingot (7);
Step S5: in the deposition production process, the supporting system (3) and the deposition crucible (5) are driven by a power device to repeatedly move transversely while rotating downwards, and the furnace bottom baffle (21) is driven by the supporting system (3) to repeatedly move transversely; the distance between the lower end of the blast lamp component (6) and the top of the loose quartz ingot (7) is always controlled to be 300-500mm; high-clean inert gas is introduced into the reaction cavity (41) through the air supplementing channel (411), and the air supplementing speed range is 2-10m/s; exhausting air through the air exhausting channel (421), wherein exhaust gas and silicon dioxide in the reaction cavity (41) enter the exhaust cavity (42) through the air exhausting micro holes (211) in the deposition production process, and then are exhausted through the air exhausting channel (421), and the air speed range of the air exhausting is 2-10m/s;
step S6: after deposition production for 50-80 hours, obtaining the loose quartz ingot (7) with the weight not less than 250kg, and then carrying out process ending and stopping operation; and transferring the loose quartz ingot (7) into a sintering furnace for vitrification sintering to finally obtain the infrared synthetic quartz rod with the diameter of 600 mm.
7. The method for preparing the large-size infrared synthetic quartz material according to claim 6, wherein the method comprises the following steps: in the step S1, hydrogen and oxygen are high-purity gases with the purity of more than 5N; the flow rate of hydrogen ranges from 75L/min to 230L/min, and the flow rate of oxygen ranges from 50L/min to 150L/min.
8. The method for preparing the large-size infrared synthetic quartz material according to claim 7, wherein the method comprises the following steps: in the step S2, argon is high-purity gas with the purity of 5N, and the flow rate of the argon is 20-80L/min.
9. The method for preparing the large-size infrared synthetic quartz material according to claim 8, wherein the method comprises the following steps: in the step S4, the flow range of the gaseous silicon tetrachloride raw material is 20-40L/min; chlorine and helium are high-purity gases with the purity of more than 5N, and the molar ratio of the mixed gases of the chlorine and the helium is 1:0.75, wherein the flow range of the mixed gas is 5-20L/min; the flow rate of the titanium halide is in the range of 3-20L/min.
10. The method for preparing the large-size infrared synthetic quartz material according to claim 9, wherein the method comprises the following steps: in the step S5, the rotating speed of the deposition crucible (5) is 15-50rpm, the traversing speed is 0.1-5m/S, the interval is +/-200 mm, and the rotation speed is a curve with maximum center speed and gradually decreasing towards the edge; when the deposition crucible (5) transversely moves, the lower projection of the blast lamp assembly (6) does not exceed the inner bottom of the deposition crucible (5).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310985729.8A CN116969669A (en) | 2023-08-07 | 2023-08-07 | Preparation device and method for large-size infrared synthetic quartz material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310985729.8A CN116969669A (en) | 2023-08-07 | 2023-08-07 | Preparation device and method for large-size infrared synthetic quartz material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN116969669A true CN116969669A (en) | 2023-10-31 |
Family
ID=88472990
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310985729.8A Pending CN116969669A (en) | 2023-08-07 | 2023-08-07 | Preparation device and method for large-size infrared synthetic quartz material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN116969669A (en) |
-
2023
- 2023-08-07 CN CN202310985729.8A patent/CN116969669A/en active Pending
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN1227171C (en) | Process and apparatus for manufacturing a glass ingot from synthetic silica | |
| EP1160209B1 (en) | Method and apparatus for manufacturing quartz glass ingot | |
| JP2014514236A (en) | Manufacture of silica housing | |
| CN1097737C (en) | Process for producing optical fiber preform | |
| JP5397857B2 (en) | Method and apparatus for producing quartz glass crucible | |
| KR102545712B1 (en) | Method and apparatus for manufacturing porous glass preform for optical fiber | |
| EP2067751A1 (en) | Method and device for manufacturing silica glass | |
| JP5500687B2 (en) | Method and apparatus for producing silica glass crucible | |
| JP5600687B2 (en) | Multi-nozzle tubular plasma deposition burner for producing preforms as semi-finished products for optical fibers | |
| JPH0686300B2 (en) | Soot-like silica body and method for producing the same | |
| CN102906038B (en) | Manufacture the method with the quartz glass crucibles of the transparent inwall be made up of synthetic quartz | |
| CN116969669A (en) | Preparation device and method for large-size infrared synthetic quartz material | |
| JP7428413B2 (en) | Synthetic quartz manufacturing method | |
| WO2006080294A1 (en) | Quartz glass preform for optical fiber and process for producing the same | |
| US8281620B1 (en) | Apparatus for manufacturing vitreous silica crucible | |
| CN108467186B (en) | Method for preventing large-size silicon dioxide loose body from cracking | |
| JP5485003B2 (en) | Optical fiber preform manufacturing method | |
| JP2010064934A (en) | Burner for producing synthetic silica glass, and apparatus for producing synthetic silica glass using the burner | |
| JP2009234860A (en) | Apparatus for producing synthetic silica glass tube and method for producing synthetic silica glass tube | |
| KR102636792B1 (en) | Synthetic quartz manufacturing facility that can prevent surface defects of deposits through improved exhaust performance | |
| JP3381309B2 (en) | Method for producing glass particle deposit | |
| CN117776505A (en) | Large-size high-uniformity synthetic quartz glass ingot deposition furnace and preparation method thereof | |
| JPH0585761A (en) | Porous glass base material | |
| CN108298798B (en) | Preparation device and method of large-size silica loose body | |
| JP3998228B2 (en) | Optical fiber porous base material, optical fiber glass base material, and manufacturing methods thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |