CN116536763A - Optical grade rutile monocrystal growth device and method - Google Patents
Optical grade rutile monocrystal growth device and method Download PDFInfo
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- CN116536763A CN116536763A CN202211102013.0A CN202211102013A CN116536763A CN 116536763 A CN116536763 A CN 116536763A CN 202211102013 A CN202211102013 A CN 202211102013A CN 116536763 A CN116536763 A CN 116536763A
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 59
- 238000000034 method Methods 0.000 title claims abstract description 25
- 230000003287 optical effect Effects 0.000 title claims abstract description 22
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 144
- 238000010438 heat treatment Methods 0.000 claims abstract description 102
- 239000000919 ceramic Substances 0.000 claims abstract description 94
- 230000003647 oxidation Effects 0.000 claims abstract description 42
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 42
- 230000005674 electromagnetic induction Effects 0.000 claims abstract description 41
- 239000013078 crystal Substances 0.000 claims abstract description 36
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 28
- 239000010431 corundum Substances 0.000 claims abstract description 28
- 230000006698 induction Effects 0.000 claims abstract description 15
- 238000004321 preservation Methods 0.000 claims abstract description 14
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 238000002844 melting Methods 0.000 claims description 23
- 230000008018 melting Effects 0.000 claims description 23
- 239000000463 material Substances 0.000 claims description 15
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 13
- 239000001301 oxygen Substances 0.000 claims description 13
- 229910052760 oxygen Inorganic materials 0.000 claims description 13
- 239000000843 powder Substances 0.000 claims description 11
- 239000000155 melt Substances 0.000 claims description 9
- 230000008569 process Effects 0.000 claims description 9
- 239000004408 titanium dioxide Substances 0.000 claims description 7
- 238000002347 injection Methods 0.000 claims description 6
- 239000007924 injection Substances 0.000 claims description 6
- 239000011449 brick Substances 0.000 claims description 5
- 239000011810 insulating material Substances 0.000 claims description 4
- 229910001220 stainless steel Inorganic materials 0.000 claims description 4
- 239000010935 stainless steel Substances 0.000 claims description 4
- 230000001276 controlling effect Effects 0.000 description 8
- 230000001105 regulatory effect Effects 0.000 description 6
- 238000009826 distribution Methods 0.000 description 5
- 239000007789 gas Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 230000001590 oxidative effect Effects 0.000 description 4
- 239000002131 composite material Substances 0.000 description 3
- 238000004134 energy conservation Methods 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 206010063385 Intellectualisation Diseases 0.000 description 1
- 238000000563 Verneuil process Methods 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000005672 electromagnetic field Effects 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/16—Oxides
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
- C30B11/003—Heating or cooling of the melt or the crystallised material
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
- C30B11/006—Controlling or regulating
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
- C30B11/04—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method adding crystallising materials or reactants forming it in situ to the melt
- C30B11/08—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method adding crystallising materials or reactants forming it in situ to the melt every component of the crystal composition being added during the crystallisation
- C30B11/10—Solid or liquid components, e.g. Verneuil method
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention relates to an optical grade rutile monocrystal growth device and method, comprising a heating section and a heat preservation section, wherein the heating section comprises an oxidation-resistant high-temperature conductive ceramic tube sleeved at the middle section of the zirconia ceramic tube, an induction coil is wound on the outer side of the oxidation-resistant high-temperature conductive ceramic tube, and the induction coil is controlled to be heated by an electromagnetic induction heating power supply system; the parts of the upper end and the lower end of the zirconia ceramic tube, which are not sleeved with the oxidation-resistant high-temperature conductive ceramic tube, are respectively provided with zirconia electrodes, and the zirconia electrodes are connected with an external resistance heating system through a water-cooling zirconia electrode busbar; the corundum base rod for seed crystal growth is arranged at the growth interface at the lower end of the heat preservation section, and the corundum base rod can realize no volatile matter pollution and accurate and controllable parameters at the temperature of about 2000 ℃ through an electromagnetic induction and resistance dual-heating system so as to meet the requirements of growing special high-temperature oxide single crystals such as high-quality rutile.
Description
Technical Field
The invention belongs to a special photoelectric functional crystal growth furnace, in particular to an optical grade rutile monocrystal growth device and method, and belongs to the field of monocrystal growth.
Background
Rutile single crystals are of great interest because of their excellent physicochemical properties. The preparation method is mainly characterized by high refractive index and double refractive index, good permeability in visible-infrared wave bands, and wide application in preparing devices such as optical isolators, optical circulators and the like in optical communication systems, refraction of electronic computers, polarizers, nicote prisms in polarizing microscopes, polarometers, photometers, gyroglycometers, interference laser resolvers, colorimeters for chemical analysis and the like, and is an indispensable material for modern national defense, aerospace and scientific research.
The flame fusion method growth furnace for growing large-size rutile monocrystal, which is used at present, uses oxyhydrogen flame as a heat source, and cannot form a growth environment of pure oxidizing gas. Meanwhile, due to the reasons of inaccurate control precision of air flow impact, temperature distribution and atmosphere distribution, larger axial temperature gradient, difficulty in realizing automatic control and the like, the quality of the rutile monocrystal grown in the furnace still has defects at present, the labor intensity is high, and the degree of automation is low.
The existing optical floating zone method for growing rutile monocrystal has the problems of complex procedures, limited growth size, poor growth stability and the like because the heating process is carried out inwards from the outer surface of the bar, the heat capacity of a molten pool is low, the prefabricated rod is prepared and the like.
The electromagnetic induction heating rutile monocrystal growing furnace used at present has the advantages that under the high temperature approaching 2000 ℃, silicon carbide, zirconium boride and other components serving as oxidation-resistant high-temperature conductive ceramic tubes volatilize to a certain extent, so that grown crystals are polluted, and the quality of the crystals is affected.
Disclosure of Invention
The technical problem to be solved by the invention is to provide an optical grade rutile monocrystal growth device and method, which can realize special high-temperature oxide monocrystal growth environments such as rutile under pure oxygen conditions without volatile pollution, with accurate and controllable parameters and easy realization of automation and intellectualization at a temperature of about 2000 ℃ through an electromagnetic induction and resistance dual-heating system so as to meet the requirements of growing high-quality rutile and other special high-temperature oxide monocrystals.
The present invention has been achieved in such a way that,
an optical grade rutile single crystal growth apparatus, the apparatus comprising:
the material injection section is used for carrying and injecting titanium dioxide powder into the furnace body by oxygen;
the device comprises a furnace body, a heating section and a heat preservation section, wherein the heating section comprises an oxidation-resistant high-temperature conductive ceramic tube sleeved on the middle section of the zirconia ceramic tube, an induction coil is wound on the outer side of the oxidation-resistant high-temperature conductive ceramic tube, and the induction coil is controlled to be heated through an electromagnetic induction heating power supply system; the zirconia electrodes are respectively arranged at the parts, which are not sleeved with the oxidation-resistant high-temperature conductive ceramic tubes, of the upper end and the lower end of the zirconia ceramic tube, and are connected with an external resistance heating system through a water-cooling zirconia electrode busbar; and a growth interface at the lower end of the heat preservation section is provided with a corundum base rod for seed crystal growth.
Further, the length of the heating section is 150mm, and the length of the heat preservation section is 180mm.
Further, the material injection section comprises a hopper and an inverted triangle material nozzle connected with the hopper, a vibrating rod is arranged on the central axis of the hopper, and the upper end of the vibrating rod is knocked according to frequency through a knocking hammer to generate vibration.
Further, part of the cooling section and the periphery from below the growth interface to the bottom of the corundum base rod for seed crystal growth are provided with a heat-insulating layer consisting of a growth furnace refractory brick, a growth furnace heat-insulating material and a stainless steel shell.
Further, the corundum base rod is of a lifting structure, and when molten drops continuously fall onto the melting cap, the corundum base rod is adjusted to move downwards, and melt on the melting cap is continuously crystallized.
Further, the system also comprises a control system for controlling the heating process of the resistance heating system and the electromagnetic induction heating power supply system, wherein the heating process comprises the following steps: the electromagnetic induction heating power supply system is started to perform electromagnetic induction heating, after the oxidation-resistant high-temperature conductive ceramic tube is heated, the zirconia ceramic tube in the oxidation-resistant high-temperature conductive ceramic tube is heated to the conductive temperature through heat conduction, the control system is automatically switched to the resistance heating system to heat, the zirconia ceramic tube is subjected to resistance heating, the zirconia ceramic tube and the inside of the zirconia ceramic tube are heated to the temperature required by the process, and the temperature condition required by the growth of rutile monocrystal is met;
the control system is used for controlling the lifting of the corundum base rod, and when molten drops continuously fall onto the melting cap, the corundum base rod is adjusted to move downwards, and the melt on the melting cap is continuously crystallized.
A method for preparing an optical grade rutile monocrystal, which is characterized by comprising the following steps:
controlling a resistance heating system and an electromagnetic induction heating power supply system to heat, starting the electromagnetic induction heating power supply system to perform electromagnetic induction heating, heating the zirconia ceramic tube inside the oxidation-resistant high-temperature conductive ceramic tube to a conductive temperature through heat conduction, and automatically switching the control system to the resistance heating system to heat, heating the zirconia ceramic tube in a resistance way, heating the zirconia ceramic tube and the inside of the zirconia ceramic tube to a temperature required by a process, and meeting a temperature condition required by growing rutile monocrystal;
carrying titanium dioxide powder into a furnace body from a hopper through a material nozzle by oxygen;
heating by a zirconia tube in a growth furnace heated by an electromagnetic induction and resistance dual-heating system to heat and melt the zirconia tube to form molten drops;
and controlling the lifting of the corundum base rod, and adjusting the corundum base rod to move downwards when the molten drops continuously fall onto the melting cap, so that the melt on the melting cap is continuously crystallized.
Further, the flow rate of oxygen was adjusted to 0.1m/s, the heating section was adjusted to 150mm, and the heat-insulating section was adjusted to 180mm.
Further, after the oxidation-resistant high-temperature ceramic tube is heated to 1200 ℃, the ceramic tube is automatically switched to a resistance heating system, and the zirconia ceramic tube is heated to 2400 ℃.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the rutile monocrystal growth method adopting the electromagnetic induction and resistance double heating system, firstly, a high-temperature resistant conductive ceramic tube is heated through electromagnetic induction, after the zirconia ceramic tube in the tube is heated to a conductive temperature (1200-1200 ℃), the heating system is automatically switched to the zirconia ceramic tube for resistance heating, the zirconia ceramic tube and the inside of the tube are heated to about 2000 ℃ required by the process, after the temperature is heated, the temperature distribution required by rutile monocrystal growth can be met, namely, the powder can be fully melted in the upper area of a crystal growth interface, the temperature of a crystallization point of 1850 ℃ is met at the crystal growth interface, the crystallization point temperature of the powder is lower than 1850 ℃ under the crystal growth interface, and the temperature condition required by growing rutile monocrystal is met.
2. The powder is carried by oxygen to enter the furnace body from the nozzle, so that the requirements of continuous feeding and pure oxidizing atmosphere required by the growth of rutile monocrystal can be met.
3. The induction heating is used for replacing oxyhydrogen flame heating, so that energy conservation and environmental protection can be achieved, and the danger in the production process is reduced.
4. As the zirconia tube of the resistance heating system is added in the oxidation-resistant high-temperature conductive ceramic tube, the phenomena of oxidation and volatilization of trace components existing at high temperature when the oxidation-resistant high-temperature conductive ceramic tube is directly used are effectively avoided, and the pollution to the grown crystal is avoided.
5. Compared with the currently used rutile monocrystal growth method heated by oxyhydrogen flame, the method can achieve accurate parameter control, is easy to realize automation, saves energy and protects environment, and reduces the risk in the production process.
Drawings
FIG. 1 is a schematic diagram of a device according to the present invention;
fig. 2 is a schematic view showing a temperature distribution state in the furnace body.
Detailed Description
The present invention will be described in further detail with reference to the following examples in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
The invention provides an optical grade rutile monocrystal growing device,
the material injection section is used for carrying and injecting titanium dioxide powder into the furnace body by oxygen;
the device comprises a furnace body, a heating section and a heat preservation section, wherein the heating section comprises an oxidation-resistant high-temperature conductive ceramic tube sleeved on the middle section of the zirconia ceramic tube, an induction coil is wound on the outer side of the oxidation-resistant high-temperature conductive ceramic tube, and the induction coil is controlled to be heated through an electromagnetic induction heating power supply system; the zirconia electrodes are respectively arranged at the parts, which are not sleeved with the oxidation-resistant high-temperature conductive ceramic tubes, of the upper end and the lower end of the zirconia ceramic tube, and are connected with an external resistance heating system through a water-cooling zirconia electrode busbar; and a growth interface at the lower end of the heat preservation section is provided with a corundum base rod for seed crystal growth.
The ceramic furnace comprises a crystal growth corundum base 1, a growth furnace refractory brick 2, a growth furnace heat-insulating material 3, a growing crystal 4, a growth furnace refractory brick 5, an observation hole 6, water-cooled zirconia electrode buses (red copper) (7 and 14), zirconia ceramic resistor electrodes (8 and 13), zirconia ceramic tubes 9, wherein the zirconia ceramic resistor electrodes 8 are arranged at two ends of the zirconia ceramic tubes 9, the zirconia electrodes 8 are connected with an external heating system through the water-cooled zirconia electrode buses, an oxidation-resistant high-temperature conductive ceramic tube 10 is sleeved at the middle section of the zirconia ceramic tubes 9, an induction coil 11 is wound on the outer side of the oxidation-resistant high-temperature conductive ceramic tube 10, and the induction coil is controlled to be heated through an electromagnetic induction heating power system.
When the electromagnetic induction heating power supply system heats the oxidation-resistant high-temperature conductive ceramic 10 to a temperature above 2400 ℃ through electromagnetic induction, the oxidation-resistant high-temperature conductive ceramic 10 heats the zirconia ceramic tube 9 to a temperature above 1200 ℃ through a heat conduction mode, and the zirconia ceramic tube starts to conduct electricity at a temperature above 1000 ℃, so that the zirconia ceramic tube can be heated through resistance. The oxidation-resistant high-temperature conductive ceramic tube 10 is an oxidation-resistant high-temperature composite ceramic material which is conductive at normal temperature, so that the oxidation-resistant high-temperature composite ceramic tube can be heated by an electromagnetic induction coil; whereas zirconia ceramic tubes are non-conductive below 800 ℃ and cannot be heated by electromagnetic induction or electrical resistance. The oxidation-resistant high-temperature conductive ceramic tube 10 heats itself to a high temperature by an electromagnetic induction coil, and then heats the zirconia ceramic tube 9 to a conductive temperature by itself. The induction coil is capable of generating an electromagnetic field that heats a conductive, high temperature resistant composite ceramic tube located inside the induction coil. The induction coil is wrapped with a layer 12 of growth furnace firebrick.
The two sets of power supplies are automatically switched according to the insulator-conductor transition temperature of the zirconia ceramic tube, so that the low-temperature Duan You oxidation-resistant high-temperature ceramic tube 10 and the electromagnetic induction heating power supply system 11 thereof are started to heat, the oxidation-resistant high-temperature ceramic tube 10 is heated to 1200 ℃, then the two sets of power supplies are automatically switched to the zirconia ceramic tube 9 and the resistance heating system thereof, and the zirconia ceramic tube 9 is heated to about 2000 ℃ by the system (according to the process requirement), so that an oxidation-resistant high-temperature environment is formed in the tube.
The furnace fully utilizes the radiation, conduction and convection heat transfer principles, and the temperature in the furnace can be heated to 2400 ℃ at the highest, so that the requirement of most high-temperature oxide single crystal growth can be met. For growing rutile monocrystal, seed crystal fixed on the upper end of crystal growth corundum base rod is first dissolved to form molten cap. Then, the titanium dioxide powder is carried by oxygen and enters into the furnace body through the material nozzle 15 from the material hopper 16, and then is heated by a zirconia tube in a growth furnace heated by an electromagnetic induction and resistance dual-heating system, so that the temperature is raised and melted to form molten drops. The molten drops continuously fall onto the melting cap, and the growth mechanism drives the crystal growth base to move downwards, so that the melt on the melting cap is continuously crystallized, and the crystal growth process is completed.
As can be seen from FIG. 2, when the flow rate of oxygen is regulated to be 0.1m/s, the furnace wall temperature is heated to 2400 ℃, the heating section is regulated to be 150mm, and the heat preservation section is regulated to be 180mm, the temperature at the center of a growth interface can be ensured to be slightly higher than 1850 ℃, and the surrounding temperature is slightly lower than 1850 ℃, so that the shoulder expanding requirement of the growing rutile monocrystal is met. The outer wall of the heat preservation section adopts a stainless steel furnace shell 21.
The traditional flame melting furnace for growing rutile monocrystal adopts oxyhydrogen flame as a heat source, the heat is transmitted to a melting cap in a conduction mode by gas combustion, the larger the crystal size is, the flow of the required gas is increased, the larger the impact of the gas flow on the melting cap is, and the more defects in the crystal are increased and even the overflow is dangerous; meanwhile, a large amount of hydrogen and water vapor exist in the growth environment, so that the high-temperature melt such as rutile is reduced or decomposed. The invention heats in a heat radiation and convection mode, and obtains pure oxidizing atmosphere under the condition of avoiding air flow impact, thereby being suitable for growing high-temperature oxide single crystals such as high-quality rutile and the like.
In the embodiment, the length of the heating section is 150mm, and the length of the heat preservation section is 180mm.
The material injection section comprises a hopper 16 and an inverted triangle material nozzle 15 connected with the hopper, a storage bin 18 is arranged on the central axis of the hopper, a vibrating rod 19 is arranged in the storage bin 18, vibration is generated at the upper end of the vibrating rod 19 through a knocking hammer 20 according to frequency knocking, and a screen 17 is arranged on the interface between the storage bin 18 and the hopper.
And part of the cooling section and the periphery from the lower part of the growth interface to the bottom of the corundum base rod for seed crystal growth are provided with an insulating layer consisting of a growth furnace refractory brick (2, 5), a growth furnace insulating material 3 and a stainless steel shell 21. The corundum base rod 1 is of a lifting structure, and when molten drops continuously fall onto the melting cap, the corundum base rod is adjusted to move downwards, and the melt on the melting cap is continuously crystallized. An observation hole 6 is arranged on the heat preservation layer.
The invention comprises a control system for controlling the heating process of the resistance heating system and the electromagnetic induction heating power supply system, wherein the heating process comprises the following steps: the electromagnetic induction heating power supply system is started to perform electromagnetic induction heating, after the oxidation-resistant high-temperature conductive ceramic tube is heated, the zirconia ceramic tube in the oxidation-resistant high-temperature conductive ceramic tube is heated to the conductive temperature through heat conduction, the control system is automatically switched to the resistance heating system to heat, the zirconia ceramic tube is subjected to resistance heating, the zirconia ceramic tube and the inside of the zirconia ceramic tube are heated to the temperature required by the process, and the temperature condition required by the growth of rutile monocrystal is met; and the device is also used for controlling the lifting of the corundum base rod, and adjusting the corundum base rod to move downwards when the molten drops continuously fall onto the melting cap, so that the melt on the melting cap is continuously crystallized.
The invention provides a preparation method of an optical grade rutile monocrystal, which comprises the following steps:
controlling a resistance heating system and an electromagnetic induction heating power supply system to heat, starting the electromagnetic induction heating power supply system to perform electromagnetic induction heating, heating the zirconia ceramic tube inside the oxidation-resistant high-temperature conductive ceramic tube to a conductive temperature through heat conduction, and automatically switching the control system to the resistance heating system to heat, heating the zirconia ceramic tube in a resistance way, heating the zirconia ceramic tube and the inside of the zirconia ceramic tube to a temperature required by a process, and meeting a temperature condition required by growing rutile monocrystal;
carrying titanium dioxide powder into a furnace body from a hopper through a material nozzle by oxygen;
heating by a zirconia tube in a growth furnace heated by an electromagnetic induction and resistance dual-heating system to heat and melt the zirconia tube to form molten drops;
and controlling the lifting of the corundum base rod, and adjusting the corundum base rod to move downwards when the molten drops continuously fall onto the melting cap, so that the melt on the melting cap is continuously crystallized.
The flow of oxygen is regulated to be 0.1m/s, the heating section is regulated to be 150mm, and the heat preservation section is regulated to be 180mm.
And after the oxidation-resistant high-temperature ceramic tube is heated to 1200 ℃, the ceramic tube is automatically switched to a resistance heating system, and the zirconia ceramic tube is heated to 2400 ℃.
The electromagnetic induction and resistance dual-heating system adopts electromagnetic induction heating, and can accurately change the temperature distribution in the furnace by adjusting current so as to meet the temperature condition required by the growth of rutile monocrystal. The powder is carried by oxygen to enter the furnace body from the nozzle, so that the requirements of continuous feeding and pure oxidizing atmosphere required by the growth of rutile monocrystal can be met. The induction heating is used for replacing oxyhydrogen flame heating, so that energy conservation and environmental protection can be achieved, and the danger in the production process is reduced. By adding the zirconia tube of the resistance heating system in the oxidation-resistant high-temperature conductive ceramic tube, the phenomena of oxidation and volatilization of trace components existing at high temperature by directly using the oxidation-resistant high-temperature conductive ceramic tube can be effectively avoided, and pollution to the grown crystal is avoided. The rutile monocrystal growth method heated by oxyhydrogen flame is replaced by an electromagnetic induction and resistance double-heating system, so that the precise parameter control, easy realization of automation, energy conservation and environmental protection can be achieved, and the danger in the production process is reduced.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, and alternatives falling within the spirit and principles of the invention.
Claims (9)
1. An optical grade rutile single crystal growth apparatus, comprising:
the material injection section is used for carrying and injecting titanium dioxide powder into the furnace body by oxygen;
the device comprises a furnace body, a heating section and a heat preservation section, wherein the heating section comprises an oxidation-resistant high-temperature conductive ceramic tube sleeved on the middle section of the zirconia ceramic tube, an induction coil is wound on the outer side of the oxidation-resistant high-temperature conductive ceramic tube, and the induction coil is controlled to be heated through an electromagnetic induction heating power supply system; the zirconia electrodes are respectively arranged at the parts, which are not sleeved with the oxidation-resistant high-temperature conductive ceramic tubes, of the upper end and the lower end of the zirconia ceramic tube, and are connected with an external resistance heating system through a water-cooling zirconia electrode busbar; and a growth interface at the lower end of the heat preservation section is provided with a corundum base rod for seed crystal growth.
2. The optical grade rutile single crystal growth apparatus of claim 1, wherein the heating section has a length of 150mm and the insulating section has a length of 180mm.
3. The optical grade rutile single crystal growth apparatus of claim 1, wherein the material injection section comprises a hopper and an inverted triangle material nozzle connected with the hopper, a vibration rod is arranged on the central axis of the hopper, and the upper end of the vibration rod is knocked according to frequency by a knocking hammer to generate vibration.
4. The optical grade rutile single crystal growth apparatus of claim 1, wherein a portion of the cooling section and the periphery of the bottom of the corundum base rod below the growth interface to the seed crystal growth are provided with a heat-insulating layer comprising a growth furnace refractory brick, a growth furnace heat-insulating material and a stainless steel housing.
5. The optical grade rutile single crystal growth apparatus of claim 1, wherein the corundum base rod is of a liftable structure, and the corundum base rod is adjusted to move downwards when the molten drops continuously fall onto the melting cap, and the melt on the melting cap is continuously crystallized.
6. The optical grade rutile single crystal growth apparatus of claim 1, further comprising a control system for controlling the heating process of the resistive heating system and the electromagnetic induction heating power system, the heating process comprising: the electromagnetic induction heating power supply system is started to perform electromagnetic induction heating, after the oxidation-resistant high-temperature conductive ceramic tube is heated, the zirconia ceramic tube in the oxidation-resistant high-temperature conductive ceramic tube is heated to the conductive temperature through heat conduction, the control system is automatically switched to the resistance heating system to heat, the zirconia ceramic tube is subjected to resistance heating, the zirconia ceramic tube and the inside of the zirconia ceramic tube are heated to the temperature required by the process, and the temperature condition required by the growth of rutile monocrystal is met;
the control system is used for controlling the lifting of the corundum base rod, and when molten drops continuously fall onto the melting cap, the corundum base rod is adjusted to move downwards, and the melt on the melting cap is continuously crystallized.
7. A method for preparing an optical grade rutile monocrystal, which is characterized by comprising the following steps:
controlling a resistance heating system and an electromagnetic induction heating power supply system to heat, starting the electromagnetic induction heating power supply system to perform electromagnetic induction heating, heating the zirconia ceramic tube inside the oxidation-resistant high-temperature conductive ceramic tube to a conductive temperature through heat conduction, and automatically switching the control system to the resistance heating system to heat, heating the zirconia ceramic tube in a resistance way, heating the zirconia ceramic tube and the inside of the zirconia ceramic tube to a temperature required by a process, and meeting a temperature condition required by growing rutile monocrystal;
carrying titanium dioxide powder into a furnace body from a hopper through a material nozzle by oxygen;
heating by a zirconia tube in a growth furnace heated by an electromagnetic induction and resistance dual-heating system to heat and melt the zirconia tube to form molten drops;
and controlling the lifting of the corundum base rod, and adjusting the corundum base rod to move downwards when the molten drops continuously fall onto the melting cap, so that the melt on the melting cap is continuously crystallized.
8. The method for preparing an optical grade rutile single crystal according to claim 7, wherein the flow rate of oxygen is adjusted to 0.1m/s, the heating section is adjusted to 150mm, and the heat-preserving section is adjusted to 180mm.
9. The method for preparing an optical grade rutile single crystal according to claim 7, wherein the oxidation-resistant high temperature ceramic tube is heated to 1200 degrees and then automatically switched to a resistance heating system to heat the zirconia ceramic tube to 2400 degrees.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211102013.0A CN116536763A (en) | 2022-09-09 | 2022-09-09 | Optical grade rutile monocrystal growth device and method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211102013.0A CN116536763A (en) | 2022-09-09 | 2022-09-09 | Optical grade rutile monocrystal growth device and method |
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| CN116536763A true CN116536763A (en) | 2023-08-04 |
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| CN202211102013.0A Withdrawn CN116536763A (en) | 2022-09-09 | 2022-09-09 | Optical grade rutile monocrystal growth device and method |
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| Country | Link |
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| CN (1) | CN116536763A (en) |
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- 2022-09-09 CN CN202211102013.0A patent/CN116536763A/en not_active Withdrawn
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