CN1160551C - Real-time measuring method of solid-liquid interface structure in high-temperature melt process of crystal growth and high-temperature heating stage - Google Patents
Real-time measuring method of solid-liquid interface structure in high-temperature melt process of crystal growth and high-temperature heating stage Download PDFInfo
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- CN1160551C CN1160551C CNB01113657XA CN01113657A CN1160551C CN 1160551 C CN1160551 C CN 1160551C CN B01113657X A CNB01113657X A CN B01113657XA CN 01113657 A CN01113657 A CN 01113657A CN 1160551 C CN1160551 C CN 1160551C
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Abstract
The present invention discloses a method and a high-temperature heat table for measuring a solid / liquid interface layer structure of grown crystals in real time by a high-temperature fused mass method. The present invention is characterized in that a high-temperature heat table with a unique structure is designed; the heat table has an automatic warming and temperature control system, a cooling water circulation system, an inert gas protection system and a suction gas system; thermal insulation media are arranged in a table body, and an electric heating device has horizontal temperature gradients and longitudinal temperature gradients. A platinum crucible is arranged on the electric heating device; measured samples are put in the crucible so as to be heated, and by using laser microscopic high-temperature Raman spectroscopic technology, the solid / liquid interface layer structure of growing crystals is observed and measured in real time by a quartz window of the high-temperature heat table.
Description
Technical field
The present invention relates to the measuring technique and the equipment of a kind of high-temperature fusant method crystal growth solid-liquid boundary layer structure, character and variation, belong to optical detection experimental technique and instrument field.
Background technology
Crystal growth is that growth unit is superimposed and form the process of crystal in the solid-liquid boundary layer.When the melt method for growing crystal, have the solid-liquid boundary layer---by the transition bed of melt to the crystal conversion, the crystal growth primitive is at crystallization behaviors such as the fractional condensation behavior of superimposed, the crystal growth at interface, crystal defects, and is all relevant with the structure and the character in this boundary layer.Desire obtains high-quality crystal, is necessary structure, character and the variation thereof etc. in solid-liquid boundary layer in the crystal growing process are studied with the inner link of crystallization behavior, discloses the mechanism of crystal growth.
Nineteen ninety-five Yuan Hui the artificial lens journal third phase disclose a kind of when measuring the crystal high-temperature fusion surface tension and the method and apparatus of action of gravity PARTICLE TRANSPORT FROM direction.Device includes the high temperature crystal growth chamber; crystal growth is indoor annular platinum filament well heater; there is quartz window the device top; can lead to protective gas in the growth room; observing system is the BH-2 type differential interference microscope that the Japanese OLKMPUS of employing company produces; and done corresponding improvement, and the cinephotomicrography light path is connected with the shooting register system, observe in the high temperature crystal melting process in the horizontal direction and gravity direction PARTICLE TRANSPORT FROM phenomenon.
Professor Yu Xiling of Shandong University designed a cover glass crystallizer in the structure of measuring Crystal Growth from Aqueous Solution solid-liquid boundary layer and boundary layer below 100 ℃ in 1998, and applied for patent of invention and utility model patent, the patent No. is respectively 981100309,98220096.
Above-mentioned several method all can't carry out Real Time Observation to thickness, shape, the structure in high temperature (700 ℃～1500 ℃) functional crystal material growth solid-liquid boundary layer, and the micro-Raman spectrum of Laser Measurement, further the variation of research structure and with the relation of growth mechanism.
Summary of the invention
The objective of the invention is requirement according to the experiment condition of the principle of zone-melting process crystal growth and laser capture microdissection high temperature raman spectroscopy instrument, design one is enclosed within the high-temperature fusant method crystal growing process shape, thickness to its solid-liquid boundary layer to be carried out Real Time Observation and measures, and also measures the method and the hot table apparatus of special-purpose high temperature of the micro raman spectra of crystal phase, melt phase, solid-liquid boundary layer phase simultaneously in real time.
The objective of the invention is to be achieved through the following technical solutions.
Measure the method for high-temperature fusant method grown crystal solid-liquid boundary layer structure in real time, it is characterized in that using the quartz window of laser capture microdissection high temperature raman spectroscopy technology by high-temperature stage, in real time the structure in the solid-liquid boundary layer in the crystal growth is observed measurement, take the photograph by CCD and will observe mutually that sample forms solid-state phase in the Platinum crucible from display, the solid-liquid boundary layer, the melt phase, measure the thickness in solid-liquid boundary layer, writing edge interlayer shape, switched mirror, the Raman light signal of scattering is passed through reflection, import monochromator, through opto-electronic conversion, photon counting, the input microcomputer, carry out data and collection of illustrative plates and handle, thus the research boundary layer structure, the inner link of the variation of character and crystal structure behavior discloses mechanism of crystal growth.
Measure the high-temperature stage of high-temperature fusant method grown crystal solid/liquid interfaces layer structure in real time; stage body and Tai Gai are arranged; platform has covered quartz window, and electric heater, thermal insulation medium are arranged in the stage body, it is characterized in that stage body and Tai Gai are two layers of housing; in stage body, the platform lid crustless sandwich chilled water circulation is arranged; connect inertia protection gas system in the stage body, the platform side of covering connects extract system, is placed with electric heater on the thermal insulation medium; be placed with crucible on the electric heater, have a slice to have the back backing of light hole on the crucible.
Described electric heater can be realized the vertical and horizontal gradient temperature.
Described electric heater is formed flute profile by three blocks of trapezoidal corundum, the platinum that twines on the corundum by grow out of nothing, mode from rare to close twines.
Described thermal insulation medium is a foamed alumina, and back backing is a graphite flake, and crucible is a Platinum crucible.
Described high-temperature stage, the requirement for experiment condition of adaptation laser capture microdissection High Temperature Raman Spectrometer, it highly only has about 50mm, and diameter is (can select height and diameter according to different requirement for experiment condition) about 75mm.
The present invention includes following system:
(1) intensification temperature-controlling system: temperature can be raised to 1500 ℃, and constant temperature is in fusing point time error ± 0.1 ℃.
(2) circulating water cooling system: the surface temperature of hot platform was in room temperature when intensification reached 1000 ℃.
(3) filling with inert gas protection system: prevent sample at the intensification rear oxidation, guarantee that the crystal chemistry composition is constant.
(4) extract system: extract the Re Tainei volatile matter, guarantee that quartz window not by dirt, normally obtains light signal.
(5) electric heater laterally, Temperature Distribution longitudinally, can form stable solid-liquid boundary layer.
(6) micro raman spectra picked-up signal system: through opto-electronic conversion, photon counting, the input microcomputer carries out data and collection of illustrative plates is handled.
(7) CCD takes the photograph phase system: by display, crystal phase, solid-liquid boundary layer, the shape of melt phase, thickness are shown.
(8) thermal insulation medium: keep the temperature in the stove, reduce thermal loss.
Effect of the present invention:
1, adopted unique miniature high-temperature stage, sample is formed with crystal phase, melt mutually and the growth conditions in solid-liquid boundary layer in its temperature field, crystal phase, solid-liquid boundary layer, melt are on good terms under the detection object lens that are exposed to the micro raman spectra instrument fully.
2, the present invention has realized real-time detection, can observe the solid-liquid boundary layer when melting temperature, and measure its shape and thickness, measures the laser capture microdissection high temperature raman spectroscopy in crystalline phase, melt phase and crystal solid-liquid boundary layer simultaneously again in real time.
Description of drawings
Fig. 1 is a fundamental diagram of the present invention.
Embodiment
Embodiment
Referring to accompanying drawing.
The present invention's high-temperature stage, stage body 11 is arranged, platform lid 12, on the platform lid 12 quartz window 13 is arranged, thermal insulation medium 18 is arranged in the stage body 11, stage body 11, platform lid 12 is two layers of housing, stage body 11, platform covers and charges into recirculated cooling water 2 in 12 crustless sandwiches, stage body 11, chilled water in the platform lid 12 is communicated with, one tracheae is arranged on the stage body 11, filling with inert gas argon gas 3 has tracheae to connect the decontamination system 4 of bleeding on the platform lid 12, is placed with electric heater 5 on the thermal insulation medium 18, be placed with Platinum crucible 14 on the electric heater 5, place sample 15 in the Platinum crucible 14, backing 16 behind the graphite of band viewport in the middle of being placed with on the Platinum crucible 14, electric heater is formed flute profile by three blocks of corundum that are wound with platinum wire, platinum wire connects automatic intensification temperature-controlling system 1, platinum wire is by growing out of nothing on the corundum, mode from rare to close around, corundum is trapezoidal, corundum of middle placing flat, its both sides respectively stand up a corundum, realize the gradient temperature of sample vertical and horizontal when heating.
The present invention measures the method for crystal growth solid-liquid boundary layer structure, is to use laser capture microdissection high temperature raman spectroscopy technology, by the quartz window of high-temperature stage, to crystal and melt in the growth mutually, the solid-liquid boundary layer structure carries out Real Time Observation, measurement.During use,, make the laser of light source Ar ion laser output wavelength 488nm, power stability earlier with the start of laser capture microdissection high temperature raman spectroscopy instrument.Regulate light path, make high-temperature stage enter light path, adjust focal length, make it on the focal plane.Open the receiving system of light source, enter normal duty.Open the cooling water recirculation system of hot platform, open the heating system follow procedure and be warming up to fusing point and temperature control automatically, error is ± 0.1 ℃, take the photograph phase 6 by CCD, the sample of observing in the Platinum crucible from display 8 forms solid-state phase, solid-liquid boundary layer, melt phase, measure the solid-liquid boundary layer thickness, the shape of writing edge interlayer.Switched mirror imports monochromator with Raman light signal 6, through opto-electronic conversion, carries out photon counting 9, and the input microcomputer carries out data and image processing 10.
The applicant has used this method to functional material Bi
12SiO
20(890 ℃ of fusing points), tellurium oxide (733.8 ℃ of fusing points) are tested, observe the solid-liquid boundary layer, and its shape and thickness have been write down, measured simultaneously the micro raman spectra in crystal phase, melt phase and the solid-liquid boundary layer of these materials in real time, at first drawn the boundary layer in the world and existed structure to be different from the experimental result that crystal also is different from the growth unit of melt.But, guarantee that simultaneously quartz window is not contaminated with this method and system continuous working and measurement.
Claims (3)
1, measure the method for melt method for growing crystal solid-liquid boundary layer structure in real time, it is characterized in that:
(1), a high-temperature stage is set, stage body and Tai Gai are arranged, and platform has covered quartz window, and electric heater, thermal insulation medium are arranged in the stage body, stage body and Tai Gai are two layers of housing, in stage body, the platform lid crustless sandwich chilled water circulation is arranged, connect inertia protection gas system in the stage body, the platform side of covering connects extract system, be placed with electric heater on the thermal insulation medium, be placed with crucible on the electric heater, have a slice to have the back backing of light hole on the crucible, tested crystal prototype is placed in the crucible;
(2), earlier with the start of laser capture microdissection high temperature raman spectroscopy instrument, regulate light path, open the receiving system of light source, enter normal duty, open the cooling water recirculation system of hot platform, open heating system and be warming up to fusing point and temperature control;
(3), use the quartz window of laser capture microdissection high temperature raman spectroscopy technology by high-temperature stage, in real time the crystal solid-liquid boundary layer structure in the growth is observed, take the photograph mutually and will observe sample formation crystal phase in the Platinum crucible by CCD from display, the solid-liquid boundary layer, the melt phase, measure the thickness in solid-liquid boundary layer, the shape of writing edge interlayer, switched mirror, the Raman light signal of scattering is passed through reflection, import monochromator, through opto-electronic conversion, photon counting, the input microcomputer carries out data and collection of illustrative plates and handles, the research boundary layer structure, the inner link of the variation of character and crystal structure behavior discloses mechanism of crystal growth.
2, the method for real-time measurement melt method for growing crystal solid-liquid boundary layer structure according to claim 1, it is characterized in that described electric heater forms flute profile by three blocks of trapezoidal corundum, the platinum wire that twines on the corundum by grow out of nothing, mode from rare to close twines, electric heater can be realized the vertical and horizontal gradient temperature.
3, the method for real-time measurement melt method for growing crystal solid-liquid boundary layer structure according to claim 1 is characterized in that described thermal insulation medium is a foamed alumina, and back backing is a graphite flake, and crucible is a Platinum crucible.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB01113657XA CN1160551C (en) | 2001-05-27 | 2001-05-27 | Real-time measuring method of solid-liquid interface structure in high-temperature melt process of crystal growth and high-temperature heating stage |
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| CNB01113657XA CN1160551C (en) | 2001-05-27 | 2001-05-27 | Real-time measuring method of solid-liquid interface structure in high-temperature melt process of crystal growth and high-temperature heating stage |
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| CN1160551C true CN1160551C (en) | 2004-08-04 |
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| CN101561401B (en) * | 2009-05-23 | 2011-08-17 | 青岛大学 | Real-time observation method of crystal growing surface microstructure |
| CN102936748B (en) * | 2011-08-15 | 2015-07-29 | 江苏协鑫硅材料科技发展有限公司 | A kind of well heater of ingot furnace |
| CN102393356B (en) * | 2011-10-26 | 2013-07-10 | 东北大学 | Microscope heating stage for Raman spectral measurement of high-temperature volatile molten salt |
| TWI438313B (en) * | 2011-12-16 | 2014-05-21 | C Sun Mfg Ltd | A method, a detecting system and an apparatus for monitoring and controlling the state of crystal growth |
| CN103045787B (en) * | 2013-01-21 | 2014-09-10 | 重庆大学 | Method and device for observing growth process of iron whiskers on surfaces of iron ore powder particles |
| CN103645200B (en) * | 2013-11-20 | 2016-06-01 | 中国科学院合肥物质科学研究院 | The method of ��-XAFS technology in site measurement scorification crystal growth microtexture and miniature crystal growing furnace |
| CN103698348B (en) * | 2013-12-16 | 2018-04-27 | 中国科学院合肥物质科学研究院 | The method and minicrystal growth furnace of the GIXRD technologies crystal growth boundary layer microstructure of measurement in real time in situ |
| CN104567402B (en) * | 2015-01-14 | 2016-06-01 | 中国科学院合肥物质科学研究院 | The method of synchrotron radiation ��-SAXS technology in site measurement scorification crystal microscopic growth base unit particle diameter and miniature crystal growing furnace |
| CN106757349A (en) * | 2016-11-25 | 2017-05-31 | 中国科学院长春应用化学研究所 | Rare earth crystal growth equipment, rare earth crystal growth technique and application |
| CN107966468A (en) * | 2017-12-21 | 2018-04-27 | 广东核电合营有限公司 | A kind of fuel pellet fusing point measuring device and method |
| CN110917998A (en) * | 2019-12-02 | 2020-03-27 | 长沙新材料产业研究院有限公司 | Diamond growth on-line monitoring method and diamond synthesis equipment |
| CN111455455A (en) * | 2020-02-29 | 2020-07-28 | 武汉大学 | Crystal growth device with online monitoring function |
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