CN103645200A - Method used for in-situ measurement of melting method crystal growth microstructures via mu-XAFS technology and minicrystal growth furnace - Google Patents
Method used for in-situ measurement of melting method crystal growth microstructures via mu-XAFS technology and minicrystal growth furnace Download PDFInfo
- Publication number
- CN103645200A CN103645200A CN201310582505.9A CN201310582505A CN103645200A CN 103645200 A CN103645200 A CN 103645200A CN 201310582505 A CN201310582505 A CN 201310582505A CN 103645200 A CN103645200 A CN 103645200A
- Authority
- CN
- China
- Prior art keywords
- crystal
- growth
- crystal growth
- heater
- fusion method
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Landscapes
- Crystals, And After-Treatments Of Crystals (AREA)
- Analysing Materials By The Use Of Radiation (AREA)
Abstract
The invention discloses a method used for in-situ real-time measurement of melting method crystal growth microstructures via mu-XAFS technology. The method is based on mu-XAFS technology, and is respectively used for in-situ real-time measurement of coordination states and evolution rules of characteristic elements of different melting method crystal growth zones (crystals, boundary layers and melts) so as to obtain change rules from melts to crystal microstructures in melting method crystal growth processes. The invention also provides a minicrystal growth furnace used for in-situ measurement of melting method crystal growth microstructures via mu-XAFS technology. In-situ real-time measurement of coordination numbers of the characteristic elements in crystals, boundary layers and melts in crystal growth processes can be realized using the minicrystal growth furnace.
Description
Technical field
The present invention relates to μ-XAFS technology original position and measure in real time method and the minicrystal growth furnace of fusion method crystal growth micromechanism, belong to the experimental technique field that material microstructure original position is measured in real time.
Background technology
Crystal growth is a complicated phase transition process, past is owing to being subject to the restriction of observation procedure and means, current many crystal growth theories be not to be all based upon on the basis of growth course original position real-time monitored microstructure change, so these theories more or less all come with some shortcomings.By real-time in-situ, observe in crystal growing process, the variation of zones of different micromechanism and Changing Pattern, be the basis of setting up new real crystal growth theory.
Within 1998, professor Yu Xiling of Shandong University designs a set of glass crystallizer, adopt holographic phase contrast interference microscopy, find that the growth of aqua-solution method crystal exists solute boundary layer, and applied for that patent of invention and practical patent, the patent No. are respectively 98110030.9,98220096.X.Calendar year 2001 peace light has been invented the method for growth unit microstructure change and Changing Pattern in application high-temperature laser micro Raman spectra real-time in-situ measurement crystal growing process, and adapt to crystal that high temperature Raman original position measures the in real time hot table apparatus of growing, the micromechanism in the melt of tens kinds of crystal, crystal and boundary layer has been carried out to real-time monitored and research, obtained important achievement in research.Method and apparatus has obtained respectively patent of invention and practical license, and the patent No. is respectively ZL01238010.5, ZL01113657.X.
Raman spectrum is the reflection of chemical bond vibrational state between material particle, by Raman spectrum, can obtain the information of the structure of matter, therefore applying laser capture microdissection Raman spectroscopy can be in crystal growing process, and original position, real-time monitored are carried out in crystal, boundary layer, melt micromechanism and variation thereof.The present invention is coordination number and the variation thereof of measuring in real time element-specific in melt in crystal growing process, boundary layer and crystal by synchrotron radiation micro-beam X-ray Absorption Fine Structure spectral technology (μ-XAFS) original position, thereby obtain the information of zones of different microstructure change, it is a kind of new method of research crystal growth microscopic mechanism, kinds of experiments method can mutually be confirmed and supplement, and makes crystal growth Study on Microcosmic Mechanism more improve and go deep into.
Summary of the invention
Technical matters to be solved by this invention is to provide a kind of method and minicrystal growth furnace of μ-XAFS technology in site measurement fusion method crystal growth zones of different coordination structure, can realize the coordination number of the element-specific in crystal, boundary layer and melt when crystal is grown and carry out original position, real-time monitored.
Technical matters to be solved by this invention realizes by the following technical solutions:
μ-XAFS technology original position is measured the method for fusion method crystal growth micromechanism in real time, it is characterized in that:
This method based on μ-XAFS technology respectively original position measure in real time co-ordination state and the development law thereof of the characteristic element of fusion method crystal when growth zones of different (crystal, boundary layer, melt), thereby the Changing Pattern from melt to crystal microscopic structure while obtaining the growth of fusion method crystal.
The minicrystal growth furnace of μ-XAFS technology in site measurement fusion method crystal growth coordination structure, this stove comprises body of heater and bell, described body of heater both sides have a window, in described body of heater, be provided with electric heater, a flat crucible is put in electric heater inside, the outer thermal insulation medium that is arranged with of electric heater and flat crucible;
Described bell top has one for observing the silica glass window of crystal growing state, is respectively equipped with apopore and inlet opening on described body of heater and bell.
Described electric heater is comprised of two blocks of parallel corundum, and it is shaped as " U " shape, on described every block of corundum, is wound with heating wire.
Heating wire two ends on described every block of corundum are connected with heating temperature-control system respectively.
Apopore on described bell is connected by water pipe with the inlet opening on body of heater.
Inlet opening on described bell is connected with cooling water system respectively by water pipe with the apopore on body of heater.
On described body of heater, the window of both sides is all on same level one axis.
Described thermal insulation medium is that foamed alumina or foam zirconia are wherein a kind of.
Described flat crucible is quartz or the flat crucible of white stone.
μ-XAFS technology original position is measured the method for fusion method crystal growth coordination structure in real time, and its concrete steps are as follows:
Step 1, crystal (or crystal and accordingly admittedly molten vitreum) sample is put into the flat crucible of stove, and stove is placed on the experiment table at synchrotron radiation micro-beam X-ray Absorption Fine Structure line station, open the X ray light source on synchrotron radiation line station, adjust the position of stove, make micro-beam X-ray just in time can see through the region that the sample in stove will be measured, then close X ray light source;
Step 2, open the cooling water system electric heater of unifying, by heating temperature-control system, control the heating power of electric heater, make the sample bottom fusing in flat crucible, form crystal, boundary layer and melt three subregions; Open X ray light source, and by temperature control or three-dimensional trim holder, regulate the position of crystal growth interface, make micro-beam X-ray see through respectively these three regions and gather experimental data;
CCD on step 3. micro-beam X-ray Absorption Fine Structure line station can show the image of experimentation, the trizonal state of the crystal of sample, boundary layer and melt in display can be observed flat crucible.
The invention has the beneficial effects as follows:
1, this minicrystal growth furnace is controlled with the design of unique temperature and accurate temperature, during in-situ observation, crystal prototype can form stable crystal, boundary layer and melt three subregions, and is presented on completely in the measurement range of micro-beam X-ray Absorption Fine Structure spectral technology;
2, realized original position, real-time measurement, can in crystal growing process, observe the shape in crystal, boundary layer and melt three regions, again can in site measurement to the micromechanism in three regions.
Accompanying drawing explanation
Fig. 1 is the structural representation of minicrystal growth furnace in the present invention;
Fig. 2 is the part-structure enlarged diagram of minicrystal growth furnace in the present invention.
In figure: 1-body of heater; 2-bell; 3-window; 4-electric heater; 41-corundum; 42-corundum; 43-heating wire; The flat crucible of 5-; 6-thermal insulation medium; 7-silica glass window; 8-apopore; 81-inlet opening; 9-apopore; 91-inlet opening; 10-heating temperature-control system; 11-water pipe; 111-water pipe; 12-cooling water system; 13-crystal prototype; 14-crystal; 15-boundary layer; 16-melt.
Embodiment
For technological means, creation characteristic that the present invention is realized, reach object and effect is easy to understand, below in conjunction with concrete diagram, further set forth the present invention.
As shown in Figure 1-2, the minicrystal growth furnace of μ-XAFS technology in site measurement fusion method crystal growth coordination structure, this stove comprises body of heater 1 and bell 2, body of heater 1 both sides have a window 3, state and in body of heater 1, be provided with electric heater 4, a flat crucible 5 is put in electric heater 4 inside, the outer thermal insulation medium 6 that is arranged with of electric heater 4 and flat crucible 5;
Bell 2 tops have one for observing the silica glass window 7 of crystal prototype 13 growing states, are respectively equipped with apopore 8,9 and inlet opening 81,91 on body of heater 1 and bell 2.
Apopore 9 on bell 2 is connected by water pipe 11 with the inlet opening 81 on body of heater 1.
Inlet opening 91 on bell 2 is connected with cooling water system 12 respectively by water pipe 111 with the apopore 8 on body of heater 1.
On body of heater 1, the window 3 of both sides is all on same level one axis.
Thermal insulation medium 6 is lightweight, the machinable foamed alumina of shape or foam zirconia.
Flat crucible 5 is quartz or the flat crucible of white stone.
μ-XAFS technology original position is measured the method for fusion method crystal growth micromechanism in real time, we based on μ-XAFS technology respectively original position measure in real time co-ordination state and the development law thereof of the characteristic element of fusion method crystal when growth zones of different (crystal, boundary layer, melt), thereby the Changing Pattern while obtaining the growth of fusion method crystal from melt to crystal microscopic structure, its concrete steps are as follows:
1., by crystal prototype 13(or crystal and admittedly molten vitreum accordingly) put into the flat crucible 5 of body of heater 1, and body of heater 1 is placed on the experiment table at synchrotron radiation micro-beam X-ray Absorption Fine Structure line station, open the X ray light source on synchrotron radiation line station, adjust the position of body of heater 1, make micro-beam X-ray just in time can see through the region that the crystal prototype 13 in body of heater 1 will be measured, then close X ray light source;
2., open cooling water system 12 and electric heater 4, by heating temperature-control system 10, control the heating power of electric heaters 4, make the crystal prototype 13 bottoms fusings in flat crucible 5, form crystal 14, boundary layer 15 and melt 16 3 subregions; Open X ray light source, and by temperature control or three-dimensional trim holder, regulate the position of crystal prototype 13 growth interfaces, make micro-beam X-ray see through respectively these three regions and gather experimental data;
3.. the CCD on micro-beam X-ray Absorption Fine Structure line station can show the image of experimentation, from display, can be observed crystal 14, boundary layer 15 and the trizonal state of melt 16 of the interior crystal prototype 13 of flat crucible 5.
In above-mentioned, in order to measure the spectrum of crystal prototype 13 optimum signal-noise ratios, for measurement elements different in different crystal prototype 13 or sample of the same race, adopt the flat crucible 5 of different-thickness.
More than show and described ultimate principle of the present invention, principal character and advantage.The technician of the industry should understand; the present invention is not restricted to the described embodiments; that in above-described embodiment and instructions, describes just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention.The claimed scope of the present invention is defined by appending claims and equivalent thereof.
Claims (10)
1. μ-XAFS technology original position is measured the method for fusion method crystal growth micromechanism in real time, it is characterized in that: this method based on μ-XAFS technology respectively original position measure in real time co-ordination state and the development law thereof of the characteristic element of fusion method crystal when growth zones of different (crystal, boundary layer, melt), thereby the Changing Pattern from melt to crystal microscopic structure while obtaining the growth of fusion method crystal.
2. the minicrystal growth furnace of μ-XAFS technology in site measurement fusion method crystal growth coordination structure, this stove comprises body of heater and bell, it is characterized in that: described body of heater both sides have a window, in described body of heater, be provided with electric heater, a flat crucible is put in electric heater inside, the outer thermal insulation medium that is arranged with of electric heater and flat crucible;
Described bell top has one for observing the silica glass window of crystal growing state, is respectively equipped with apopore and inlet opening on described body of heater and bell.
3. the minicrystal growth furnace of μ-XAFS technology in site measurement fusion method crystal growth coordination structure according to claim 2, it is characterized in that: described electric heater is comprised of two blocks of parallel corundum, it is shaped as " U " shape, on described every block of corundum, is wound with heating wire.
4. the minicrystal growth furnace of μ-XAFS technology in site measurement fusion method crystal growth coordination structure according to claim 3, is characterized in that: the heating wire two ends on described every block of corundum are connected with heating temperature-control system respectively.
5. the minicrystal growth furnace of μ-XAFS technology in site measurement fusion method crystal growth coordination structure according to claim 2, is characterized in that: the apopore on described bell is connected by water pipe with the inlet opening on body of heater.
6. the minicrystal growth furnace of μ-XAFS technology in site measurement fusion method crystal growth coordination structure according to claim 2, is characterized in that: the inlet opening on described bell is connected with cooling water system respectively by water pipe with the apopore on body of heater.
7. the minicrystal growth furnace of μ-XAFS technology in site measurement fusion method crystal growth coordination structure according to claim 2, is characterized in that: on described body of heater, the window of both sides is all on same level one axis.
8. the minicrystal growth furnace of μ-XAFS technology in site measurement fusion method crystal growth coordination structure according to claim 2, is characterized in that: described thermal insulation medium is that foamed alumina or foam zirconia are wherein a kind of.
9. the minicrystal growth furnace of μ-XAFS technology in site measurement fusion method crystal growth coordination structure according to claim 2, is characterized in that: described flat crucible is quartz or the flat crucible of white stone.
10. μ-XAFS technology original position is measured the method for fusion method crystal growth coordination structure in real time, and its concrete steps are as follows:
A, crystal prototype is put into the flat crucible of stove, and stove is placed on the experiment table at synchrotron radiation micro-beam X-ray Absorption Fine Structure line station, open the X ray light source on synchrotron radiation line station, adjust the position of stove, make micro-beam X-ray just in time can see through the region that the sample in stove will be measured, then close X ray light source;
B, open the cooling water system electric heater of unifying, by heating temperature-control system, control the heating power of electric heater, make the sample bottom fusing in flat crucible, form crystal, boundary layer and melt three subregions; Open X ray light source, and by temperature control or three-dimensional trim holder, regulate the position of crystal growth interface, make micro-beam X-ray see through respectively these three regions and gather experimental data;
C. the CCD on micro-beam X-ray Absorption Fine Structure line station can show the image of experimentation, the trizonal state of the crystal of sample, boundary layer and melt in display can be observed flat crucible.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310582505.9A CN103645200B (en) | 2013-11-20 | 2013-11-20 | The method of ��-XAFS technology in site measurement scorification crystal growth microtexture and miniature crystal growing furnace |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310582505.9A CN103645200B (en) | 2013-11-20 | 2013-11-20 | The method of ��-XAFS technology in site measurement scorification crystal growth microtexture and miniature crystal growing furnace |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103645200A true CN103645200A (en) | 2014-03-19 |
| CN103645200B CN103645200B (en) | 2016-06-01 |
Family
ID=50250451
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310582505.9A Active CN103645200B (en) | 2013-11-20 | 2013-11-20 | The method of ��-XAFS technology in site measurement scorification crystal growth microtexture and miniature crystal growing furnace |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103645200B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104122279A (en) * | 2014-07-18 | 2014-10-29 | 中国科学院高能物理研究所 | Measurement method of X-ray micro-zone absorption fine structure with spatial resolving capability |
| CN104567402A (en) * | 2015-01-14 | 2015-04-29 | 中国科学院合肥物质科学研究院 | In situ measuring method for grain diameter of melting method crystal microscopic growth element via synchrotron radiation mu-SAXS technology and micro crystal growing furnace |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2126918Y (en) * | 1992-07-03 | 1993-02-10 | 中国科学院大连化学物理研究所 | In-situ cell of expanded x-ray absorption fine structural spectrum |
| WO2002057763A2 (en) * | 2000-10-19 | 2002-07-25 | Structural Genomix, Inc. | Apparatus and method for identification of crystals by in-situ x-ray diffraction |
| CN1388368A (en) * | 2001-05-27 | 2003-01-01 | 中国科学院安徽光学精密机械研究所 | Real-time measuring method of solid-liquid interface structure in high-temperature melt process of crystal growth and high-temperature heating stage |
| CN201589756U (en) * | 2009-08-14 | 2010-09-22 | 中国科学院山西煤炭化学研究所 | Sample pool for carrying out in-situ characterization on crystallizing process of molecular sieve based catalyst |
| CN203629298U (en) * | 2013-11-20 | 2014-06-04 | 中国科学院合肥物质科学研究院 | Minicrystal growing furnace for measuring melting method crystal growth coordination structure through miu-XAFS technology in situ |
-
2013
- 2013-11-20 CN CN201310582505.9A patent/CN103645200B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2126918Y (en) * | 1992-07-03 | 1993-02-10 | 中国科学院大连化学物理研究所 | In-situ cell of expanded x-ray absorption fine structural spectrum |
| WO2002057763A2 (en) * | 2000-10-19 | 2002-07-25 | Structural Genomix, Inc. | Apparatus and method for identification of crystals by in-situ x-ray diffraction |
| CN1388368A (en) * | 2001-05-27 | 2003-01-01 | 中国科学院安徽光学精密机械研究所 | Real-time measuring method of solid-liquid interface structure in high-temperature melt process of crystal growth and high-temperature heating stage |
| CN201589756U (en) * | 2009-08-14 | 2010-09-22 | 中国科学院山西煤炭化学研究所 | Sample pool for carrying out in-situ characterization on crystallizing process of molecular sieve based catalyst |
| CN203629298U (en) * | 2013-11-20 | 2014-06-04 | 中国科学院合肥物质科学研究院 | Minicrystal growing furnace for measuring melting method crystal growth coordination structure through miu-XAFS technology in situ |
Non-Patent Citations (2)
| Title |
|---|
| 姚涛: "原位XAFS新方法及其功能材料动力学研究", 《中国博士论文全文数据库》, 15 April 2012 (2012-04-15) * |
| 王静等: "CsLiB6O10晶体及熔体微结构的高温拉曼光谱研究", 《人工晶体学报》, vol. 42, no. 3, 31 March 2013 (2013-03-31), pages 397 - 401 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104122279A (en) * | 2014-07-18 | 2014-10-29 | 中国科学院高能物理研究所 | Measurement method of X-ray micro-zone absorption fine structure with spatial resolving capability |
| CN104567402A (en) * | 2015-01-14 | 2015-04-29 | 中国科学院合肥物质科学研究院 | In situ measuring method for grain diameter of melting method crystal microscopic growth element via synchrotron radiation mu-SAXS technology and micro crystal growing furnace |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103645200B (en) | 2016-06-01 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Cao et al. | Femtosecond laser-induced crystallization in glasses: growth dynamics for orientable nanostructure and nanocrystallization | |
| CN103698348B (en) | The method and minicrystal growth furnace of the GIXRD technologies crystal growth boundary layer microstructure of measurement in real time in situ | |
| CN108698126A (en) | Consummate 3 D-printing | |
| CN104959577A (en) | Method for simulating growth of solidification structure of large ingot under slow cooling condition, and fusion casting experiment apparatus | |
| Lipatiev et al. | Direct laser writing of LaBGeO5 crystal-in-glass waveguide enabling frequency conversion | |
| CN104651934B (en) | A kind of energy-saving sapphire crystal growing furnace | |
| CN106757362A (en) | Selenium germanium cadmium strontium compound and preparation method thereof, selenium germanium cadmium strontium crystal and its preparation method and application | |
| Nishii et al. | Morphology and orientation of β-BaB2O4 crystals patterned by laser in the inside of samarium barium borate glass | |
| CN103645200A (en) | Method used for in-situ measurement of melting method crystal growth microstructures via mu-XAFS technology and minicrystal growth furnace | |
| Fang et al. | Numerical study of the micro-pulling-down process for sapphire fiber crystal growth | |
| CN100557091C (en) | A kind of micro-reaction device and method of utilizing the thermograde synthesizing cadmium selenide nano-crystal | |
| CN203629298U (en) | Minicrystal growing furnace for measuring melting method crystal growth coordination structure through miu-XAFS technology in situ | |
| McAnany et al. | Challenges of laser-induced single-crystal growth in glass: incongruent matrix composition and laser scanning rate | |
| CN107966467A (en) | The experimental provision and experimental method of material solidification under a kind of research microgravity condition | |
| CN104534879B (en) | The method of synchrotron radiation ��-XRD technology in site measurement fusion method crystal growth microstructure and minicrystal growth furnace | |
| Oliveira et al. | Temperature uniformity improvement in a solar furnace by indirect heating | |
| CN105112990B (en) | A kind of method of the special-shaped nearly device frequency-doubling crystal of micro- drop-down oriented growth | |
| Sun et al. | Abnormal elemental redistribution in oxyfluoride glasses induced by high repetition rate femtosecond laser | |
| KR20120078620A (en) | Method of manufacturing vitreous silica crucible | |
| CN105115860A (en) | Synchrotron radiation imaging-based visual alloy melt interdiffusion measuring method | |
| CN107488874A (en) | A kind of design method of temperature field structure for rare earth crystal growth technique and the growth technique of low-cost rare earth crystal | |
| Zhu et al. | A simulation model for the temperature field in bioceramic coating cladded by wide-band laser | |
| CN209979473U (en) | High-temperature tube furnace suitable for in-situ optical microscopic observation and spectral analysis | |
| CN109022246A (en) | True Three-dimensional high-integration level temperature control microreactor and its processing method | |
| CN104567402B (en) | The method of synchrotron radiation ��-SAXS technology in site measurement scorification crystal microscopic growth base unit particle diameter and miniature crystal growing furnace |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |