CN104567402B - The method of synchrotron radiation ��-SAXS technology in site measurement scorification crystal microscopic growth base unit particle diameter and miniature crystal growing furnace - Google Patents
The method of synchrotron radiation ��-SAXS technology in site measurement scorification crystal microscopic growth base unit particle diameter and miniature crystal growing furnace Download PDFInfo
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- CN104567402B CN104567402B CN201510017797.0A CN201510017797A CN104567402B CN 104567402 B CN104567402 B CN 104567402B CN 201510017797 A CN201510017797 A CN 201510017797A CN 104567402 B CN104567402 B CN 104567402B
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Abstract
The present invention discloses the method for synchrotron radiation ��-SAXS technology in site measurement scorification crystal growth unit particle diameter, the size of microscopic growth base unit in different zones (frictional belt, melt) when present method grows based on synchrotron radiation ��-SAXS technology in site measurement scorification crystal, obtains the Changing Pattern of crystal microscopic growth base unit particle diameter from melt to crystal; Present invention also offers the miniature crystal growing furnace of application the method, the in-situ observation of the particle diameter of microscopic growth base unit in frictional belt and melt when can realize being grown by crystal by this miniature crystal growing furnace.
Description
Technical field
The present invention relates to the methods and applications of synchrotron radiation ��-SAXS technology in site measurement scorification crystal microscopic growth base unit particle diameter in the miniature crystal growing furnace of ��-SAXS commercial measurement, belong to the experimental technique field of material in site measurement of microscopic growth base unit size when crystal grows.
Background technology
Scorification crystal growth Study on Microcosmic Mechanism is the key of Study of Crystal Growth Mechanism, the method of microscopic growth base unit microstructure change in application high temperature micro Raman spectra in site measurement crystal growing process has been invented by Hefei material science research institute of the Chinese Academy of Sciences (Anhui light machine institute of the Chinese Academy of Sciences), and adapt to crystal growth thermal station (miniature crystal growing furnace) device of high temperature Raman in site measurement, the microscopic growth mechanism of tens kinds of crystal is studied, find the region that there is a structural transition between melt and crystal, this region is called as crystal growth boundary layer, the microscopic growth base unit formed in frictional belt has had some constitutional features of crystal list born of the same parents. the method and device obtain patent of invention and utility model patent mandate respectively, and the patent No. is respectively ZL01238010.5, ZL01113657.X.
But in crystal growth boundary layer, the differentiation mode of microscopic growth base unit is that quantity increases gradually or particle diameter is grown up gradually, is the insoluble problem of Raman spectroscopy, and this problem is very important for setting up new scorification crystal growth theories pattern. Synchrotron radiation small angle X ray scattering technology (SAXS) provides effective ways for head it off.
SAXS technology has effectively been applied to and has measured nanoclusters race particle diameter. When in x-ray bombardment to sample, if there is the uneven district of electron density of nanoscale in sample inside, then (general 2 �ȡ�6 ��) scattered x-ray can occur in the small angle range around incoming beam, this kind of phenomenon is called small angle X ray scattering (SmallAngleX-rayScattering), is abbreviated as SAXS. Its physical substance is the difference of the cloud density of scattering object and surrounding medium, and in its scatter intensity distribution and sample, nanoclusters race size and distribution is closely related, and SAXS technology has become that research submicron order is solid-state or the strong instrument of Liquid Structure.
In view of melt when scorification crystal grows and the growth unit particle diameter in frictional belt are in sub-micrometer scale, belonging within SAXS commercial measurement scope, therefore SAXS technology can be applied to the size and Changing Pattern thereof of measuring growth unit particle diameter in high-temperature fusant and frictional belt. The present invention is by the size of microscopic growth base unit in melt, frictional belt in synchrotron radiation ��-SAXS technology in site measurement crystal growing process, obtain the change information of different zones microscopic growth base unit size, it is a kind of novel method disclosing crystal growth microscopic mechanism.
Summary of the invention
Technical problem to be solved by this invention is to provide the method for synchrotron radiation ��-SAXS technology in site measurement scorification crystal microscopic growth base unit particle diameter and miniature crystal growing furnace, by the utilization of the method and growth furnace, size and the Changing Pattern of microscopic growth base unit particle diameter in frictional belt and melt regions can be measured.
Technical problem to be solved by this invention realizes by the following technical solutions:
The method of synchrotron radiation ��-SAXS technology in site measurement scorification crystal microscopic growth base unit particle diameter, its concrete steps are as follows:
Step 1, the raw material of growing crystal is placed in crucible, place the crystal microchip of one piece of function with seed crystal at an upper portion thereof simultaneously, thin slice bottom has in partial insertion crucible, and this crystal microchip is fixed on seed rod by platinum wire, and is regulated the position of crystal microchip by screw rod knob; Body of heater is placed on the experiment table at micro-beam X-ray scattered ray station, synchrotron radiation little angle; Open the X-ray source on synchrotron radiation line station, the position of adjustment body of heater, make micro-beam X-ray pass through the crystal microchip region in body of heater by entrance port, then close X-ray source;
Step 2, open cooling water system to unify electric heater, by temperature controller, electric heater is slowly heated up to body of heater, until raw material in crucible and crystal microchip go deep into the partial melting of crucible, crystal microchip and melt composition seed crystal is in upper melt-growth system, suitably regulate and stablize heating power, under the acting in conjunction of surface tension and capillarity, the region that one comprises melt and frictional belt will be formed at the bottom of crystal microchip, regulate the lifting device of experiment table pedestal, this region is made to be presented in the light path of X-ray of measurement, micro-beam X-ray respectively through frictional belt and melt regions and gather experimental data,
Step 3, image by the display experimentation of the CCD on small angle X ray scattering line station, can be observed two regions of frictional belt and melt in thin slice shape crystal growth system in micro furnace, microscopic growth base unit's size and changing conditions in site measurement two regions, obtain the rule of crystal microscopic growth base unit change of size.
The invention also discloses the miniature crystal growing furnace of synchrotron radiation ��-SAXS technology in site measurement scorification crystal microscopic growth base unit particle diameter, it comprises body of heater and bell, described body of heater and bell are bilayer structure, it it is circulating water channel between its bilayer structure, described body of heater and bell are respectively equipped with a prosopyle and posticum, prosopyle on described body of heater is connected with the posticum on bell by pipe connecting, and the posticum on described body of heater is connected with cooling water system with the prosopyle on bell;
It is provided with electric heater in described body of heater, this electric heater is made up of " U " shape corundum and platinum wire, described platinum wire is wrapped on " U " shape corundum, is provided with lagging material, is also placed with crucible in the middle of described " U " shape corundum between described " U " shape corundum periphery and inboard wall of furnace body;
A thermopair also it is provided with between described lagging material and " U " shape corundum;
Described body of heater both sides also have through hole, and wherein the through hole of side is that body of heater is outer to be connected with temperature controller for passing for the wire of electric heater, and another side is then be connected with temperature controller outside the data line for temperature thermocouple passes body of heater;
Described body of heater right on also has an entrance port, and the body of heater another side relative with entrance port also has an exit portal, and described entrance port communicates with exit portal;
Mid-way, described bell top has an apical pore, also fixes a support at described bell top, and the heart is equipped with a nut in the bracket, screw rod is had in described nut, having screw rod knob on the top of screw rod, be also provided with a clamping part in its bottom, this clamping part is provided with a seed rod.
Further, the lower end of described seed rod also has a platinum wire.
Further, described crucible is the crucible of flats platinum or other material.
Further, described entrance port and exit portal shape are rectangle, and enter, the caliber size of exit portal equal.
Further, the both sides, top of described crystal microchip have a recess, as the bayonet socket of the fixing LED reverse mounting type of platinum wire.
Further, the width of described crystal microchip and thickness are slightly less than width and the thickness of crucible bore.
Further, lagging material also it is filled with between described crucible bottom and " U " shape corundum.
The invention has the beneficial effects as follows:
1, this miniature crystal growing furnace is with the temperature control of the warm field design of uniqueness and precision, stable crystal, frictional belt and melt three part region can be formed, and make this three part be presented on measuring beam by scope, be that condition is created in the in site measurement of synchrotron radiation ��-SAXS technology;
2, achieve original position, real-time measurement, frictional belt and melt two region can be observed in crystal growing process, the size of microscopic growth base unit particle diameter in ��-SAXS technology in site measurement to two regions can be adopted again.
Accompanying drawing explanation
Fig. 1 is the miniature crystal growing furnace Facad structure schematic diagram of the present invention;
Fig. 2 is the present invention miniature crystal growing furnace side cut-away view;
Fig. 3 is part-structure enlarged diagram in Fig. 1;
Fig. 4 is crystal microchip of the present invention and crucible structure schematic diagram;
Fig. 5 is electric heater structural representation;
Fig. 6 is two regions that crystal microchip presents in body of heater.
Embodiment
In order to the present invention is realized technique means, character of innovation, reach object and effect is easy to understand, below in conjunction with concrete diagram, set forth the present invention further.
As shown in figures 1 to 6, the method for synchrotron radiation ��-SAXS technology in site measurement scorification crystal microscopic growth base unit particle diameter, its concrete steps are as follows:
First just the raw material of growing crystal is placed in crucible 7, again by ready crystal produced as sheets, and the both sides above crystal microchip 21 make recess 210 respectively, recess on this crystal microchip 21 is fixed on seed rod 19 by platinum wire 20, and is regulated the position of crystal microchip 21 by screw rod knob 17; Body of heater 1 is placed on the experiment table at micro-beam X-ray scattered ray station, synchrotron radiation little angle; Open the X-ray source on synchrotron radiation line station, the position of adjustment body of heater 1, make micro-beam X-ray pass through crystal microchip 21 region in body of heater 1 by entrance port 10, then close X-ray source;
Open cooling water system 4 and electric heater 5, by temperature controller 9, electric heater 5 is slowly heated up to body of heater 1, until raw material in crucible 7 and crystal microchip 21 (wafer) go deep into the partial melting of crucible 7, crystal microchip 21 and melt composition seed crystal is in upper melt-growth system, suitably regulate and stablize heating power, under the acting in conjunction of surface tension and capillarity, the bottom of crystal microchip 1 will form one and comprise melt 211 and the region in frictional belt 212, and make this region be presented in the light path of X-ray of measurement, micro-beam X-ray respectively through frictional belt 212 and melt 211 region and gather experimental data,
By the image of the display experimentation of the CCD on small angle X ray scattering line station, can be observed two regions of crystal growth boundary layer 212 and melt 211 in crystal microchip 21 growing system in micro furnace, microscopic growth base unit's size and changing conditions in site measurement two regions, obtain the rule of crystal microscopic growth base unit change of size.
As preferred embodiment, the width of above-mentioned crystal microchip 21 and thickness are slightly less than width and the thickness of crucible 7 bore.
As Figure 1-5, the invention also discloses the miniature crystal growing furnace of synchrotron radiation ��-SAXS technology in site measurement scorification crystal microscopic growth base unit particle diameter, it comprises body of heater 1 and bell 2, body of heater 1 and bell 2 are bilayer structure, it it is circulating water channel 100 between its bilayer structure, 200, body of heater 1 and bell 2 are respectively equipped with a prosopyle 101, 201 and posticum 102, 202, prosopyle 101 on body of heater 1 is connected with the posticum 202 on bell 2 by pipe connecting 3, posticum 102 on body of heater 1 is connected with cooling water system 4 with the prosopyle 201 on bell 2, electric heater 5 it is provided with in body of heater 1, this electric heater 5 is made up of " U " shape corundum 50 and platinum wire 51, platinum wire 51 is wrapped on " U " shape corundum 50, is provided with lagging material 6, is also placed with crucible 7 in the middle of " U " shape corundum 50 between " U " shape corundum 50 periphery and body of heater 1 inwall, a temperature thermocouple 8 also it is provided with so that it is do not have gaseous exchange around, to ensure to survey stability and the accuracy of temperature between lagging material 6 and " U " shape corundum 50,
Both sides, body of heater 1 bottom also have through hole 103, and wherein the through hole 103 of side is that body of heater 1 is outer to be connected with temperature controller 9 for passing for the wire 52 of electric heater 5, and another side is then be connected with temperature controller 9 outside the data line 80 for temperature thermocouple 8 passes body of heater 1;
Body of heater 1 right on also has an entrance port 10, and body of heater 1 another side relative with entrance port 10 also has an exit portal 11, and entrance port 10 communicates with exit portal 11;
Mid-way, bell 2 top has an apical pore 12, a support 14 is also fixed at bell 2 top, it is equipped with a nut 15 at support 14 center, screw rod 16 is had in nut 15, screw rod knob 17 is had on the top of screw rod 16, also be provided with a chuck 18 in its bottom, this chuck 18 is provided with a seed rod 19.
As preferred embodiment, above-mentioned seed rod 19 times ends also have a platinum wire 20.
As preferred embodiment, above-mentioned earthenware 7 crucible is flats platinum or other material crucible.
As preferred embodiment, above-mentioned entrance port 10 and exit portal 11 shape are rectangle, and enter, the caliber size of exit portal equal.
As preferred embodiment, at the bottom of described crucible, between 7 and " U " shape corundum 50, also it is filled with lagging material 60.
More than show and describe the ultimate principle of the present invention, main feature and advantage. The technician of the industry should understand; the present invention is not restricted to the described embodiments; the principle that the present invention is just described described in above-described embodiment and specification sheets; 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 (4)
1. the method for synchrotron radiation ��-SAXS technology in site measurement scorification crystal microscopic growth base unit particle diameter, it is characterised in that:
A, the raw material of growing crystal being placed in crucible, place one piece of crystal microchip simultaneously at an upper portion thereof, thin slice bottom has in partial insertion crucible, and this crystal microchip is fixed on seed rod by platinum wire, and is regulated the position of crystal microchip by screw rod knob; Body of heater is placed on the experiment table at micro-beam X-ray scattered ray station, synchrotron radiation little angle; Open the X-ray source on synchrotron radiation line station, the position of adjustment body of heater, make micro-beam X-ray pass through the crystal microchip region in body of heater by entrance port, then close X-ray source;
B, open cooling water system to unify electric heater, by temperature controller, electric heater is slowly heated up to body of heater, until raw material in crucible and crystal microchip go deep into the partial melting of crucible, crystal microchip and melt composition seed crystal is in upper melt-growth system, suitably regulate and stablize heating power, under the acting in conjunction of surface tension and capillarity, the region that one comprises melt and frictional belt will be formed at the bottom of crystal microchip, regulate the lifting device of experiment table pedestal, this region is made to be presented on the optical path of X-ray, micro-beam X-ray respectively through frictional belt and melt regions and gather experimental data,
C, image by the display experimentation of the CCD on small angle X ray scattering line station, can be observed two regions of frictional belt and melt in thin slice shape crystal growth system in micro furnace, microscopic growth base unit's size and changing conditions in site measurement two regions, obtain the rule of crystal microscopic growth base unit change of size.
2. the method for synchrotron radiation ��-SAXS technology in site measurement scorification crystal microscopic growth base according to claim 1 unit particle diameter, it is characterised in that: the both sides, top of described crystal microchip have a recess.
3. the method for synchrotron radiation ��-SAXS technology in site measurement scorification crystal microscopic growth base according to claim 1 unit particle diameter, it is characterised in that: the width of crystal microchip and thickness are slightly less than width and the thickness of crucible bore.
4. the miniature crystal growing furnace of a synchrotron radiation ��-SAXS technology in site measurement scorification crystal microscopic growth base unit particle diameter, it comprises body of heater and bell, described body of heater and bell are bilayer structure, it it is circulating water channel between its bilayer structure, described body of heater and bell are respectively equipped with a prosopyle and posticum, prosopyle on described body of heater is connected with the posticum on bell by pipe connecting, and the posticum on described body of heater is connected with cooling water system with the prosopyle on bell;
It is provided with electric heater in described body of heater, this electric heater is made up of " U " shape corundum and platinum wire, described platinum wire is wrapped on " U " shape corundum, is provided with lagging material, is also placed with crucible in the middle of described " U " shape corundum between described " U " shape corundum periphery and inboard wall of furnace body;
A thermopair also it is equipped with between described lagging material and " U " shape corundum;
Described lower portion of furnace body both sides also have through hole, and wherein the through hole of side is that body of heater is outer to be connected with temperature controller for passing for the wire of electric heater, and another side is then be connected with temperature controller outside the data line for thermopair passes body of heater, it is characterised in that:
Described body of heater right on also has an entrance port, and the body of heater another side relative with entrance port also has an exit portal, and described entrance port communicates with exit portal; Described entrance port and exit portal shape are rectangle, and enter, the caliber size of exit portal equal;
Lagging material also it is filled with between described crucible bottom and " U " shape corundum;
Mid-way, described bell top has an apical pore, also fixes a support at described bell top, and the heart is equipped with a nut in the bracket, screw rod is had in described nut, there is screw rod knob on the top of screw rod, also it is provided with a chuck in its bottom, fixing seed rod below on this chuck; The lower end of described seed rod also has the platinum wire of a fixing LED reverse mounting type.
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