CN104567402A - 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 - Google Patents
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 Download PDFInfo
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- CN104567402A CN104567402A CN201510017797.0A CN201510017797A CN104567402A CN 104567402 A CN104567402 A CN 104567402A CN 201510017797 A CN201510017797 A CN 201510017797A CN 104567402 A CN104567402 A CN 104567402A
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Abstract
The invention discloses an in situ measuring method for grain diameter of melting method crystal microscopic growth element via synchrotron radiation mu-SAXS technology, the change rule of the grain diameter of the crystal microscopic growth element from the melt to the crystal can be obtained by in situ measuring method for grain diameter of microscopic growth element in different regions (boundary layer, melt) based on the synchrotron radiation mu-SAXS technology; the micro crystal growing furnace used by the method is also provided, the in situ observation for the grain diameter of the microscopic growth element in the boundary layer and melt during the growing process of the crystal can be realized by the micro crystal growing furnace.
Description
Technical field
The methods and applications that the present invention relates to synchrotron radiation μ-SAXS technology in site measurement fusion method crystalline mi growth unit particle diameter, in the minicrystal growth furnace of μ-SAXS commercial measurement, belong to the experimental technique field of material in site measurement of microscopic growth primitive particle size when crystal growth.
Background technology
Fusion method crystal growth Study on Microcosmic Mechanism is the key of Study of Crystal Growth Mechanism, the method of microscopic growth primitive 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 ray machine institute of the Chinese Academy of Sciences), and adapt to crystal growth thermal station (minicrystal growth 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 primitive formed in boundary layer has had some architectural feature of crystal unit cell.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 primitive is that quantity increases gradually or particle diameter is grown up gradually, be the insoluble problem of Raman spectroscopy, and this problem is very important for setting up new fusion method crystal growth theories pattern.Synchrotron radiation Advance of Small-angle X-ray Scattering Technique (SAXS) provides effective ways for head it off.
SAXS technology has effectively been applied to measures 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 can (general 2 θ≤6 in the small angle range around incident beam
o) there is scattered x-ray, this phenomenon is called small angle X ray scattering (Small Angle X-ray Scattering), is abbreviated as SAXS.Its physical substance is the difference of the cloud density of scatterer and surrounding medium, and in its scatter intensity distribution and sample, nanoclusters race size and distribution is closely related, and SAXS technology has become the powerful of the solid-state or Liquid Structure of research submicron order.
In view of the growth unit particle diameter in melt during fusion method crystal growth and boundary layer is in sub-micrometer scale, belong 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 boundary layer.The present invention is by the particle size of microscopic growth primitive in melt, boundary layer in synchrotron radiation μ-SAXS technology in site measurement crystal growing process, obtaining the change information of zones of different microscopic growth primitive particle size, is a kind of new method disclosing crystal growth microscopic mechanism.
Summary of the invention
Technical matters to be solved by this invention is the method and the minicrystal growth furnace that provide synchrotron radiation μ-SAXS technology in site measurement fusion method crystalline mi growth unit particle diameter, by the utilization of the method and growth furnace, size and the Changing Pattern of microscopic growth primitive particle diameter in boundary layer and melt regions can be measured.
Technical matters to be solved by this invention realizes by the following technical solutions:
The method of synchrotron radiation μ-SAXS technology in site measurement fusion method crystalline mi growth unit particle diameter, its concrete steps are as follows:
Step 1, the raw material of grown crystal is placed in crucible, place the crystal microchip that a piece has the function of 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 regulates 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, makes micro-beam X-ray by entrance port through the crystal microchip region in body of heater, then can 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, suitable adjustment also stablizes heating power, under the acting in conjunction of surface tension and capillarity, the region that one comprises melt and boundary layer will be formed at the bottom of crystal microchip, regulate the jacking gear of experiment table pedestal, this region is made to be presented in the light path of the X ray of measurement, micro-beam X-ray gathers experimental data through boundary layer and melt regions respectively,
Step 3, image by the display experimentation of the CCD on small angle X ray scattering line station, can be observed two regions of boundary layer and melt in flake-like crystals growing system in micro furnace, microscopic growth primitive particle size and situation of change in site measurement two regions, obtain the rule of crystalline mi growth unit change of size.
The invention also discloses the minicrystal growth furnace of synchrotron radiation μ-SAXS technology in site measurement fusion method crystalline mi growth unit particle diameter, it comprises body of heater and bell, described body of heater and bell are double-decker, it is circulating water channel between its double-decker, described body of heater and bell are respectively equipped with an inlet opening and apopore, inlet opening on described body of heater is connected with the apopore on bell by connecting pipe, and the apopore on described body of heater is connected with cooling water system with the inlet opening on bell;
Electric heater is provided with 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 insulation material, in the middle of described " U " shape corundum, is also placed with crucible between described " U " shape corundum periphery and inboard wall of furnace body;
A thermopair is also provided with between described insulation material and " U " shape corundum;
Described body of heater both sides also have through hole, and wherein the through hole of side passes for the wire of fed heater that body of heater is outer to be connected with temperature controller, and opposite side is then pass for the data line of temperature thermocouple that body of heater is outer to be connected with temperature controller;
Described body of heater dead ahead 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 bell crown center position 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, have screw rod knob on the top of screw rod, be also provided with a holder in its bottom, this holder is provided with a seed rod.
Further, described seed rod lower end also has a platinum wire.
Further, described crucible is the crucible of flat platinum or other material.
Further, described entrance port and exit portal shape are rectangle, and enter, the caliber size of exit portal is equal.
Further, the both sides, top of described crystal microchip have a recess, fix the bayonet socket of LED reverse mounting type as platinum wire.
Further, the width of described crystal microchip and thickness are slightly less than width and the thickness of crucible bore.
Further, also insulation material is filled with between described crucible bottom and " U " shape corundum.
The invention has the beneficial effects as follows:
1, this minicrystal growth furnace controls with the temperature of the warm field design of uniqueness and precision, stable crystal, boundary layer and melt three subregion can be formed, and make this three part be presented on measuring beam by scope, for the in site measurement of synchrotron radiation μ-SAXS technology creates conditions;
2, achieve original position, real-time measurement, boundary layer and melt two region can be observed in crystal growing process, the size of microscopic growth primitive particle diameter in the in site measurement to two regions of μ-SAXS technology can be adopted again.
Accompanying drawing explanation
Fig. 1 is minicrystal growth furnace Facad structure schematic diagram of the present invention;
Fig. 2 is minicrystal growth furnace cross-sectional side view of the present invention;
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 structure schematic diagram;
Fig. 6 is two regions that crystal microchip presents in body of heater.
Embodiment
The technological means realized to make the present invention, character of innovation, reaching object and effect is easy to understand, below in conjunction with concrete diagram, setting forth the present invention further.
As shown in figures 1 to 6, the method for synchrotron radiation μ-SAXS technology in site measurement fusion method crystalline mi growth unit particle diameter, its concrete steps are as follows:
, first just the raw material of grown crystal be 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 regulates 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, makes micro-beam X-ray by entrance port 10 through crystal microchip 21 region in body of heater 1, then can 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, suitable adjustment also stablizes heating power, under the acting in conjunction of surface tension and capillarity, the region that one comprises melt 211 and boundary layer 212 will be formed at the bottom of crystal microchip 1, and make this region be presented in the light path of the X ray of measurement, micro-beam X-ray gathers experimental data through boundary layer 212 and melt 211 region respectively,
, 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 primitive particle size and situation of change in site measurement two regions, obtain the rule of crystalline mi growth 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 minicrystal growth furnace of synchrotron radiation μ-SAXS technology in site measurement fusion method crystalline mi growth unit particle diameter, it comprises body of heater 1 and bell 2, body of heater 1 and bell 2 are double-decker, it is circulating water channel 100 between its double-decker, 200, body of heater 1 and bell 2 are respectively equipped with an inlet opening 101, 201 and apopore 102, 202, inlet opening 101 on body of heater 1 is connected with the apopore 202 on bell 2 by connecting pipe 3, apopore 102 on body of heater 1 is connected with cooling water system 4 with the inlet opening 201 on bell 2, electric heater 5 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 insulation material 6, in the middle of " U " shape corundum 50, is also placed with crucible 7 between " U " shape corundum 50 periphery and body of heater 1 inwall, also be provided with a temperature thermocouple 8 between insulation material 6 and " U " shape corundum 50, make there is no gaseous exchange around it, to ensure stability and the accuracy of thermometric,
Both sides, body of heater 1 bottom also have through hole 103, and wherein the through hole 103 of side passes for the wire 52 of fed heater 5 that body of heater 1 is outer to be connected with temperature controller 9, and opposite side is then pass body of heater 1 for the data line 80 of temperature thermocouple 8 to be connected with temperature controller 9 outward;
Body of heater 1 dead ahead 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;
Bell 2 crown center position has an apical pore 12, a support 14 is also fixed at bell 2 top, a nut 15 is equipped with 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 lower end also has a platinum wire 20.
As preferred embodiment, above-mentioned earthenware 7 crucible is flat 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 is equal.
As preferred embodiment, at the bottom of described crucible, between 7 and " U " shape corundum 50, be also filled with insulation material 60.
More than show and describe 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; what describe in above-described embodiment and instructions 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.Application claims protection domain is defined by appending claims and equivalent thereof.
Claims (6)
1. the method for synchrotron radiation μ-SAXS technology in site measurement fusion method crystalline mi growth unit particle diameter, is characterized in that:
A, the raw material of grown crystal is placed in crucible, place one piece of crystal microchip 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 simultaneously, and regulates 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, makes micro-beam X-ray by entrance port through the crystal microchip region in body of heater, then can 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, suitable adjustment also stablizes heating power, under the acting in conjunction of surface tension and capillarity, the region that one comprises melt and boundary layer will be formed at the bottom of crystal microchip, regulate the jacking gear of experiment table pedestal, this region is made to be presented on the optical path of X ray, micro-beam X-ray can gather experimental data through boundary layer and melt regions respectively,
C, image by the display experimentation of the CCD on small angle X ray scattering line station, can be observed two regions of boundary layer and melt in flake-like crystals growing system in micro furnace, microscopic growth primitive particle size and situation of change in site measurement two regions, obtain the rule of crystalline mi growth unit change of size.
2. the method for synchrotron radiation μ-SAXS technology in site measurement fusion method crystalline mi growth unit particle diameter according to claim 1, is characterized in that: the both sides, top of described crystal microchip have a recess.
3. the method for synchrotron radiation μ-SAXS technology in site measurement fusion method crystalline mi growth unit particle diameter according to claim 1, is characterized in that: the width of crystal microchip and thickness are slightly less than width and the thickness of crucible bore.
4. the minicrystal growth furnace of a synchrotron radiation μ-SAXS technology in site measurement fusion method crystalline mi growth unit particle diameter, it comprises body of heater and bell, described body of heater and bell are double-decker, it is circulating water channel between its double-decker, described body of heater and bell are respectively equipped with an inlet opening and apopore, inlet opening on described body of heater is connected with the apopore on bell by connecting pipe, and the apopore on described body of heater is connected with cooling water system with the inlet opening on bell;
Electric heater is provided with 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 insulation material, in the middle of described " U " shape corundum, is also placed with crucible between described " U " shape corundum periphery and inboard wall of furnace body;
A thermopair is also equipped with between described insulation material and " U " shape corundum;
Described lower portion of furnace body both sides also have through hole, and wherein the through hole of side passes for the wire of fed heater that body of heater is outer to be connected with temperature controller, and opposite side is then pass for the data line of thermopair that body of heater is outer to be connected with temperature controller, it is characterized in that:
Described body of heater dead ahead 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;
Also insulation material is filled with between described crucible bottom and " U " shape corundum;
Described bell crown center position 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, be also provided with a chuck in its bottom, this chuck can be fixed seed rod below.
5. the minicrystal growth furnace of synchrotron radiation μ-SAXS technology in site measurement fusion method crystalline mi growth unit particle diameter according to claim 4, is characterized in that: described seed rod lower end also has a platinum wire can fixing LED reverse mounting type.
6. the minicrystal growth furnace of synchrotron radiation μ-SAXS technology in site measurement fusion method crystalline mi growth unit particle diameter according to claim 4, it is characterized in that: described entrance port and exit portal shape are rectangle, and enter, the caliber size of exit portal is equal.
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