CN101482525A - High-temperature heating equipment used for orientation texture measurement - Google Patents
High-temperature heating equipment used for orientation texture measurement Download PDFInfo
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- CN101482525A CN101482525A CNA2009100457656A CN200910045765A CN101482525A CN 101482525 A CN101482525 A CN 101482525A CN A2009100457656 A CNA2009100457656 A CN A2009100457656A CN 200910045765 A CN200910045765 A CN 200910045765A CN 101482525 A CN101482525 A CN 101482525A
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Abstract
The invention relates to a high-temperature heating device for measuring the orientation texture in a measurement technical field, comprising a heating furnace, a heating element, a sample stage, a sample rack, a thermocouple, a water cooling pipe, a step motor, wherein the exterior of the heating furnace is a ceramics socket sleeve and a spiral drum type heating element is embedded into the heating furnace and the heating furnace is set on the sample stage; and the sample rack is set in the step motor and separated from the heating furnace, capable of rotating along the self-axle in the heating furnace; a water cooling pipe is set at the lower part of the sample rack and coils in parallel with the sample undersurface to form a cooling plane; and the thermocouple is set in the heating furnace. During heating process, the sample can rotate and the uniform heating of sample can be ensured; at the same time the rotation is consistent with the Phi rotation in general texture measurement, thereby ensuring the texture measurement at high-temperature; in addition, the whole of the heating furnace is set on the texture measurement stage, thus Psi rotation of stress rolling method, therefore the high-temperature stress measurement can be performed.
Description
Technical field
The present invention relates to a kind of device of field of measuring technique, specifically, what relate to is a kind of high-temperature heating equipment that is used for orientation texture measurement.
Background technology
X-ray diffraction technology (XRD) is one of basic means that characterizes the structure of matter, and except that conventional crystal structure analysis, it can also carry out qualitative, the quantitative test of crystal orientation and texture.So-called " texture " is meant that in the polycrystal crystal orientation of many crystal grain appears at the concentrated distribution on a certain or some particular space direction.Different with the Bragg cone that general powdered sample forms in the space; the diffracted signal of texture sample can form some spots usually on the specific direction of space; this just requires sample except that can carrying out θ-2 θ rotation, and the axle that can also carry out φ rotation and parallel sample surfaces around the axle of vertical sample surfaces carries out x and rotates.Monocrystalline, accurate monocrystalline, epitaxial film, plated film and pressure rolling sheet metal are the main samples that orientation or texture are arranged, wherein some monocrystalline, epitaxial film and pressure rolling preparation of plates need be carried out under hot conditions, and it is very necessary therefore to measure their crystal orientation or TEXTURE STATE under hot conditions.
The high temperature sample stage that the at present domestic and international main manufacturing firm of XRD provides only limits to carry out the measurement of powdered sample, the HTK16 high temperature sample cavity that provides as German BRUKER company can be heated to powdered sample 1300 degree and measure, and WATLOW 988 type warm tables can be heated to the kapillary sample 500 degree; A series of high temperature platforms of other manufacturer such as Dutch PANalytical (Panalytical) HTK1200 type, Japan (Rigaku) of science also only provide the high-temperature heating process of common sample, and still do not have any report at the heating arrangement of texture sample.
High temperature orientation texture measurement device is the high-temperature heating equipment of constructing on the texture measurement specimen holder, the technical difficulty of its design is: the introducing of this device can not influence sample one of any rotation on θ, 2 θ, φ and x four direction, all the time accurately be positioned at the center of diffraction ball and the accurate control of heating condition in any case will guarantee to rotate sample simultaneously, introducing device also should not influence the collection to diffraction information in addition.
Find through literature search prior art, (the patent No.: ZL200620079376.7) that China's utility model patent " is taken into account the XRD sample table device that orientation and non-oriented crystal are analyzed ", be specially: the sample stage main body that keeps X diffractometer conventionally test, increased the spin orientation device of suitable orientation sample measurement in the side with base, its deficiency is: can't finish x and rotate and high temperature measurement.The rich efforts of everyone etc. are published in MATERIALS SCIENCE FORUM (material science forum) (Volume:475-479,2005, Pages:4183-4186, Part:Part 1-5) paper " The orientation characterization ofsingle crystal superconductor film with 2-dimensional x-ray diffraction " (direction characterizes monocrystalline superconducting thin film two-dimensional x-ray diffraction) adopts the two positions x angle measurement platform of Bruker company to finish the measurement of orientation utmost point figure, and weak point is: do not have heating arrangement can't finish measurement under the hot conditions.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art, a kind of high-temperature heating equipment that is used for orientation texture measurement is provided, this device can be finished from room temperature to a certain specified temp in (as 1600 degree, depending primarily on the heating furnace Material Selection) scope the real-time texture orientation under continuous or a series of different temperatures and measure.In addition, can simulate the temperature conditions of some crystal growth, for preparation degree of orientation crystal good, excellent quality is groped best growth conditions.The present invention can also measure the variation of material stress under hot conditions.
The present invention is achieved by the following technical solutions, the present invention includes heating furnace body, heating element, sample stage, specimen holder, thermopair, water-cooled pipeline, stepper motor, the heating furnace body outside is ceramic cover for seat, embedded heating element, and the type of heating element is looked the design maximum temperature and is selected; Heating furnace body is arranged on the sample stage; Specimen holder is put into stepper motor, separates with heating furnace body, can rotate by the axle around self in heating furnace body, and this φ that finishes on the one hand in the texture measurement rotates, and sample is evenly heated; The water-cooled pipeline is arranged at the specimen holder bottom, and the coiling of its parallel sample lower surface forms cooling and plane; There is thermopair to contact with the temperature on measuring samples surface in the heating furnace body and also controls heating-cooling velocity with the sample bottom.
Described heating cover for seat is the one-piece construction that branch has upper and lower two parts cavity, upper chamber embeds heating element, lower cavity is placed stepper motor, there is insulating pad layer upper and lower cavity separated place, there is hole at the center, specimen holder passes one of them hole and is connected with stepper motor, and cooling line stretches into epicoele by two holes from the cavity of resorption of heating cover for seat, and the lower disc of specimen holder around.
Described thermopair stretches out along the direction of specimen holder from heating cover for seat bottom, places the lower surface or the upper surface center of sample.
Described heating element adopts the spiral tubular construction, is close to the inwall that heats cover for seat.
Concrete job step during measurement: at first sample is placed in the specimen holder, and the axis of rotation of the surface that guarantees sample and specimen holder is vertical and with the upper port that heats cover for seat on same plane, starting the external heating control system starts working heating element, stepper motor begins to rotate simultaneously, when the temperature of thermopair feedback and preset temperature near the time, water-cooling system work starts, and firing rate reduces simultaneously; After arriving design temperature, regulating water velocity and firing rate respectively is that the two reaches dynamic thermal equilibrium, thus near the fluctuation among a small circle design temperature of the temperature of control sample surfaces; Can begin the texture orientation this moment and measure Information Monitoring.
The present invention be directed to existing XRD instrument and under hot conditions, measure the crystal orientation of texture sample or the variation of TEXTURE STATE, it can be heated to a certain high-temperature temperature by room temperature with sample, and be stabilized in and carry out the texture degree of orientation under a certain specified temp and measure, this crystal quality for monocrystalline oriented growth, epitaxial film provides optimized parameters, and also texture, the crystal orientation variation for various types of materials under the researching high-temperature state provides a kind of reliable experiment method.
Beneficial effect of the present invention: in heating process, sample can rotate, and has guaranteed being heated evenly of sample, and this rotation simultaneously is consistent with the φ rotation in the common texture measurement, can guarantee to carry out under hot conditions texture measurement; This externally heated oven integral body is on sample stage, and the ψ that can also finish stress inclination method like this rotates, and measures thereby can carry out high temperature stress.
Application scenario of the present invention comprises: the research temperature variation is to the texture orientation influence of material; Detect the crystal growth orientation in the crystal high-temperature growth course and change definite best growth technique; The stress state of test material under hot conditions determined best stress relief annealing technology.
Description of drawings
Fig. 1 is the structural representation of the embodiment of the invention
Embodiment
Below in conjunction with accompanying drawing embodiments of the invention are elaborated: present embodiment is being to implement under the prerequisite with the technical solution of the present invention, provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1
As shown in Figure 1, the measurement mechanism that present embodiment relates to comprises heating furnace body (not marking among the figure), heating element 2, specimen holder 3, thermopair 5, water-cooled pipeline 6, stepper motor 7, sample stage base 9, the heating furnace body outside is ceramic cover for seat 1, embedded heating element 2, heating furnace body are arranged on the sample stage base 9; Specimen holder 3 is put into stepper motor 7, separates with heating furnace body, can rotate by the axle around self in heating furnace body, and this φ that finishes on the one hand in the texture measurement rotates, and sample is evenly heated; Water-cooled pipeline 6 is arranged at specimen holder 3 bottoms, and the coiling of its parallel sample lower surface forms cooling and plane; There is thermopair 5 to contact with the temperature on measuring samples surface in the heating furnace body and also controls heating-cooling velocity with the sample bottom.
In the present embodiment, heating cover for seat 1 is the one-piece construction that branch has upper and lower two parts cavity, and upper chamber embeds heating element 2, and the type of heating element is looked the design maximum temperature and selected; Lower cavity is mainly placed stepper motor 7, there is insulating pad layer 4 separated place, and there is hole at the center, and specimen holder 3 can pass this hole and be connected with stepper motor 7, have cooling line 6 to stretch into epicoele from the cavity of resorption of cover for seat 1 in addition by other two holes, and the lower disc of specimen holder 3 around; Sample is installed in the upper end of specimen holder 3, and when specimen holder 3 rotated under stepper motor 7 drives, sample also rotated thereupon.
In the present embodiment, thermopair 5 stretches out along the direction of specimen holder 3 from heating cover for seat 1 bottom, places the lower surface or the upper surface center of sample during measurement.
In the present embodiment, heating element 2 adopts the spiral tubular construction, is close to the inwall that heats cover for seat 1.
In the present embodiment, heating cover for seat 1 is connected with sample stage base 9 usefulness bolts 8.
The specimen that present embodiment uses is block or Powdered, bulk sample be processed into be fit to specimen holder 3 sizes, regular shape can be directly used in measurement; Powdered sample will be packed into earlier and be put into specimen holder 3 more together behind the center hole groove of ceramics sample frame and measure.Whole heating arrangement is installed to by sample stage base 9 to have on the angle measurement platform that x rotates, and this step is installed the center of circle of the upper surface that should guarantee to heat cover for seat and the diffraction center inregister of diffractometer.
Sample is put into specimen holder 3, specimen holder 3 is that 4 pawl type stupaliths are made, and has reduced the obstruction that sample is heated so preferably, puts into the axle of stepper motor 7 then, heating element 2 adopts Elema or Si-Mo rod, and maximum temperature can reach the 1200-1600 degree.Thermopair 5 contacts with sample surfaces, and measurement result can further feed back to heating controller and water flow controller to remain on the constant of a certain temperature.
Embodiment 2
The installation of sample is with embodiment 1, heating element 2 adopts electric heating coil or electrothermal tube, heating-up temperature can reach the 500-800 degree, and sample stage 9 bases are installed on the outstanding draw ring sample stage of 1/4 circle, and the x by outstanding draw ring rotates the ψ that realizes in the inclination stress measurement method fascinate (relation that the two has x=90 °-ψ).
Concrete steps are: sample is placed on the specimen holder 3, confirm that the diffraction center is in the sample surfaces plane, (scope is usually at 110-160 ° to select 2 specific θ values according to the crystallography characteristics of sample, when the plain carbon steel exemplar being adopted CrK α radiation source 156 ° of measurements), forward detector and light pipe to corresponding angle position respectively, start heating arrangement this moment, begins to carry out the inclination normal stress when waiting to reach preset temperature and measure.In ψ=0 °, ± 15 °, ± 25 °, ± 30 °, ± 35 °, ± 40 °, select the measurement of fascinating of some different ψ position in ± 45 ° of these angles, ψ fascinates and finishes by the slip of sample stage base 9 on outstanding draw ring sample stage, and stepper motor 7 rotates (measuring simultaneously, sample carries out the φ rotation) simultaneously when each ψ position measurement, has increased the harmful effect to measurement result of number, the big crystal grain of elimination and the texture of tested crystal grain like this.At last measurement data is carried out ε-sin
2The measuring and calculating of sample stress value is finished in the ψ processing of mapping, thereby realizes sin under the specified temp
2The material stress of ψ method is measured.
Claims (4)
1, a kind of high-temperature heating equipment that is used for orientation texture measurement, comprise heating furnace body, heating element, sample stage, specimen holder, thermopair, water-cooled pipeline, stepper motor, the heating furnace body outside is ceramic cover for seat, and embedded heating element, heating furnace body are arranged on the sample stage; Specimen holder is put into stepper motor, separates with heating furnace body, and the water-cooled pipeline is arranged at the specimen holder bottom, and its parallel sample lower surface coiling forms cooling and plane, thermopair is arranged in the heating furnace body and contacts with the sample bottom.
2, the high-temperature heating equipment that is used for orientation texture measurement according to claim 1, it is characterized in that, described heating cover for seat is the one-piece construction that branch has upper and lower two parts cavity, upper chamber embeds heating element, and lower cavity is placed stepper motor, and there is insulating pad layer upper and lower cavity separated place, there is hole at the center, specimen holder passes one of them hole and is connected with stepper motor, and cooling line stretches into epicoele by two holes from the cavity of resorption of heating cover for seat, and the lower disc of specimen holder around.
3, the high-temperature heating equipment that is used for orientation texture measurement according to claim 1 is characterized in that, described thermopair stretches out along the direction of specimen holder from heating cover for seat bottom, places the lower surface or the upper surface center of sample.
4, the high-temperature heating equipment that is used for orientation texture measurement according to claim 1 and 2 is characterized in that, described heating element is the spiral tubular construction, is close to the inwall that heats cover for seat.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101750427B (en) * | 2009-12-31 | 2011-11-16 | 中国科学院等离子体物理研究所 | Temperature controlling sample holder capable of adjusting incident ion energy and monitoring ion flux in real time |
| CN103207192A (en) * | 2013-04-08 | 2013-07-17 | 中国科学技术大学 | Biaxial uniaxial tension device for in-situ structure detection in combination with scattering of X-rays and experimental method thereof |
| CN107419327A (en) * | 2017-07-24 | 2017-12-01 | 共慧冶金设备科技(苏州)有限公司 | Sigmatron three dimensions imaging bridgman furnace |
| CN109210941A (en) * | 2018-09-06 | 2019-01-15 | 大连理工大学 | A kind of Reflection X-ray original position diffraction heating furnace |
| CN110784947A (en) * | 2019-10-29 | 2020-02-11 | 北京理工大学 | Heating device and heating method for heating sample before flat plate impact experiment |
-
2009
- 2009-02-05 CN CNA2009100457656A patent/CN101482525A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101750427B (en) * | 2009-12-31 | 2011-11-16 | 中国科学院等离子体物理研究所 | Temperature controlling sample holder capable of adjusting incident ion energy and monitoring ion flux in real time |
| CN103207192A (en) * | 2013-04-08 | 2013-07-17 | 中国科学技术大学 | Biaxial uniaxial tension device for in-situ structure detection in combination with scattering of X-rays and experimental method thereof |
| CN103207192B (en) * | 2013-04-08 | 2016-08-03 | 中国科学技术大学 | With twin shaft simple tension device and the experimental technique thereof that X-ray scattering combination carries out structure detection in situ |
| CN107419327A (en) * | 2017-07-24 | 2017-12-01 | 共慧冶金设备科技(苏州)有限公司 | Sigmatron three dimensions imaging bridgman furnace |
| CN109210941A (en) * | 2018-09-06 | 2019-01-15 | 大连理工大学 | A kind of Reflection X-ray original position diffraction heating furnace |
| CN110784947A (en) * | 2019-10-29 | 2020-02-11 | 北京理工大学 | Heating device and heating method for heating sample before flat plate impact experiment |
| CN110784947B (en) * | 2019-10-29 | 2020-10-27 | 北京理工大学 | Heating device and heating method for heating sample before flat plate impact experiment |
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