CN205991950U - A kind of in situ X-ray diffraction diffraction test sample platform - Google Patents
A kind of in situ X-ray diffraction diffraction test sample platform Download PDFInfo
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- CN205991950U CN205991950U CN201620780020.XU CN201620780020U CN205991950U CN 205991950 U CN205991950 U CN 205991950U CN 201620780020 U CN201620780020 U CN 201620780020U CN 205991950 U CN205991950 U CN 205991950U
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Abstract
This utility model is related to a kind of in situ X-ray diffraction diffraction test sample platform, and it includes:Thermal station base plate;Ceramic heating flake;Cover on the upper front of described thermal station base plate and surround the outer housing of the sealing space for accommodating described ceramic heating flake with this thermal station base plate;The spike at multiple back sides being supported on described thermal station base plate;Platform base below described spike is supported on by a substrate;The temperature control equipment being connected with described heating wire and thermocouple;And it is connected the water-circulating cooling device to be cooled down to this thermal station base plate and outer housing with described thermal station base plate and outer housing.This utility model is placed in X-ray diffractometer and can realize the liter of testing sample under fine vacuum, hot environment gently lowering the temperature control, and because temperature control equipment and water-circulating cooling device are independent of each other, can be under conditions of ensureing water-circulating cooling device normal work, make example platform temperature be unlikely to too high, and do not affect the normal hot operation of ceramic heating flake.
Description
Technical field
This utility model is related to a kind of in-situ testing device, more particularly, to a kind of original position X for fine vacuum, hot environment
X ray diffraction test sample platform.
Background technology
The research of world today's material science just gradually from traditional observation era trend to the structure of matter in atom
On molecular level, is manipulated to matter and energy the epoch controlling.In order to preferably design, instruct and optimize functional material in nanometer
The even physics on atomic scale and chemical dynamics process, constantly reform and create existing matter and energy system, people
How to form and finally how to play the work process of its performance more concerned with material.Therefore, material micro-variations are deeply recognized
The mechanism of process and essence are the emphasis of current Science Times.
However, existing room temperature characterization technique cannot meet have studied of the dynamic process of various functions material,
In order to effectively manipulate the synthesis of material and the transmission controlling energy, particularly heavy to the structure change research in its pyroprocess
Will.X-ray, with its unique advantage, occupies irreplaceable status in terms of material microstructure study, and method of X-ray diffraction is several
Become material and characterize indispensable instrument.Therefore, develop real-time, dynamic in-situ high temperature X-ray characterization technique, special
It is not the X-ray original position diffraction experiment under high vacuum environment protection, in the forming process studying and manipulating material and its in high temperature
Most important during physical and chemical reaction under nonequilibrium state, and it is expected to more deep reason on the basis of original understanding
The forming process of solution functional material and work process.
But in the prior art although partly external commercial X-ray diffractometer is furnished with high temperature accessory at present, but due to it
Expensive, target is single, and is difficult to compatibility and is arranged on other X ray test equipment, thus result in in-situ high temperature X penetrating
The sign of line is extremely restricted.Therefore, development is practical, convenient, have preferable compatibility for fine vacuum, hot environment
In situ X-ray diffraction diffraction instrument is even more important.
Utility model content
In order to solve the problems, such as above-mentioned prior art, this utility model aims to provide a kind of in situ X-ray diffraction diffraction and surveys
Test agent platform, in order to carry out the X of original position on-line manner to the intensification of testing sample, high-temperature heat treatment and temperature-fall period
Ray diffraction studies.
A kind of in situ X-ray diffraction diffraction test sample platform described in the utility model, it includes:
Thermal station base plate;
It is erected at the ceramic heating flake for carrying sample of the upper front of described thermal station base plate, be internally provided with electric heating
Silk and thermocouple;
Cover on the upper front of described thermal station base plate and surround for accommodating described ceramic heating flake with this thermal station base plate
The outer housing of sealing space;
The spike at multiple back sides being supported on described thermal station base plate;
Platform base below described spike is supported on by a substrate, the sample of its X-ray diffractometer mounted externally
Product lifting platform axle head position;
It is connected with described heating wire and thermocouple with the temperature control equipment of ceramic heating flake temperature described in real-time control;With
And
It is connected the water-circulating cooling device to be cooled down to this thermal station base plate and outer housing with described thermal station base plate and outer housing.
In above-mentioned in situ X-ray diffraction diffraction test sample platform, the front of described thermal station base plate is additionally provided with two symmetrically
It is distributed in the boss of the opposite sides of described ceramic heating flake, each described boss is in three layers of stairstepping, and includes from top to bottom
Upper strata ladder, middle level ladder and lower floor's ladder, wherein,
Described lower floor ladder is fixedly mounted on the front of described thermal station base plate;
The top surface of described upper strata ladder is fixedly connected one end of a platinum filament by the first securing member, and the other end of this platinum filament is used
In described sample is fixed on described ceramic heating flake.
In above-mentioned in situ X-ray diffraction diffraction test sample platform, in the middle level of one of two described boss boss
The top surface of ladder and be located at this boss upper strata ladder both sides further respectively have with described heating wire and with described thermocouple
The binding post connecting;The back side of described thermal station base plate is provided with the conductive jack being connected correspondingly with described binding post, for
Described temperature control equipment passes through described conductive jack and binding post is connected with described heating wire and thermocouple.
In above-mentioned in situ X-ray diffraction diffraction test sample platform, described binding post passes through heating wire wire and heat respectively
Galvanic couple wire is connected with described heating wire and thermocouple, and wherein, described heating wire wire and thermocouple wire are all by earthenware bag
Wrap up in.
In above-mentioned in situ X-ray diffraction diffraction test sample platform, described water-circulating cooling device includes:Device body, set
Put the circulated water warehouse at the described thermal station base plate back side, the circulating water pipeline being connected between described circulated water warehouse and device body with
And it is arranged on the water cooled pipeline at described outer housing top, wherein, described water cooled pipeline is connected with described circulating water pipeline.
In above-mentioned in situ X-ray diffraction diffraction test sample platform, the back side of described thermal station base plate is additionally provided with one and is used for holding
Put the groove of described circulated water warehouse.
In above-mentioned in situ X-ray diffraction diffraction test sample platform, described ceramic heating flake passes through a heating plate bracing frame
It is erected at the upper front of described thermal station base plate.
In above-mentioned in situ X-ray diffraction diffraction test sample platform, described heating plate bracing frame includes being arranged on described pottery
Two of porcelain heating plate bottom surface be parallel to each other and the ceramics pole of horizontal expansion and be bearing in respectively described ceramics pole two ends
Cushion cap.
In above-mentioned in situ X-ray diffraction diffraction test sample platform, each described supporting table includes:
It is supported on the support sheet metal below described ceramics pole;
The compression sheet metal covering above described ceramics pole and be arrangeding in parallel with described support sheet metal;And
Two are arranged on the front of described thermal station base plate and pass through the second securing member and described support sheet metal and pressure respectively
The metal mainstay that the two ends of tight sheet metal are fixedly connected.
In above-mentioned in situ X-ray diffraction diffraction test sample platform, the forward and backward side of described outer housing is respectively equipped with front window
And rear window, its top surface is provided with roof window, its left and right side is respectively equipped with air vent and inflation inlet, wherein, described front window, after
Window and roof window are made by Kapton film.
Due to employing above-mentioned technical solution, this utility model is placed in X-ray diffractometer and can be in Gao Zhen
The liter realizing testing sample under empty, hot environment is gently lowered the temperature control, and due to temperature control equipment and water-circulating cooling device
It is independent of each other, example platform temperature can be made to be unlikely to too high under conditions of ensureing water-circulating cooling device normal work, and
Do not affect the normal hot operation of ceramic heating flake.In addition, the spike design of this device can thermal station base plate and substrate separately larger
Distance, decreases the impact to platform base for the heating, thus reaching the purpose that can carry out long high-temp in-situ experiment.
Brief description
Fig. 1 is a kind of structural representation of this utility model in situ X-ray diffraction diffraction test sample platform;
Fig. 2 is the schematic diagram of the Facad structure of thermal station base plate in this utility model;
Fig. 3 is the schematic diagram of the backside structure of thermal station base plate in this utility model;
Fig. 4 is the structural representation of outer housing in this utility model.
Specific embodiment
Below in conjunction with the accompanying drawings, provide preferred embodiment of the present utility model, and be described in detail.
As shown in figure 1, this utility model, i.e. a kind of in situ X-ray diffraction diffraction test sample platform, it includes:Thermal station base plate
1st, ceramic heating flake 2, outer housing 3, spike 4, platform base 5, temperature control equipment 6, water-circulating cooling device, wherein,
It is provided with heating wire and thermocouple (not shown), it is arranged by heating plate bracing frame 20 inside ceramic heating flake 2
In the upper front of thermal station base plate 1, and it is used for carrying sample (not shown);In the present embodiment, ceramic heating flake 2 adopts platinum
Gold as thermo electric material, its height that not only can heat up, long service life, and not oxide etch, there is no volatile matter, can guarantee that experiment
Atmosphere in cavity is pure;In addition, also adopting thermal conductive ceramic plane, its not only heatproof high, and post-heating plane of being heated is constant
Shape;High temperature sintering solidification after using high temperature adhesive bonding between thermo electric material and pottery;Ceramic heating flake 2 is by being propped up using heating plate
The high mounting design of support 20 frame, to reducing the conductive quantity to thermal station base plate 1 for the high temperature.
Outer housing 3 covers on the upper front of thermal station base plate 1, and surrounds for accommodating the close of ceramic heating flake 2 with thermal station base plate 1
Envelope space;
Spike 4 is supported on the back side of thermal station base plate 1;
Platform base 5 is supported on below spike 4 by substrate 50, thus by spike 4 by between substrate 50 and thermal station base plate 1
Separate, and this platform base 5 may be installed the sample lifting platform axle head position of external x-ray diffractometer;
Temperature control equipment 6 is connected with ceramic heating flake 2, with the temperature of precise control ceramic heating flake 2;
Water-circulating cooling device is connected with thermal station base plate 1 and outer housing 3, to cool down to thermal station base plate 1 and outer housing 3, from
And effectively reduce its temperature, thus significantly reduce the heat affecting to equipment for the high temperature.
As shown in Fig. 2 the front of thermal station base plate 1 is additionally provided with two opposite sides being symmetrically distributed in ceramic heating flake 2
Boss 10, each boss 10 is in three layers of stairstepping, and includes upper strata ladder 11 from top to bottom, middle level ladder 12 and lower floor's ladder
13, wherein,
Lower floor's ladder 13 is mounted by means of bolts on the front of thermal station base plate 1;
The top surface of middle level ladder 12 is apart from the height in thermal station base plate 1 front and the bottom surface of ceramic heating flake 2 apart from thermal station bottom
Plate 1 front highly consistent, i.e. the top surface of middle level ladder 12 is flushed with the bottom surface of ceramic heating flake 2;
The top surface of upper strata ladder 11 is fixedly connected one end of platinum filament 15 by the first securing member (such as housing pin) 14, should
The other end of platinum filament 15 is used for for sample being fixed on ceramic heating flake 2, can be by the platinum filament on two boss 10 by this sample
15 are fixed on ceramic heating flake 2;In the present embodiment, because the top surface of middle level ladder 12 is neat with the bottom surface of ceramic heating flake 2
Flat, platinum filament 15 compacting such that it is able to be easy on upper strata ladder 11 is placed on the sample on ceramic heating flake 2.
Meanwhile, the top surface in the middle level ladder 12 of one of two boss 10 boss 10 positioned at upper strata ladder 11 two
Side further respectively has two binding posts 16, and wherein, two binding posts 16 are by the heating wire wire positioned at ceramic heating flake 2 bottom surface
21 are connected with the heating wire within ceramic heating flake 2, and two other binding post 16 is by the thermoelectricity positioned at ceramic heating flake 2 bottom surface
Even wire 22 is connected with the thermocouple within ceramic heating flake 2.In addition, in order to high temperature resistant and prevent heating wire wire 21 and thermoelectricity
Even wire 22 is interconnected, and heating wire wire 21 and thermocouple wire 22 are all wrapped up with earthenware.
Again as shown in Fig. 2 heating plate bracing frame 20 include being arranged on two of ceramic heating flake 2 bottom surface be parallel to each other and
The ceramics pole 201 of horizontal expansion and the supporting station 202 being bearing in ceramics pole 201 two ends respectively between two boss 10, wherein,
Each supporting table 202 includes:
It is supported on the support sheet metal 2021 of ceramics pole 201 lower section;
The compression sheet metal 2022 covering above ceramics pole 201 and be arrangeding in parallel with support sheet metal 2021;And
Pass through on two fronts being arranged on thermal station base plate 1 and respectively the second securing member (such as housing pin) 2023 with
The metal mainstay 2024 that support sheet metal 2021 is fixedly connected with the two ends of compression sheet metal 2022;
Thus the end of ceramics pole 201 can be pressed between support sheet metal 2021 and compression sheet metal 2022.
As shown in figure 3, the back side of thermal station base plate 1 is provided with 4 conductive jacks being connected correspondingly with binding post 16 17,
So that temperature control equipment 6 passes through this conductive jack 17, binding post 16 and heating wire wire 21 and thermocouple wire 22 and pottery
Porcelain heating plate 2 connects.
Again as shown in figure 3, the back side of thermal station base plate 1 is additionally provided with a groove 18, water-circulating cooling device 7 includes:Device is originally
Body (not shown), the circulated water warehouse 71 being contained in this groove 18, it is connected to following between circulated water warehouse 71 and device body
Ring waterpipe 72 and the water cooled pipeline 73 (as shown in Figure 4) being arranged on outer housing 3 top, wherein, water cooled pipeline 73 passes through miniature
Band check valve is connect valve (not shown) and is connected with circulating water pipeline 72, and in the present embodiment, device body is, for example, SSRF
The water-cooling system of diffracted ray station configuration.
As shown in figure 4, outer housing 3 is in the trapezoidal shape of bottom-open, its forward and backward side is respectively equipped with front window 31, rear window 32,
Its top surface is provided with roof window 33, and its left and right side is respectively equipped with air vent 34 and inflation inlet 35, for outside air distribution system,
Vacuum system is attached thereto, thus realizing evacuation, filling/arrange the purposes such as shielding gas, wherein, front window 31, rear window 32 and roof window
33 are made by Kapton film (that is, Kapton), and with the sealing of sealing gasket (not shown), front window 31, rear window 32 can
Pass through for synchrotron radiation X light, roof window 33 is available for vertically light being used;The interface of the bottom of outer housing 3 and thermal station base plate 1 or seam crossing
All using Seal Design, thus the air-tightness in the space that outer housing 3 is surrounded with thermal station base plate 1 can be improved.It should be noted that it is outer
Cover 3 can also be using cylindrical, taper or rectangle etc., and the trapezoidal shape structure adopting in the present embodiment can effectively reduce outer
Cover space, thus be conducive to improving vacuum.It should be noted that this utility model vacuum system vacuum is up to 10-2Pa.
In addition, it is necessary to explanation, the temperature control equipment 6 in this utility model can adopt commonly used in the prior art
Online temperature control system is realized.Due in this platform and be not provided with any low-temperature accessory, so temperature controlled minimum temperature
It is preferably room temperature;Simultaneously as the heater strip in ceramic heating flake 2 is usually platinum rhodium heater strip, easily burn out more than 1100 degree,
So temperature controlled maximum temperature is no more than 1100 DEG C, so that this utility model is capable of from room temperature to 1100 DEG C
Online sign in situ.In addition, preferably 0 to 80 DEG C/min of the heating rate of temperature control equipment 6 is adjustable;At 1100 DEG C to 800
Preferably 0-400 DEG C/min of rate of temperature fall in the range of DEG C is adjustable, and the rate of temperature fall in the range of 800 DEG C to 500 DEG C is excellent
Elect as 0-600 DEG C/min adjustable, rate of temperature fall in the range of 500 DEG C to 300 DEG C is preferably 0 to -200 DEG C/min can
Adjust, preferably 0 to 50 DEG C/min of the rate of temperature fall in the range of 200 DEG C to room temperature is adjustable.
This utility model can be used for the situ measurement study at room temperature~1000 DEG C, under atmosphere protection or vacuum condition.This
Platform can be fixed on X-ray diffractometer sample lifting platform axle head position by platform base 5, by sample axle and diffractometer
Lifting rotation, complete sample centering and rotary test.Chamber between the outer housing 3 of this platform and thermal station base plate 1 has well
Air-tightness, vacuum-pumping or be filled with protective atmosphere, applicable sample includes thin film, powder and block etc..Specifically, this practicality
New operating process is as follows:
(1) testing sample is positioned on ceramic heating flake 2, and compresses the two ends of sample by two platinum filaments 15, to protect
Card sample is fixed on ceramic heating flake 2 in the rotary course of example platform all the time;
(2) example platform is put into X-ray diffractometer, and be fixedly mounted on the sample of X-ray diffractometer by platform base 5
Product lifting platform axle head position;
(3) wire of temperature control equipment 6 and control line are inserted the corresponding conductive jack 17 in thermal station base plate 1 back side respectively
Interior, to electrically connect with the heating wire and thermocouple of ceramic heating flake 2, wherein, temperature control equipment 6 passes through in ceramic heating flake 2
Actual temperature T1 to detect sample for the thermocouple, the then temperature difference Δ T=T1- according to actual temperature T1 and ideal temperature T0
The PID automatic control algorithm that T0 combination temperature control device 6 carry exports to the output of heating wire adjusting direct voltage source
Voltage, to realize liter gently degree of the cooling control to ceramic heating flake 2, passes through X ray test instrument synchronous collection corresponding simultaneously
The characterize data of the sample of temperature;
(4) open water circulating pump and switch, make current pass through circulating water pipeline 72 and circulate between water-cooling system import and export
Flowing, realizes the cooling effect to thermal station base plate 1, and passes through water cooled pipeline 73, realizes the cooling effect to outer housing 3.
In sum, this utility model has the advantages that:
(1) real time temperature control is carried out to ceramic heating flake by temperature control equipment, be easy to treat on-line manner
The intensification of test sample product, high-temperature heat treatment and temperature-fall period carry out the X-ray diffraction studies of original position.
(2) pass through to arrange platform base, can be in order to example platform be arranged on X-ray diffractometer sample lifting platform axle head
Position, by circulated water warehouse is arranged on the thermal station base plate back side, and arranges water cooled pipeline on outer housing, increases setting of spike simultaneously
Meter, ensure that under the normal running conditions of water-circulating cooling device, the temperature of the junction of example platform and X-ray diffractometer
Will not be too high, thus not damaging test instrunment.
(3) passing through setting heating plate bracing frame can make ceramic heating flake vacantly be fixed on the top of thermal station base plate, from
And so that temperature control equipment and water-circulating cooling device will not be influenced each other, can be in the normal work bar ensureing water-circulating cooling device
Under part, make example platform temperature be unlikely to too high, and do not affect the normal hot operation of ceramic heating flake.
(4) rational in infrastructure, safety is easy to operate, and heating-cooling speed is accurately controlled.
(5) compatibility good, be easy to carry, fast demountable.
Above-described, preferred embodiment only of the present utility model, it is not limited to scope of the present utility model, this
Above-described embodiment of utility model can also make a variety of changes.I.e. every claims according to this utility model application and
Simple, equivalence changes and modification that description is made, fall within the claims of this utility model patent.This
The not detailed description of utility model be routine techniquess content.
Claims (10)
1. a kind of in situ X-ray diffraction diffraction test sample platform is it is characterised in that described platform includes:
Thermal station base plate;
Be erected at the ceramic heating flake for carrying sample of the upper front of described thermal station base plate, be internally provided with heating wire and
Thermocouple;
Cover on the upper front of described thermal station base plate and surround the sealing for accommodating described ceramic heating flake with this thermal station base plate
The outer housing in space;
The spike at multiple back sides being supported on described thermal station base plate;
Platform base below described spike is supported on by a substrate, the sample liter of its X-ray diffractometer mounted externally
Fall platform axle head position;
It is connected with described heating wire and thermocouple with the temperature control equipment of ceramic heating flake temperature described in real-time control;And
It is connected the water-circulating cooling device to be cooled down to this thermal station base plate and outer housing with described thermal station base plate and outer housing.
2. in situ X-ray diffraction diffraction test sample platform according to claim 1 is it is characterised in that described thermal station base plate
Front is additionally provided with the boss of two opposite sides being symmetrically distributed in described ceramic heating flake, and each described boss is in three layers of ladder
Shape, and include upper strata ladder from top to bottom, middle level ladder and lower floor's ladder, wherein,
Described lower floor ladder is fixedly mounted on the front of described thermal station base plate;
The top surface of described upper strata ladder is fixedly connected one end of a platinum filament by the first securing member, and the other end of this platinum filament is used for will
Described sample is fixed on described ceramic heating flake.
3. in situ X-ray diffraction diffraction test sample platform according to claim 2 is it is characterised in that in two described boss
One of the top surface of middle level ladder of boss be located at the both sides of upper strata ladder of this boss and further respectively have and described electric heating
Silk and the binding post being connected with described thermocouple;The back side of described thermal station base plate is provided with and is connected correspondingly with described binding post
The conductive jack connecing, so that described temperature control equipment passes through described conductive jack and binding post and described heating wire and thermocouple
Connect.
4. in situ X-ray diffraction diffraction test sample platform according to claim 3 is it is characterised in that described binding post is distinguished
It is connected, wherein, described heating wire wire and thermoelectricity with described heating wire and thermocouple by heating wire wire and thermocouple wire
Even wire is all wrapped up by earthenware.
5. in situ X-ray diffraction diffraction test sample platform according to claim 1 is it is characterised in that described water-circulating cooling
Put including:Device body, it is arranged on the circulated water warehouse at the described thermal station base plate back side, is connected to described circulated water warehouse and device body
Between circulating water pipeline and the water cooled pipeline being arranged on described outer housing top, wherein, described water cooled pipeline and described circulation
Waterpipe connects.
6. in situ X-ray diffraction diffraction test sample platform according to claim 5 is it is characterised in that described thermal station base plate
The back side is additionally provided with one for housing the groove of described circulated water warehouse.
7. in situ X-ray diffraction diffraction test sample platform according to claim 1 is it is characterised in that described ceramic heating flake
It is erected at the upper front of described thermal station base plate by a heating plate bracing frame.
8. in situ X-ray diffraction diffraction test sample platform according to claim 7 is it is characterised in that described heating plate supports
Frame includes being arranged on two of described ceramic heating flake bottom surface and is parallel to each other and the ceramics pole of horizontal expansion and being bearing in respectively
The supporting station at described ceramics pole two ends.
9. in situ X-ray diffraction diffraction test sample platform according to claim 8 is it is characterised in that each described supporting table
Including:
It is supported on the support sheet metal below described ceramics pole;
The compression sheet metal covering above described ceramics pole and be arrangeding in parallel with described support sheet metal;And
Two are arranged on the front of described thermal station base plate and pass through the second securing member and described support sheet metal and compression gold respectively
Belong to the metal mainstay that the two ends of piece are fixedly connected.
10. in situ X-ray diffraction diffraction test sample platform according to claim 1 it is characterised in that before described outer housing,
Front window and rear window are respectively equipped with trailing flank, its top surface is provided with roof window, its left and right side is respectively equipped with air vent and inflation
Mouthful, wherein, described front window, rear window and roof window are made by Kapton film.
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CN110865090A (en) * | 2019-12-23 | 2020-03-06 | 陕西师范大学 | Portable variable-temperature die of powder diffractometer and application |
CN111624216A (en) * | 2020-07-23 | 2020-09-04 | 丹东通达科技有限公司 | Detection device for measuring sample characteristics of X-ray diffractometer at high temperature |
CN111624216B (en) * | 2020-07-23 | 2023-09-19 | 丹东通达科技有限公司 | Detection device for measuring sample characteristics of X-ray diffractometer at high temperature |
CN112834538A (en) * | 2021-01-08 | 2021-05-25 | 南京大学 | Variable-temperature sample stage for XRD (X-ray diffraction) and atomic force microscope and using method thereof |
CN112986292A (en) * | 2021-02-08 | 2021-06-18 | 中国科学院上海应用物理研究所 | Temperature-stress coupled X-ray in-situ measuring device |
CN115683988A (en) * | 2022-09-29 | 2023-02-03 | 西北核技术研究所 | Radiation effect research test device and method |
CN115683988B (en) * | 2022-09-29 | 2024-08-16 | 西北核技术研究所 | Radiation effect research test device and method |
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