CN109556970A - A kind of device in situ for small-angle neutron scattering experiment high temperature and stretching coupling load - Google Patents

A kind of device in situ for small-angle neutron scattering experiment high temperature and stretching coupling load Download PDF

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Publication number
CN109556970A
CN109556970A CN201811559897.6A CN201811559897A CN109556970A CN 109556970 A CN109556970 A CN 109556970A CN 201811559897 A CN201811559897 A CN 201811559897A CN 109556970 A CN109556970 A CN 109556970A
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China
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high temperature
small
situ
temperature
load
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CN201811559897.6A
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Chinese (zh)
Inventor
陈东风
孙凯
王子军
李天富
李博楠
张莉
刘荣灯
刘蕴韬
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China Institute of Atomic of Energy
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China Institute of Atomic of Energy
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Priority to CN201811559897.6A priority Critical patent/CN109556970A/en
Publication of CN109556970A publication Critical patent/CN109556970A/en
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N3/00Investigating strength properties of solid materials by application of mechanical stress
    • G01N3/08Investigating strength properties of solid materials by application of mechanical stress by applying steady tensile or compressive forces
    • G01N3/18Performing tests at high or low temperatures
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/20Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
    • G01N23/201Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials by measuring small-angle scattering
    • G01N23/202Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials by measuring small-angle scattering using neutrons
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2203/00Investigating strength properties of solid materials by application of mechanical stress
    • G01N2203/0014Type of force applied
    • G01N2203/0016Tensile or compressive
    • G01N2203/0017Tensile
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2203/00Investigating strength properties of solid materials by application of mechanical stress
    • G01N2203/02Details not specific for a particular testing method
    • G01N2203/022Environment of the test
    • G01N2203/0222Temperature
    • G01N2203/0226High temperature; Heating means

Abstract

The present invention relates to a kind of for small-angle neutron scattering experiment high temperature and stretches the device in situ of coupling load, including loading frame, high-temperature clamp and high temperature furnace;The high temperature furnace and high-temperature clamp are installed on the loading frame;The high-temperature clamp protrudes into the high temperature furnace and carries out stretching operation to sample;Middle child window is provided on the high temperature furnace.Beneficial effects of the present invention are as follows: 1) using the arrangement achieves the small-angle neutron scattering of high temperature and stretching coupling load, experiment is measured in situ.2) high temperature furnace shape is cuboid, includes two pieces of flat-plate heating bodies, is symmetrically arranged, and slot milling arrangement sample and high-temperature clamp, can make Proper Design beauty compact, sample position temperature is uniform in this way among two pieces of heaters.High temperature furnace reduces the decaying to neutron to the greatest extent while guaranteeing sealing.Be conducive to obtain biggish scattering angle simultaneously, collect the high Q data of small-angle scattering.

Description

A kind of device in situ for small-angle neutron scattering experiment high temperature and stretching coupling load
Technical field
The invention belongs to Neutron scattering technologies, and in particular to one kind is for small-angle neutron scattering experiment high temperature and stretches coupling The device in situ of load.
Background technique
Current neutron scattering experiment room major in the world all measures material using small-angle neutron scattering technology actively developing The related work of nanoscale microstructure, but specially design and produce small for the original position under the conditions of high temperature and stretching coupling Angle neutron scattering experiment device yet there are no open source literature report.
Currently, having high-temp in-situ device for small-angle neutron scattering spectrometer, also there is tensile load original position device;But These devices are unable to satisfy while carrying out tensile load and temperature coupling experiment to sample, and the prior art is merely by the two Test the processing of obtained data individually theoretically analyzed the case where coupling, which not necessarily meets Actual conditions.
Therefore, it is necessary to complete a kind of drawing by high temperature coupling load experiment dress in situ for small-angle neutron scattering measurement It sets, can meet while carry out under the conditions of high temperature relents tensile loads to sample the primary demand of small-angle neutron scattering measurement, Further expand the range of Neutron scattering technology research application.
In view of this, the present invention is specifically proposed.
Summary of the invention
In view of the deficiencies in the prior art, the object of the present invention is to provide it is a kind of for small-angle neutron scattering measurement Drawing by high temperature coupling loads experimental provision in situ, can meet while carry out under the conditions of high temperature relents tensile loads to sample small The primary demand of angle neutron scattering measurement further expands the range of Neutron scattering technology research application.
Technical scheme is as follows:
A kind of device in situ for small-angle neutron scattering experiment high temperature and stretching coupling load, including loading frame, height Warm fixture and high temperature furnace;The high temperature furnace and high-temperature clamp are installed on the loading frame;The high-temperature clamp protrudes into institute It states in high temperature furnace and stretching operation is carried out to sample;Middle child window is provided on the high temperature furnace.
Further, the above-mentioned device in situ for small-angle neutron scattering experiment high temperature and stretching coupling load, it is described High-temperature clamp includes upper connecting rod, connecting rod, collet and lower pull rod;Described upper connecting rod one end is installed on the loading frame, separately One end is connect by the connecting rod with the collet;Described style one end is connect with the collet, the other end and the drop-down Bar connection;The lower pull rod and loading mechanism are drivingly connected to stretch the sample under the driving of the loading mechanism.
Further, the above-mentioned device in situ for small-angle neutron scattering experiment high temperature and stretching coupling load, it is described Loading mechanism includes ball-screw and load actuator;The ball wire and driving mechanism are drivingly connected;The load actuator Be mounted on the loading frame and fixed with the screw of ball-screw, in the load actuator install rotation-preventing mechanism so that plus Carrying actuator can only move up and down without being able to rotate;Load cell is installed in the load actuator.
Further, the above-mentioned device in situ for small-angle neutron scattering experiment high temperature and stretching coupling load, it is described Temperature compensation module is provided on load cell.
Further, the above-mentioned device in situ for small-angle neutron scattering experiment high temperature and stretching coupling load, it is described High-temperature clamp further includes high-temperature extensometer, the high-temperature extensometer include the upper snap ring being connected with the sample and with the drop-down The connected lower snap ring of bar;Bar of extending is connected between the upper snap ring and lower snap ring;The lower snap ring can be along the bar of extending It is mobile;The bar end of extending is equipped with grating sensor.
Further, the above-mentioned device in situ for small-angle neutron scattering experiment high temperature and stretching coupling load, it is described The pin hole with the screw thread of cylindrical sample head fits and/or with the cooperation of tabular sample is provided on collet.
Further, the above-mentioned device in situ for small-angle neutron scattering experiment high temperature and stretching coupling load, it is described High temperature furnace includes stove outer covering, bell, muffle tube, ceramic end seat, magnetic board and heater;The bell is opposite with the stove outer covering Fixed, muffle tube is supported in the end seat being installed on the bell;The heater is mounted in the groove of the muffle tube; The electrode plate is installed on the stove outer covering;Middle child window is located at the two sides of the high temperature furnace, and side is incident window, another Side is exit window;Thermal insulation material is filled between the muffle tube and the stove outer covering;Reserved neutron beam passage, and it is described in Cadmium is added in the furnace body material of beamlet passage proximate to absorb stray neutron.
Further, the above-mentioned device in situ for small-angle neutron scattering experiment high temperature and stretching coupling load, it is described Stove outer covering is double-layer structure, is air buffer between two layers.
Further, the above-mentioned device in situ for small-angle neutron scattering experiment high temperature and stretching coupling load, it is described Heater is writing board shape, is symmetrically arranged in the stove outer covering, sample and high-temperature clamp are arranged between two heaters.
Further, the above-mentioned device in situ for small-angle neutron scattering experiment high temperature and stretching coupling load, it is described Middle child window uses sapphire or quartz for material.
Beneficial effects of the present invention are as follows:
1) using the arrangement achieves the small-angle neutron scattering of high temperature and stretching coupling load, experiment is measured in situ.
2) high temperature furnace shape uses cuboid, includes two pieces of flat-plate heating bodies, is symmetrically arranged, intermediate slot milling cloth Sample and high-temperature clamp are set, Proper Design beauty can be made compact in this way, sample position temperature is uniform.
3) neutron beam is reserved along cuboid central axis in high temperature furnace pass through space, and the furnace body near neutron beam path Cadmium is added in material, is absorbed stray neutron, is guaranteed optimal scattered signal signal-to-noise ratio.
4) cylindrical body high temperature furnace two sides use large area sapphire or the quartz child window as in, can guarantee height in this way While warm furnace seals, the decaying to neutron is reduced to the greatest extent.It is also beneficial to obtain biggish scattering angle in this way, collects small angle Scatter high Q data.
5) entire device in situ can be moved horizontally and vertically in the plane of vertical neutron beam, be conveniently adjusted sample center Position is overlapped with neutron beam center.
Detailed description of the invention
Fig. 1 is that the structure of the device in situ tested high temperature for small-angle neutron scattering and stretch coupling load of the invention is shown It is intended to.
Fig. 2 is the structural schematic diagram of the high-temperature clamp of one embodiment of the invention.
Fig. 3 is high temperature furnace schematic diagram of internal structure of the invention.
In above-mentioned attached drawing, 1, crossbeam;2, high-temperature clamp;3, high temperature furnace;4, column;5, extensometer;6, touch screen;7, grating Sensor;8, load cell;9, workbench;10, loading mechanism;11, servo motor;12, speed reducer;13, bottom plate;101, on Pull rod;102, connecting rod;103, collet;104, upper snap ring;105, sample;106, lower snap ring;107, it extends on bar;108, draw under Boom;109, lower pull rod;301, incident window;302, exit window;303, heater;304, seal bellows;305, sample.
Specific embodiment
The present invention is described in detail below with reference to the accompanying drawings and embodiments.
As shown in Figure 1, the present invention provides a kind of for small-angle neutron scattering experiment high temperature and stretches the original of coupling load Position device, including loading frame, high-temperature clamp 2 and high temperature furnace 3;The high temperature furnace 3 and high-temperature clamp 2 are installed in the load On frame;The high-temperature clamp 2 protrudes into the high temperature furnace 3 and carries out stretching operation to sample 105;It is arranged on the high temperature furnace 3 There is middle child window.The loading frame be include the door type structure of double columns 4, and be provided with the touch screen for showing and controlling 6。
As shown in Fig. 2, the high-temperature clamp 2 includes upper connecting rod 101, connecting rod 102, collet 103 and lower pull rod 109;Institute 101 one end of upper connecting rod is stated to be installed in the upper beam 1 of the loading frame, the other end by the connecting rod 102 with it is described Collet 103 connects;Described style one end is connect with the collet 103, and the other end is connect with the lower pull rod 109;The drop-down Bar 109 is drivingly connected with the loading mechanism 10 being mounted on the loading frame to stretch under the driving of the loading mechanism 10 The sample 105;Load cell 8 is additionally provided on the loading mechanism 10.Temperature benefit is provided on the load cell 8 Repay module.The high-temperature clamp 2 further includes high-temperature extensometer 5, and the high-temperature extensometer 5 includes being connected with the sample 105 Upper snap ring 104 and the lower snap ring 106 being connected with the lower pull rod 109;It is connected between the upper snap ring 104 and lower snap ring 106 Extend bar (including above extend bar 107 and under extend bar 108);The lower snap ring 106 can be moved along the bar of extending;It is described to draw Boom end is equipped with grating sensor 7.Be provided on the collet 103 with the screw thread of 105 head fits of cylindrical sample and/ Or the pin hole cooperated with tabular sample 105.
Loading mechanism 10 shown in Fig. 1 includes ball-screw and load actuator;The ball wire and driving mechanism are driven Dynamic connection;The load actuator is mounted on the loading frame and fixes with the screw of ball-screw, the load actuation Rotation-preventing mechanism is installed on device so that load actuator can only be moved up and down without being able to rotate, to realize that adding for load unloads;Institute It states load cell 8 to be mounted in the load actuator, since load cell 8 uses technique for temperature compensation, and be in The lower end of high temperature atmosphere furnace, therefore high-temperature clamp 2 is not required to water cooling, the reliability to work when improving test captain.To protect The concentricity of confirmatory test machine is respectively equipped with cating nipple in testing machine up and down, improves the accuracy of test result.The present embodiment In, crossbeam 1, workbench 9, load actuator etc. use cast structure, effectively increase the strength and stiffness of system.On crossbeam 1 Fixed upper connecting rod 101, fixed loading mechanism 10 and driving mechanism between workbench 9 and bottom plate 13.Driving mechanism include by Servo motor 11 and turbine worm reducer 12.Servo motor 11 is defeated by synchronous tooth profile band connection turbine worm reducer 12 Enter end, 12 output end of speed reducer is connected with high precision ball lead screw.Deformation measurement uses high-precision digital raster technology, precision Height, it is noiseless, it prevents from deforming drifting problem when creep test is long, there is re-adjustments and accumulation function;Using band temperature-compensating The load sensor of function waves problem so as to avoid because of force value caused by temperature change.
Referring to Fig. 3, in the present embodiment, the high temperature furnace 3 includes stove outer covering, bell, muffle tube, ceramic end seat, magnetic board With heater 303 (part-structure is not shown);High temperature furnace shape is rectangular parallelepiped structure, high 35cm.Outside the bell and the furnace Shell is relatively fixed, and muffle tube is supported in the end seat being installed on the bell;The heater 303 is mounted on the muffle tube Groove in;The electrode plate is installed on the stove outer covering;Middle child window is located at the two sides of the high temperature furnace, and side is incidence Window 301, the other side are exit window 302, the use of sapphire are material.Sapphire diameter 10cm, thickness 0.2cm, it is ensured that small Test the acquisition of high Q data (angle of scattering reaches 200) in angle.Superfine ceramic cotton is filled between the muffle tube and the stove outer covering Thermal insulation material;Reserved neutron beam passage, and cadmium is added in the furnace body material of the neutron beam passage proximate to absorb stray neutron. The stove outer covering is double-layer structure, is air buffer between two layers, reduces furnace table temperature.The heater is writing board shape, left The right side is symmetrically arranged in the stove outer covering, and sample 305 and high-temperature clamp are arranged between two heaters.To guarantee the effective work of burner hearth It is uniform to make temperature in area, heater uses two and half bareing electric-heating-wire-heatings, and every section of heater strip respectively by having microcomputer all the way Change the temperature controller control of digital regulated instrument, 0.1 grade of precision, test temperature and setup parameter can digital displays;It is protected with upper and lower limit Function;Power cell shifts to triggering technique, works long hours reliable, temperature-controlled precision is high.Maximum temperature reaches 800 DEG C, temperature control essence ± 2 DEG C of degree detects specimen temperature as temperature sensor using thermocouple, and the hot end of thermocouple is bundled with asbestos cord is close to sample Working surface, cold end are drawn furnace and are placed outside in zero compensation device, and sample position temperature uniformity size is greater than 10mm* 10mm*5mm.The middle child window uses sapphire for material.Stove outer covering uses high-quality stainless steel making.Take into account relative motion The considerations of with sealing, seal bellows 304 is provided between high-temperature clamp 2 and high temperature furnace 3.
In use, the device in situ of the present embodiment is placed on small-angle scattering spectrometer sample stage position, neutron beam is from entrance window Mouth, which enters, to be beaten on sample, and the neutron beam after sample scattering enters small-angle scattering spectrometer detector cavity from exit window.Specifically Steps are as follows:
(1) standard size sample is fixed on fixture;
(2) for device in situ along X, Y-direction is mobile, is overlapped sample center with neutron beam center, determines X, the seat of Y-direction Mark;
(3) vacuum pump and cooling water recirculation system are opened, when vacuum degree reaches 0.1Pa, the load of setting sample application Force value and temperature value;
(4) after loading force and temperature reach target value, neutron beam lock is opened, acquires small-angle neutron scattering data;
(5) after data acquisition, neutron beam lock is closed, vacuum system is closed;
(6) when vacuum meter registration reaches atmospheric pressure, high temperature furnace is opened, sample is removed from fixture;
(7) surface radioactive pollution detector is used, sample Activation after neutron exposure is measured, if dosage is exceeded, It is put into lead screen Special sample box;
(8) first step is repeated, next sample measurement is started.
For bar shaped and cylindrical sample, using different fixtures, measuring process is similar.
The present invention realizes in-situ high temperature and stretches coupling load small-angle neutron scattering test method.Small-angle neutron scattering is surveyed Analytical technology extension is tried, it can be with the nanostructure of sample interior under researching high-temperature and stretching condition.Specific implementation case can meet Copper-rich precipitate small-angle neutron scattering test under the nearly working condition of stainless steel valve rod, relevant parameter are set as 300 DEG C of temperature, draw Power 1OKN.Other types metal or non-metal solid sample, such as nickel base superalloy test method are consistent, according to variety classes The neutron cross section of material optimizes thickness of sample.
Obviously, various changes and modifications can be made to the invention without departing from essence of the invention by those skilled in the art Mind and range.If in this way, belonging to the model of the claims in the present invention and its equivalent technology to these modifications and changes of the present invention Within enclosing, then the present invention is also intended to include these modifications and variations.

Claims (10)

1. a kind of device in situ for small-angle neutron scattering experiment high temperature and stretching coupling load, it is characterised in that: including adding Carry frame, high-temperature clamp (2) and high temperature furnace (3);The high temperature furnace (3) and high-temperature clamp (2) are installed in the loading frame On;The high-temperature clamp (2), which is protruded into the high temperature furnace (3), carries out stretching operation to sample (105);On the high temperature furnace (3) It is provided with middle child window.
2. the device in situ for small-angle neutron scattering experiment high temperature and stretching coupling load as described in claim 1, special Sign is: the high-temperature clamp (2) includes upper connecting rod (101), connecting rod (102), collet (103) and lower pull rod (109);It is described Upper connecting rod (101) one end is installed on the loading frame, and the other end passes through the connecting rod (102) and the collet (103) Connection;Described style one end is connect with the collet (103), and the other end is connect with the lower pull rod (109);The lower pull rod (109) it is drivingly connected with loading mechanism (10) to stretch the sample (105) under the driving of the loading mechanism (10).
3. the device in situ for small-angle neutron scattering experiment high temperature and stretching coupling load as claimed in claim 2, special Sign is: the loading mechanism (10) includes ball-screw and load actuator;The ball wire and driving mechanism are drivingly connected; The load actuator is mounted on the loading frame and fixes with the screw of ball-screw, installs in the load actuator Rotation-preventing mechanism is so that load actuator can only be moved up and down without being able to rotate;Load cell is installed in the load actuator (8)。
4. the device in situ for small-angle neutron scattering experiment high temperature and stretching coupling load as claimed in claim 3, special Sign is: being provided with temperature compensation module on the load cell (8).
5. the device in situ for small-angle neutron scattering experiment high temperature and stretching coupling load as claimed in claim 2, special Sign is: the high-temperature clamp (2) further includes high-temperature extensometer (5), and the high-temperature extensometer (5) includes and the sample (105) connected upper snap ring (104) and the lower snap ring (106) being connected with the lower pull rod;The upper snap ring (104) and lower snap ring (106) bar of extending is connected between;The lower snap ring (106) can move along the bar of extending;The bar end installation of extending There are grating sensor (7).
6. the device in situ for small-angle neutron scattering experiment high temperature and stretching coupling load as claimed in claim 2, special Sign is: be provided on the collet (103) with the screw thread of cylindrical sample head fits and/or with tabular sample cooperation Pin hole.
7. the device in situ for small-angle neutron scattering experiment high temperature and stretching coupling load as described in claim 1, special Sign is: the high temperature furnace (3) includes stove outer covering, bell, muffle tube, ceramic end seat, magnetic board and heater;The bell with The stove outer covering is relatively fixed, and muffle tube is supported in the end seat being installed on the bell;The heater is mounted on described In the groove of muffle tube;The electrode plate is installed on the stove outer covering;Middle child window is located at the two sides of the high temperature furnace (3), Side is incident window, and the other side is exit window;Thermal insulation material is filled between the muffle tube and the stove outer covering;It is reserved Neutron beam passage, and cadmium is added in the furnace body material of the neutron beam passage proximate to absorb stray neutron.
8. the device in situ for small-angle neutron scattering experiment high temperature and stretching coupling load as claimed in claim 7, special Sign is: the stove outer covering is double-layer structure, is air buffer between two layers.
9. the device in situ for small-angle neutron scattering experiment high temperature and stretching coupling load as claimed in claim 7, special Sign is: the heater is writing board shape, is symmetrically arranged in the stove outer covering, arranges sample between two heaters (105) and high-temperature clamp (2).
10. the dress in situ for small-angle neutron scattering experiment high temperature and stretching coupling load as described in claim 1-9 is any It sets, it is characterised in that: the middle child window uses sapphire or quartz for material.
CN201811559897.6A 2018-12-19 2018-12-19 A kind of device in situ for small-angle neutron scattering experiment high temperature and stretching coupling load Pending CN109556970A (en)

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CN110044692A (en) * 2019-05-22 2019-07-23 中国民航大学 A kind of high temperature tension test fixture for fragile material flat test piece
CN110333134A (en) * 2019-07-04 2019-10-15 西北工业大学 Uniaxial stretching device and experimental method associated with a kind of and neutron scattering
CN110779816A (en) * 2019-11-12 2020-02-11 磐翼信息科技(上海)有限公司 Detection device for detecting flexible pipeline
CN111141619A (en) * 2019-12-24 2020-05-12 长春因赛图精密仪器设备有限公司 In-situ tester for mechanical properties of materials under high and low temperature alternation
CN111665273A (en) * 2020-06-17 2020-09-15 中国科学院长春应用化学研究所 High-low temperature environment box for combined use of testing machine and X-ray light source characterization
CN114062404A (en) * 2021-11-16 2022-02-18 中国工程物理研究院核物理与化学研究所 Multi-connected in-situ cold and hot table device for neutron scattering spectrometer
CN114137006A (en) * 2021-11-04 2022-03-04 散裂中子源科学中心 High-temperature furnace for small-angle scattering experiment
US11460386B2 (en) * 2019-03-21 2022-10-04 King Abdulaziz University Heating apparatus for material testing machine
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