CN109946324B - Synchrotron radiation in-situ imaging experiment solidification device - Google Patents
Synchrotron radiation in-situ imaging experiment solidification device Download PDFInfo
- Publication number
- CN109946324B CN109946324B CN201910248594.0A CN201910248594A CN109946324B CN 109946324 B CN109946324 B CN 109946324B CN 201910248594 A CN201910248594 A CN 201910248594A CN 109946324 B CN109946324 B CN 109946324B
- Authority
- CN
- China
- Prior art keywords
- sample
- temperature
- experiment
- light
- experiment cavity
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Abstract
The invention discloses a synchrotron radiation in-situ imaging experiment solidification device, which comprises a heating furnace, wherein the side wall of the heating furnace is provided with a light inlet and a light outlet, an experiment cavity is arranged in the heating furnace, the light inlet and the light outlet are positioned on the same straight line and are vertically communicated with the experiment cavity, and light-transmitting sealing pieces are arranged at the light inlet and the light outlet; a temperature adjusting component, a temperature detecting component and a sample clamping and adjusting component are arranged in the experiment cavity; the sample is arranged on the sample clamping and adjusting component, the temperature detecting component detects the temperature of the sample and transmits the temperature to the temperature control upper computer, the temperature control upper computer displays the temperature and controls the temperature adjusting component to adjust the temperature of the sample, and the bottom of the experiment cavity is provided with an air inlet and an air outlet. The method greatly improves the success rate of the evolution process of the alloy surrounding structure observed in situ by synchrotron radiation.
Description
Technical Field
The invention belongs to the technical field of experimental teaching equipment, and particularly relates to a synchrotron radiation in-situ imaging experimental solidification device.
Background
The solidification microstructure is a bridge for connecting alloy components and performance, accurately recognizes and masters the formation mechanism, leading factors and control ways of the alloy solidification microstructure, is beneficial to accurately controlling and designing the material microstructure so as to improve the comprehensive performance of the material, and has important engineering guidance significance for improving the alloy performance. Because the opacity, the micro-nano property and the solidification of the alloy solidification structure often occur in a high-temperature environment, the traditional characterization technology cannot dynamically, completely and real-timely observe the whole solidification process. But the advent of synchrotron radiation in-situ imaging technology makes it possible to observe the dynamic evolution of metal solidification in situ. However, the synchrotron radiation in-situ observation process relates to real-time melting and solidification of the alloy, and the observation of the evolution of the alloy surrounding structure is seriously influenced by the problems of oxidation of a sample in the heating process, inaccurate temperature control and the like caused by insufficient sealing in most experimental processes.
Disclosure of Invention
Aiming at the defects described in the prior art, the invention provides the synchrotron radiation in-situ imaging experiment solidification device which has higher safety, more accurate temperature control, better sealing effect and better synchrotron radiation observation effect compared with the prior art.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
a synchrotron radiation in-situ imaging experiment solidification device comprises a heating furnace, wherein a light inlet and a light outlet are formed in the side wall of the heating furnace, an experiment cavity is arranged in the heating furnace, the light inlet and the light outlet are positioned on the same straight line and are vertically communicated with the experiment cavity, and light-transmitting sealing pieces are arranged at the light inlet and the light outlet; a temperature adjusting component, a temperature detecting component and a sample clamping and adjusting component are arranged in the experiment cavity; the sample is arranged on the sample clamping and adjusting component, the temperature detecting component detects the temperature of the sample and transmits the temperature to the temperature control upper computer, the temperature control upper computer displays the temperature and controls the temperature adjusting component to adjust the temperature of the sample, and the bottom of the experiment cavity is provided with an air inlet and an air outlet.
In order to prevent the temperature of the furnace body from diffusing outwards, the inner wall of the heating furnace is provided with a heat-resistant layer, the heat-resistant layer prevents the temperature in the experimental cavity from overflowing, and high-temperature scalding caused by touch and damage of other objects to the heating furnace can be reduced.
Specifically, the temperature regulating assembly comprises a water cooling pipeline and a U-shaped heating wire; the water cooling pipeline and the U-shaped heating wire ring are arranged on the inner wall of the experimental cavity, the water inlet of the water cooling pipeline is connected with the water inlet pipe, the water outlet of the water cooling pipeline is connected with the water outlet pipe, and the water inlet pipe and the water outlet pipe are arranged at the bottom of the experimental cavity and are exposed out of the bottom of the experimental cavity. The water inlet pipe, the water cooling pipeline and the water outlet pipe are matched with each other to realize the cooling of the experimental cavity; the U-shaped heating wire is used for heating the experiment cavity and melting the sample, and the U-shaped heating wire is also used for avoiding influencing X-rays.
The sample clamping and adjusting assembly comprises a sample table, a sample clamp, a lifting rod and a lifting table; the sample bench is equipped with the sample and presss from both sides, and the sample passes through the sample and presss from both sides vertical ann at the sample bench, and the sample bench is connected with the lifter, and the lifter is connected with the elevating platform after wearing out the experiment chamber downwards. The up and down micro-motion of the lifting platform changes the position of the sample in the experimental cavity, namely changes the position of the X-ray penetrating through the sample, so that the observation result is optimal.
The temperature detection assembly comprises a thermocouple, wherein the thermocouple is attached to a sample and can be uniformly distributed on the circumference of the sample, and the detection accuracy is improved.
And in order to facilitate the sample replacement, the upper part of the heating furnace is hinged with a sealing cover, and the sealing cover seals the upper opening of the experimental cavity.
In order to stabilize the heating furnace, the furnace body of the heating furnace is connected with the support frame.
A use method of a synchrotron radiation in-situ imaging experiment solidification device comprises the following steps:
s1, opening a sealing cover, clamping the sample on a sample table by using a sample clamp, uniformly attaching thermocouples to the sample, and connecting the thermocouples with a temperature control upper computer;
s2, closing the sealing cover and vacuumizing the experiment cavity;
s3, injecting inert gas into the experiment cavity from the gas inlet;
s4, adjusting the height of the sample stage through the lifting stage, and emitting X-rays into the experimental cavity from the light inlet, penetrating the sample and emitting from the light outlet;
and S5, heating the sample by heating the U-shaped heating wire, introducing cold water through a water cooling pipeline for circulating cooling, and measuring the temperature of the sample by connecting a thermocouple and a temperature control upper computer.
Compared with the prior art, the invention has the remarkable advantages that: the heat-resistant layer is arranged to realize heat insulation, so that high-temperature scalding and damage of other objects to the heat-resistant heat-insulating glass lamp can be reduced for operators; secondly, an internal heating wire, a thermocouple and a circulating water cooling system are arranged in the experiment cavity, so that the accurate control of the melting and solidification temperatures of the sample is facilitated; the temperature gradient of the sample is controlled by controlling the water inlet and outlet amount and the temperature rise and fall of the U-shaped heating wire; thirdly, the invention is provided with an air inlet pipe and an air outlet pipe, and inert gas can be filled in the gas inlet pipe and the air outlet pipe, so that the sample is prevented from being oxidized in the heating process. The method greatly improves the success rate of the evolution process of the alloy surrounding structure observed in situ by synchrotron radiation.
Drawings
FIG. 1 is a schematic structural diagram of the present invention.
Detailed Description
A synchrotron radiation in-situ imaging experiment solidification device is shown in figure 1 and comprises a heating furnace 1, and in order to stabilize the heating furnace, a furnace body of the heating furnace 1 is connected with a support frame 19.
The side wall of the heating furnace 1 is provided with a light inlet 2 and a light outlet 3, an experiment cavity 4 is arranged in the heating furnace 1, the light inlet 2 and the light outlet 3 are positioned on the same straight line and are vertically communicated with the experiment cavity 4, and light-transmitting sealing parts are arranged at the light inlet 2 and the light outlet 3; a temperature adjusting component, a temperature detecting component and a sample clamping and adjusting component are arranged in the experiment cavity 4; the sample is established on sample centre gripping adjusting part, and in temperature detecting component detected the temperature of sample and transmitted the control by temperature change host computer 20, the control by temperature change host computer shows the temperature and controls the temperature that the temperature adjusting component adjusted the sample, temperature detecting component, including the thermocouple, the thermocouple is attached on the sample, can improve the detection accuracy in sample circumference evenly distributed. The bottom of the experiment cavity 4 is provided with an air inlet 17 and an air outlet 18, and inert gas enters the experiment cavity from the air inlet to prevent the sample from being oxidized in the experiment process.
In order to prevent the temperature of the furnace body from diffusing outwards, the inner wall of the heating furnace 1 is provided with the heat-resistant layer 16, the heat-resistant layer 16 prevents the temperature in the experimental cavity from overflowing, and high-temperature scalding caused by touch and damage of other objects to the heating furnace can be reduced.
Specifically, the temperature adjusting assembly comprises a water cooling pipeline 5 and a U-shaped heating wire 6; water-cooling pipeline 5 and U-shaped heater strip 6 encircle and establish 4 inner walls in laboratory cavity, and the water inlet and the inlet tube 7 of water-cooling pipeline 5 are connected, and the delivery port and the play water piping 8 of water-cooling pipeline 5 are connected, and inlet tube 7 and play water piping 8 establish in the bottom in laboratory cavity 4 and expose the bottom in laboratory cavity 4.
In this embodiment, the water-cooling pipeline 5 includes a left pipeline and a right pipeline, a connection port i of the left pipeline is connected with a connection port ii of the right pipeline through a connection pipe, and water pipes on the left and right sides form a circulating water-cooling system capable of circulating; the water inlet of the left pipeline is connected with a water inlet pipe 7, and the water outlet of the right pipeline is connected with a water outlet pipe 8; the water inlet pipe, the water cooling pipeline and the water outlet pipe are matched with each other to cool the experiment cavity. The U-shaped heating wire is used for heating the experiment cavity and melting the sample, and is also arranged in a U shape so as to avoid influencing X-rays.
The sample clamping and adjusting assembly comprises a sample table 11, a sample clamp 12, a lifting rod 14 and a lifting table 15; the sample table 11 is provided with a sample clamp 12, a sample 13 is vertically arranged on the sample table 11 through the sample clamp 12, the sample table 11 is connected with a lifting rod 14, and the lifting rod 14 penetrates out of the experiment cavity 4 downwards and then is connected with a lifting table 15. The up and down micro-motion of the lifting platform changes the position of the sample in the experimental cavity, namely changes the position of the X-ray penetrating through the sample, so that the observation result is optimal.
In addition, in order to facilitate the replacement of the sample, the upper part of the heating furnace 1 is hinged with a sealing cover, and the sealing cover seals the upper opening of the experiment cavity 4.
Example 2: a use method of a synchrotron radiation in-situ imaging experiment solidification device comprises the following steps:
s1, opening a sealing cover, clamping the sample 13 on the sample table 11 by using the sample clamp 12, uniformly attaching thermocouples on the sample 13, and connecting the thermocouples with the temperature control upper computer 20;
s2, closing the sealing cover and vacuumizing the experiment cavity 4;
s3, injecting inert gas into the experiment cavity 4 from the gas inlet 17;
s4, adjusting the height of the sample stage through the lifting stage, and emitting X-rays into the experimental cavity 4 from the light inlet 2, penetrating the sample and emitting from the light outlet 3;
and S5, heating the sample 13 by heating the U-shaped heating wire 6, introducing cold water through the water cooling pipeline 5 for circulating cooling, and measuring the temperature of the sample by connecting the thermocouple 10 with the temperature control upper computer 20.
Claims (3)
1. The utility model provides a synchrotron radiation in situ imaging experiment solidification equipment, includes heating furnace (1), its characterized in that: the side wall of the heating furnace (1) is provided with a light inlet (2) and a light outlet (3), an experiment cavity (4) is arranged in the heating furnace (1), the light inlet (2) and the light outlet (3) are positioned on the same straight line and are vertically communicated with the experiment cavity (4), and light-transmitting sealing parts are arranged at the light inlet (2) and the light outlet (3); a temperature adjusting component, a temperature detecting component and a sample clamping and adjusting component are arranged in the experiment cavity (4); the sample is arranged on the sample clamping and adjusting component, the temperature detecting component detects the temperature of the sample and transmits the temperature to the temperature control upper computer (20), the temperature control upper computer displays the temperature and controls the temperature adjusting component to adjust the temperature of the sample, and the bottom of the experiment cavity (4) is provided with an air inlet (17) and an air outlet (18);
a heat-resistant layer (16) is arranged on the inner wall of the heating furnace (1);
the temperature adjusting component comprises a water cooling pipeline (5) and a U-shaped heating wire (6); the water cooling pipeline (5) and the U-shaped heating wire (6) are annularly arranged on the inner wall of the experiment cavity (4), a water inlet of the water cooling pipeline (5) is connected with a water inlet pipe (7), a water outlet of the water cooling pipeline (5) is connected with a water outlet pipe (8), and the water inlet pipe (7) and the water outlet pipe (8) are arranged at the bottom of the experiment cavity (4) and expose out of the bottom of the experiment cavity (4);
the sample clamping and adjusting assembly comprises a sample table (11), a sample clamp (12), a lifting rod (14) and a lifting table (15); a sample clamp (12) is arranged on the sample table (11), a sample (13) is vertically arranged on the sample table (11) through the sample clamp (12), the sample table (11) is connected with a lifting rod (14), and the lifting rod (14) penetrates out of the experiment cavity (4) downwards and then is connected with a lifting table (15);
the temperature detection assembly comprises a thermocouple (10), and the thermocouple (10) is attached to a sample;
the using method comprises the following steps:
s1, opening a sealing cover, clamping a sample (13) on a sample table (11) by using a sample clamp (12), uniformly attaching a thermocouple (10) on the sample (13), and connecting the thermocouple (10) with a temperature control upper computer (20);
s2, closing the sealing cover and vacuumizing the experiment cavity (4);
s3, injecting inert gas into the experiment cavity (4) from the gas inlet (17);
s4, adjusting the height of the sample stage through the lifting stage (15), and emitting X-rays into the experimental cavity (4) from the light inlet (2), penetrating through the sample and emitting from the light outlet (3);
and S5, heating the sample (13) by heating the U-shaped heating wire (6), introducing cold water through the water cooling pipeline (5) for circulation to cool, and measuring the temperature of the sample by connecting the thermocouple (10) with the temperature control upper computer (20).
2. The synchrotron radiation in-situ imaging experiment solidification apparatus of claim 1, wherein: the upper part of the heating furnace (1) is hinged with a sealing cover which seals an opening at the upper part of the experiment cavity (4).
3. The synchrotron radiation in-situ imaging experiment solidification apparatus of claim 1, wherein: the furnace body of the heating furnace (1) is connected with the supporting frame (19).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910248594.0A CN109946324B (en) | 2019-03-29 | 2019-03-29 | Synchrotron radiation in-situ imaging experiment solidification device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910248594.0A CN109946324B (en) | 2019-03-29 | 2019-03-29 | Synchrotron radiation in-situ imaging experiment solidification device |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109946324A CN109946324A (en) | 2019-06-28 |
| CN109946324B true CN109946324B (en) | 2020-04-17 |
Family
ID=67013059
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910248594.0A Active CN109946324B (en) | 2019-03-29 | 2019-03-29 | Synchrotron radiation in-situ imaging experiment solidification device |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109946324B (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112229866A (en) * | 2020-10-09 | 2021-01-15 | 大连理工大学 | Peripheral system suitable for in-situ observation of metal solidification under synchrotron radiation |
| CN112710681B (en) * | 2020-12-21 | 2022-04-15 | 中南大学 | Experimental device for solidification behavior is observed to normal position |
| CN112710680B (en) * | 2020-12-21 | 2022-04-15 | 中南大学 | Experimental method for in-situ observation of solidification behavior |
| CN114047207B (en) * | 2021-10-26 | 2023-12-12 | 中山大学 | Device for in-situ research of laser cladding process |
| CN114534819A (en) * | 2022-03-01 | 2022-05-27 | 合肥工业大学 | Atmosphere-controllable heat treatment equipment |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH10236898A (en) * | 1997-02-25 | 1998-09-08 | Ritsumeikan | Diamond synthesizing method and device therefor |
| CN101042319A (en) * | 2007-04-19 | 2007-09-26 | 华东理工大学 | In-situ measurement system of material micro-creep |
| CN102621011A (en) * | 2012-03-28 | 2012-08-01 | 天津大学 | Subminiature minimal invasion high-temperature creep fatigue testing machine and application thereof |
| CN105136824A (en) * | 2015-07-24 | 2015-12-09 | 大连理工大学 | Device and test method of alloy solidification synchronous radiation imaging static magnetic field composite direct current effect |
| CN105568018A (en) * | 2015-07-22 | 2016-05-11 | 重庆电子工程职业学院 | Directional magnesium alloy solidification device and method for directionally solidifying magnesium alloy through directional magnesium alloy solidification device |
-
2019
- 2019-03-29 CN CN201910248594.0A patent/CN109946324B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH10236898A (en) * | 1997-02-25 | 1998-09-08 | Ritsumeikan | Diamond synthesizing method and device therefor |
| CN101042319A (en) * | 2007-04-19 | 2007-09-26 | 华东理工大学 | In-situ measurement system of material micro-creep |
| CN102621011A (en) * | 2012-03-28 | 2012-08-01 | 天津大学 | Subminiature minimal invasion high-temperature creep fatigue testing machine and application thereof |
| CN105568018A (en) * | 2015-07-22 | 2016-05-11 | 重庆电子工程职业学院 | Directional magnesium alloy solidification device and method for directionally solidifying magnesium alloy through directional magnesium alloy solidification device |
| CN105136824A (en) * | 2015-07-24 | 2015-12-09 | 大连理工大学 | Device and test method of alloy solidification synchronous radiation imaging static magnetic field composite direct current effect |
Non-Patent Citations (1)
| Title |
|---|
| 具有独立温控单元的模具温控凝固成形装置的研制;游东东等;《机械工程学报》;20071031;第43卷(第10期);第187-190页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN109946324A (en) | 2019-06-28 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109946324B (en) | Synchrotron radiation in-situ imaging experiment solidification device | |
| CN105973929A (en) | Non-destructive testing method for detecting thermal contact resistance inside parts by infrared camera | |
| CN109211438A (en) | A kind of device and method of home position observation continuous casting covering slag phase transition process heat flow density | |
| TW201801821A (en) | Nickel-titanium alloy fabrication method by using high vacuum crucible-free floating melting process in which a titanium material is heated in a floating condition with an induction coil and a nickel material is added into the titanium material when the titanium material is in a partly melted condition | |
| CN105738348B (en) | High temperature resistant immersion cell for LIBS system | |
| CN203365358U (en) | Experimental apparatus for adhering slag on blast furnace copper cooling stave | |
| CN104133505A (en) | Temperature control device for refining metal solidification structure by use of pulse current | |
| CN110082372A (en) | A kind of Portable synchronous radiation regimes in situ imaging experiment coagulation system | |
| CN206832039U (en) | Vaccum sensitive stove with liftable drop-bottom | |
| CN209911259U (en) | Portable synchrotron radiation state in-situ imaging experiment solidification device | |
| CN210322543U (en) | Electromagnetic heating high-pressure digestion instrument | |
| CN211503694U (en) | Simulation test furnace for detecting real-time temperature in service process of steel ladle ventilating plug | |
| CN108693210B (en) | Equipment and method for testing relation between cooling rate of cooling wall and thermal shock | |
| CN101871821B (en) | Electrolyte primary crystal temperature measuring method | |
| CN208019579U (en) | A kind of vacuum brazing equipment | |
| CN215524163U (en) | Induction heating furnace for glove box | |
| CN107020358B (en) | Device for simulating solidification structure and unsteady state heat flow of casting blank surface layer in crystallizer | |
| CN110926619A (en) | Continuous temperature measurement method for temperature of molten steel in steel ladle | |
| CN105987602B (en) | The mechanism test method of multipurpose tube furnace | |
| CN106378526B (en) | A kind of experimental provision can be used for high heating rate Diffusion Welding | |
| CN113008033B (en) | High-temperature reaction tube furnace capable of accurately controlling temperature and atmosphere and rapidly quenching sample | |
| CN219935624U (en) | Material high temperature corrosion performance testing device | |
| CN217277615U (en) | Integrated thermal shock resistance testing device | |
| CN204065872U (en) | A kind of temperature control equipment for pulse current thinning metal solidification texture | |
| CN113030420B (en) | Measuring device and measuring method for metal saturated vapor pressure |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |