CN117092157A - High-vacuum in-situ observation device and use method thereof - Google Patents
High-vacuum in-situ observation device and use method thereof Download PDFInfo
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- CN117092157A CN117092157A CN202311072504.XA CN202311072504A CN117092157A CN 117092157 A CN117092157 A CN 117092157A CN 202311072504 A CN202311072504 A CN 202311072504A CN 117092157 A CN117092157 A CN 117092157A
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- 238000000034 method Methods 0.000 title claims abstract description 34
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 30
- 238000010438 heat treatment Methods 0.000 claims abstract description 117
- 238000012360 testing method Methods 0.000 claims abstract description 27
- 238000012544 monitoring process Methods 0.000 claims abstract description 26
- 238000002844 melting Methods 0.000 claims abstract description 23
- 230000008018 melting Effects 0.000 claims abstract description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 230000008569 process Effects 0.000 claims abstract description 19
- 238000001816 cooling Methods 0.000 claims abstract description 9
- 150000001875 compounds Chemical class 0.000 claims description 18
- 238000005086 pumping Methods 0.000 claims description 15
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 11
- 229910052802 copper Inorganic materials 0.000 claims description 11
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- 238000004891 communication Methods 0.000 claims description 9
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- 239000000956 alloy Substances 0.000 abstract description 6
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- 229910017941 Ag—Li Inorganic materials 0.000 description 3
- 238000009529 body temperature measurement Methods 0.000 description 3
- 239000001989 lithium alloy Substances 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 2
- 230000003028 elevating effect Effects 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 238000010309 melting process Methods 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 229910052715 tantalum Inorganic materials 0.000 description 2
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 2
- 101100448444 Caenorhabditis elegans gsp-3 gene Proteins 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000004992 fission Effects 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
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- 230000004048 modification Effects 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000001304 sample melting Methods 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
- F27D1/00—Casings; Linings; Walls; Roofs
- F27D1/18—Door frames; Doors, lids, removable covers
- F27D1/1808—Removable covers
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01K—MEASURING TEMPERATURE; MEASURING QUANTITY OF HEAT; THERMALLY-SENSITIVE ELEMENTS NOT OTHERWISE PROVIDED FOR
- G01K7/00—Measuring temperature based on the use of electric or magnetic elements directly sensitive to heat ; Power supply therefor, e.g. using thermoelectric elements
- G01K7/02—Measuring temperature based on the use of electric or magnetic elements directly sensitive to heat ; Power supply therefor, e.g. using thermoelectric elements using thermoelectric elements, e.g. thermocouples
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/84—Systems specially adapted for particular applications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/02—Investigating or analyzing materials by the use of thermal means by investigating changes of state or changes of phase; by investigating sintering
- G01N25/04—Investigating or analyzing materials by the use of thermal means by investigating changes of state or changes of phase; by investigating sintering of melting point; of freezing point; of softening point
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/84—Systems specially adapted for particular applications
- G01N2021/8411—Application to online plant, process monitoring
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Abstract
The application discloses a high-vacuum in-situ observation device and a use method thereof, and relates to the technical field of irradiation temperature test equipment, wherein the high-vacuum in-situ observation device comprises a heating furnace body system, a sample test platform, a vacuum acquisition system, a control system, a water cooling system and an observation system; the sample testing platform is arranged in the heating furnace body system; the control system is used for realizing the automatic operation of the vacuumizing, heating and observing processes. The irradiation temperature monitoring device can reach 1000 ℃ in the use process, and the vacuum degree can reach 5.0 multiplied by 10 within 1 hour ‑5 Pa (cold state, after baking), heating according to a set heating curve, monitoring sample state in real time by an observation system, and realizing vacuumizing, heating and control by a control systemThe automatic operation of the observation process, the monitoring condition is easy to control, the monitoring result is more accurate, the obtained melting point temperature is more accurate, and the method is suitable for real-time observation of melting behaviors of various alloy materials and accurate measurement of the melting point.
Description
Technical Field
The application relates to the technical field of material melting point monitoring equipment, in particular to a high-vacuum in-situ observation device and a use method thereof.
Background
In a reactor system, the irradiation temperature is one of the most critical parameters of neutron irradiation research, and has a decisive influence on evaluating the performance of irradiated materials. The control and calibration of the irradiation temperature is difficult due to the special environment of the reactor, especially for high-dose long-time irradiation experiments. When a fuel mesopore (e.g., about 9mm in inside diameter) of a fission reactor is used to mount a sample for neutron irradiation, a method of thermocouple temperature measurement is extremely limited and is difficult to implement. At present, a temperature field numerical model is usually established by adopting a finite element analysis mode, but the result obtained by the method still has great limitation, and large temperature errors can occur at different positions of environmental conditions. In addition, a method for measuring the temperature by adopting a fuse wire material is also adopted, the method is a technology which is lower in cost and can be used for judging the irradiation temperature in the reactor without repeated investigation, a series of alloy fuse wires with different proportions and components which can effectively summarize the whole irradiation temperature area are required to be prepared, an identification method for reversely deducing the experience temperature according to the observation phenomenon is formed, and a high-vacuum in-situ observation device is required to be used for out-of-reactor verification of the accurate melting point of the alloy fuse wires.
Patent CN207439150U discloses a high-temperature vacuum furnace, including furnace body, vacuum pump and heating chamber, the heating chamber is equipped with heating device, the heating chamber passes through the crossbearer to be connected with the support frame, the support frame includes the frame, base and vertical frame, the frame includes first framework and second framework, first framework and base fixed connection, the second framework rotates with first framework to be connected, be equipped with circulating water pipe in the first framework, the base is equipped with elevating gear, elevating gear includes the knob, the lead screw, the folding leg, supporting bench and kerve, the folding leg includes the lead screw nut, preceding supporting legs and back supporting legs, supporting bench and furnace body fixed connection, the one end and the knob fixed connection of lead screw, the other end and the lead screw nut of lead screw are connected, preceding supporting legs rotates with the kerve to be connected, back supporting legs and kerve sliding connection; the vertical frame comprises a first vertical frame and a second vertical frame, and the second vertical frame is connected with the first vertical frame in a sliding way.
The patent proposes a high-temperature vacuum furnace which is convenient to move, high in heat dissipation efficiency and adjustable in height, but cannot realize on-line monitoring and real-time recording, and the process condition in the monitoring process is controlled inaccurately, so that the monitoring result is inaccurate. Therefore, the existing vacuum furnace has the problems that the appearance change of a sample in the furnace body cannot be monitored under the high-temperature high-vacuum condition, the monitoring condition is inconvenient to control, and the melting point of the sample cannot be accurately measured.
Disclosure of Invention
The application aims to provide a high-vacuum in-situ observation device and a use method thereof, which solve the problems that the prior vacuum furnace cannot monitor the morphology change of a sample in the furnace body under the high-temperature and high-vacuum condition, the monitoring condition is inconvenient to control and the melting point of the sample cannot be accurately measured.
The application is realized by the following technical scheme:
in a first aspect, the application provides a high vacuum in-situ observation device, which comprises a heating furnace body system, a sample testing platform, a vacuum acquisition system, a control system, a water cooling system and an observation system; the sample testing platform is arranged in the heating furnace body system; the control system is used for realizing automatic operation of vacuumizing, heating and observing processes.
The testing temperature of the high vacuum in-situ observation device in the use process can reach 1000 ℃, and the vacuum degree can reach 5.0 multiplied by 10 within 1 hour -5 Pa (cold state, after baking), heating according to a set heating curve, monitoring the state of a sample in real time through an observation system, and realizing the automatic vacuumizing, heating and observation processes through a control systemThe operation is easy to control the monitoring conditions, the monitoring result is more accurate, the obtained melting point temperature is more accurate, and the method is suitable for real-time observation of melting behaviors of various alloy materials and accurate measurement of melting points.
Further, the heating furnace body system comprises a heating furnace body connected to the frame, a heating cylinder is connected inside the heating furnace body, the top of the heating furnace body is connected with a furnace cover through a lifting structure, and the furnace bottom of the heating furnace body is connected with a temperature measuring structure for measuring the temperature of samples inside the heating furnace body and on a sample testing platform; and the heating furnace body is connected with a bleed valve.
The temperature measuring structure is arranged, so that the temperature inside the heating furnace body and the temperature change of the sample in the melting process of the sample can be monitored in real time, and the temperature inside the heating furnace body can be controlled conveniently; and the air release valve is arranged on the heating furnace body, so that the temperature and the air release are conveniently and quickly reduced, and the inside of the heating furnace body can quickly reach the atmospheric pressure state.
The outside of the heating cylinder can be provided with a plurality of heat insulation layers, for example, 5 layers of stainless steel are adopted, so that the uniformity of the temperature in the temperature area can be ensured, and the appearance temperature of the cavity can be reduced.
Wherein, the rack can be provided with a storage cavity and a drawer for storing articles.
Further, the lifting structure comprises a vertical supporting plate connected to the frame, a guide rail is arranged on the vertical supporting plate, a lifting sliding block is arranged on the guide rail, a connecting plate is connected to the furnace cover, and the connecting plate is connected with the lifting sliding block; the lifting sliding block is driven by a motor.
Through connecting the bell on elevation structure, can realize the automation of bell and open and close through control system, make staff's operation more convenient, improved the automation function of device.
Further, the sample testing platform comprises a support column connected to the inside of the heating furnace body, a workpiece disc is connected to the support column, and a plurality of placing holes are formed in the workpiece disc; the temperature measuring structure comprises a first temperature thermocouple for monitoring the internal temperature of the heating furnace body and a second temperature thermocouple for monitoring the sample testing platform; the center of the workpiece disc is provided with a through hole for placing a first temperature thermocouple; each placement hole is correspondingly provided with a small hole for placing a second temperature thermocouple.
The temperature control mode of the system adopts a mode of 'temperature controller and power regulator temperature control', a closed loop control system is formed by matching with the first temperature thermocouple and the second temperature thermocouple, automatic control of temperature is realized, and the conductive temperature controller is configured for curve setting and heating control, and the temperature control precision is controlled to be +/-1 ℃.
The first temperature thermocouple and the second temperature thermocouple are flexible thermocouples, the second temperature thermocouple is in direct contact with the copper clamp in the sample testing platform, the consistency of temperature measurement can be ensured, and the accuracy of a monitoring result is improved.
Further, the vacuum obtaining system comprises a compound molecular pump, wherein the compound molecular pump is connected with a high-vacuum manual baffle valve, and the high-vacuum manual baffle valve is connected with the heating furnace body and is connected with an ionization gauge at the joint; the high-vacuum manual baffle valve is connected with a backing valve, the backing valve is connected with a first corrugated pipe, and the first corrugated pipe is connected with a vortex vacuum pump.
Further, the vortex vacuum pump is connected with the first corrugated pipe through a first three-way adapter, a second corrugated pipe is connected to the first three-way adapter, the second corrugated pipe is connected with a pre-pumping valve, the pre-pumping valve is connected with the heating furnace body through a second three-way adapter, and a resistance gauge is connected to the second three-way adapter.
Furthermore, the control system adopts the hardware configuration of a PLC and an industrial personal computer, and realizes the automatic control of the system by matching with special labview upper computer software on a main control computer.
The control system can realize automatic control of the heating process through the setting of upper computer software, can record the data of each sensor in real time, store the data, facilitate inquiry, has the functions of monitoring and alarming, and can automatically protect shutdown when abnormality occurs.
Further, the water cooling system comprises a water chiller, and a water pipe of the water chiller is connected with a control valve, a flowmeter and a temperature sensor.
Further, the observation system comprises a CCD camera; the heating furnace body is provided with an observation window for observing an internal sample, and the CCD camera is placed at the observation window.
The plurality of observation windows can be arranged, meanwhile, illumination lamps can be arranged at the observation windows, and when the brightness in the inner cavity of the heating furnace body is insufficient, the illumination lamps can be turned on to increase the brightness, so that the shot photo is clearer; the CCD camera is in communication connection with the main control computer, the main control computer is in communication connection with the CCD camera through a signal line, the fixed temperature photographing and storage can be realized, and the frequency can be set.
In a second aspect, the present application provides a method for using a high vacuum in situ observation device, comprising the steps of:
step 1: starting a cold water machine, a main power supply and a power supply of a power control cabinet, and starting an industrial control computer and a main control computer; opening a gas release valve on the heating furnace body, opening a furnace cover through a control program after the slow inflation process of the cavity is finished, placing a sample in a copper clamp and on a workpiece disc, contacting a second temperature thermocouple testing end with the copper clamp, and controlling a lifting structure to close the furnace cover through the control program;
step 2: opening a vortex vacuum pump and a pre-pumping valve, closing the pre-pumping valve when the pressure in the vacuum chamber is lower than 5Pa, opening a backing valve and a high-vacuum manual baffle valve, and opening a compound molecular pump when the pressure in the cavity and the communication pipeline is lower than 5 Pa; when the vacuum degree of the whole chamber reaches the required requirement, starting a heating control key, and heating according to heating parameters set in advance in a parameter column;
step 3: the photographing software is opened, the exposure degree and photographing frequency of the photo are set, and an auxiliary lighting lamp outside the furnace is opened; before the target photographing starting temperature is not reached, the state of the sample is observed offline in real time; after reaching the target photographing temperature, the system automatically photographs according to the set photographing frequency and records photographing time;
step 4: after the temperature is raised, the heater stops working, when the temperature in the heating furnace body is lower than 100 ℃, the high-vacuum manual baffle valve is closed, then the compound molecular pump is closed, and when the indicator lamp of the compound molecular pump stops flashing, the backing valve and the vortex vacuum pump are closed;
step 5: opening the air release valve on the heating furnace body, and the vacuum degree in the heating furnace body to be heated is 8 multiplied by 10 4 When Pa is above, opening a furnace cover, taking out a sample, and finishing the experiment;
step 6: and comparing the photo of the time and morphology of the melted sample with the data recording page to obtain the accurate melting temperature of the sample.
Compared with the prior art, the application has the following advantages and beneficial effects:
(1) The testing temperature of the high vacuum in-situ observation device in the use process can reach 1000 ℃, and the vacuum degree can reach 5.0 multiplied by 10 within 1 hour -5 Pa (cold state, after baking), heating according to a set temperature rising curve, monitoring the state of a sample in real time through an observation system, realizing automatic operation of vacuumizing, heating and observation processes through a control system, easily controlling the monitoring conditions, obtaining more accurate monitoring results, obtaining more accurate melting point temperature, and being suitable for real-time observation of melting behaviors of various alloy materials and accurate measurement of melting points;
(2) The temperature measuring structure is arranged, so that the temperature inside the heating furnace body and the temperature change of the sample in the melting process of the sample can be monitored in real time, and the temperature inside the heating furnace body can be controlled conveniently; the sample is placed in the copper clamp and in the workpiece disc placing holes, and each placing hole is correspondingly provided with a small hole for placing a second temperature thermocouple, so that the melting point of each sample can be accurately measured. The air release valve is arranged on the heating furnace body, so that the temperature and the air release are convenient and quick, and the interior of the heating furnace body can quickly reach the atmospheric pressure state;
(3) Through connecting the bell on elevation structure, can realize the automation of bell and open and close through control system, make staff's operation more convenient, improved the automation function of device.
Drawings
In order to more clearly illustrate the technical solutions of the exemplary embodiments of the present application, the drawings that are needed in the examples will be briefly described, which are only illustrative of some examples of the present application and therefore should not be considered as limiting the scope, and other related drawings can be obtained according to these drawings without inventive effort for a person skilled in the art. In the drawings:
FIG. 1 is a perspective view of a high vacuum in situ observation device according to the present application;
FIG. 2 is a schematic view of a high vacuum in situ observation device according to the present application;
FIG. 3 is an enlarged view of FIG. 2A;
FIG. 4 is a side view of a high vacuum in situ viewing device according to the present application;
FIG. 5 is a top view of a high vacuum in situ observation device according to the present application;
FIG. 6 is a top view of a sample testing platform of a high vacuum in situ observation device according to the present application;
fig. 7 is a display diagram of a control panel of the control system according to the present application.
In the drawings, the reference numerals and corresponding part names:
the device comprises the following components of a 01-second corrugated pipe, a 02-second three-way adapter, a 03-pre-pumping valve, a 04-resistor gauge, a 05-deflating valve, a 06-rack, a 07-furnace bottom, a 08-CCD camera, a 09-heating furnace body, a 10-vertical supporting plate, a 11-guide rail, a 12-lifting sliding block, a 13-connecting plate, a 14-furnace cover, a 15-ionization gauge, a 16-high-vacuum manual baffle valve, a 17-foregrade valve, a 18-compound molecular pump, a 19-first corrugated pipe, a 20-first three-way adapter, a 21-vortex vacuum pump, a 22-motor, a 23-workpiece disc, a 24-supporting column, a 25-first temperature thermocouple, a 26-second temperature thermocouple, a 27-placing hole, a 28-small hole and a 29-through hole.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present application more apparent, the technical solutions of the embodiments of the present application will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present application, and it is apparent that the described embodiments are some embodiments of the present application, but not all embodiments of the present application. The components of the embodiments of the present application generally described and illustrated in the figures herein may be arranged and designed in a wide variety of different configurations.
Thus, the following detailed description of the embodiments of the application, as presented in the figures, is not intended to limit the scope of the application, as claimed, but is merely representative of selected embodiments of the application. All other embodiments, which can be made by those skilled in the art based on the embodiments of the application without making any inventive effort, are intended to be within the scope of the application.
It should be noted that: like reference numerals and letters denote like items in the following figures, and thus once an item is defined in one figure, no further definition or explanation thereof is necessary in the following figures.
In the description of the present application, it should also be noted that, unless explicitly specified and limited otherwise, the terms "disposed," "mounted," "connected," and "connected" are to be construed broadly, and may be, for example, fixedly connected, detachably connected, connected or integrally connected; can be directly connected or indirectly connected through an intermediate medium, and can be communication between two elements. The specific meaning of the above terms in the present application will be understood in specific cases by those of ordinary skill in the art.
Example 1
As shown in fig. 1 to 6, the embodiment provides a high vacuum in-situ observation device, which comprises a heating furnace body system, a sample testing platform, a vacuum obtaining system, a control system, a water cooling system and an observation system; the sample testing platform is arranged in the heating furnace body system; the control system is used for realizing the automatic operation of the vacuumizing, heating and observing processes.
Specifically, the heating furnace body system comprises a heating furnace body 09 connected to a rack 06, a heating cylinder is connected inside the heating furnace body 09, a furnace cover 14 is connected to the top of the heating furnace body 09 through a lifting structure, and a temperature measuring structure for measuring the temperature of samples inside the heating furnace body 09 and on a sample testing platform is connected to the furnace bottom 07 of the heating furnace body 09; the heating furnace body 09 is connected with a purge valve 05. The temperature inside the heating furnace body 09 and the temperature change of the sample in the sample melting process can be monitored in real time by installing the temperature measuring structure, so that the temperature inside the heating furnace body 09 can be controlled conveniently; the air release valve 05 arranged on the heating furnace body 09 is convenient and quick to cool down and release air, so that the inside of the heating furnace body 09 can quickly reach the atmospheric pressure state.
Wherein, the inner cavity size of the heating furnace body 09 is about phi 500 x 550mm, the external dimension of the main machine is 1700x900x1870mm (length x width x height). The tantalum heating belt is adopted for heating, the power is about 12kw, the tantalum heating belt is uniformly arranged in the cavity, the ceramic is insulated, and the maximum heating temperature is 1000 ℃. The outer side of the heater is provided with a plurality of heat insulation layers, five layers of stainless steel are adopted, the temperature uniformity (better than +/-3 ℃) in a temperature area is ensured, and the external surface temperature of the cavity can be reduced.
Specifically, the lifting structure comprises a vertical supporting plate 10 connected to the frame 06, a guide rail 11 is arranged on the vertical supporting plate 10, a lifting slide block 12 is arranged on the guide rail 11, a connecting plate 13 is connected to a furnace cover 14, and the connecting plate 13 is connected with the lifting slide block 12; the lifting slide 12 is driven by a motor 22. Through connecting bell 14 on elevation structure, can realize the automation of bell 14 and open and close through control system, make staff's operation more convenient, improved the automation function of device.
Specifically, the sample testing platform comprises a support column 24 (208 mm in height) connected to the interior of the heating furnace body 09, a workpiece disc 23 (120 mm in diameter) is connected to the support column 24, and a plurality of placing holes 27 are formed in the workpiece disc 23; the temperature measuring structure comprises a first temperature thermocouple 25 for monitoring the internal temperature of the heating furnace body 09 and a second temperature thermocouple 26 for monitoring the sample testing platform; a through hole 29 for placing the first temperature thermocouple 25 is arranged in the center of the workpiece disc 23; each placement hole 27 is correspondingly provided with a small hole 28 for placing the second thermocouple 26.
The temperature control mode of the system adopts a mode of 'temperature controller plus power regulator temperature control', a closed loop control system is formed by matching the first temperature thermocouple 25 and the second temperature thermocouple 26, automatic control of temperature is realized, and the conductive temperature controller is configured for curve setting and heating control, and the temperature control precision is controlled to be +/-1 ℃.
The first temperature thermocouple 25 and the second temperature thermocouple 26 are flexible thermocouples, and the second temperature thermocouple 26 is in direct contact with the copper clamp in the sample testing platform, so that the consistency of temperature measurement can be ensured, and the accuracy of a monitoring result is improved.
The control system can realize automatic control of the heating process through the setting of upper computer software, can record the data of each sensor in real time, store the data, facilitate inquiry, has the functions of monitoring and alarming, and can automatically protect shutdown when abnormality occurs.
Specifically, the vacuum obtaining system comprises a compound molecular pump 18, a high-vacuum manual baffle valve 16 is connected to the compound molecular pump 18, the high-vacuum manual baffle valve 16 is connected with a heating furnace body 09, and an ionization gauge 15 is connected at the joint; the high vacuum manual flapper valve 16 is connected to a backing valve 17, the backing valve 17 is connected to a first bellows 19, and the first bellows 19 is connected to a scroll vacuum pump 21.
The scroll vacuum pump 21 is connected with the first corrugated pipe 19 through a first tee joint 20 (KF 40), a second corrugated pipe 01 (KF 40 x 473) is connected to the first tee joint 20, the second corrugated pipe 01 is connected with a pre-pumping valve 03, the pre-pumping valve 03 is connected with the heating furnace body 09 through a second tee joint 02, and a resistance gauge 04 is connected to the second tee joint 02.
The vacuum obtaining system is configured with a KYKY composite molecular pump FF170/700 type 18 and a Bao Si vacuum GSP3 type dry pump, can achieve excellent vacuum degree, a vacuum pipeline is made of 304 materials, partial connecting pipelines are connected by corrugated pipes, and the cold vacuum degree can reach 5.0 multiplied by 10 within 1 hour -5 Pa。
The control system adopts 'Siemens PLC+industrial personal computer hardware' configuration, realizes automatic control of the system by matching with special labview upper computer software on a main control computer, can realize automatic control of a heating process by setting of the upper computer software, can record data of each sensor in real time, stores the data, is convenient to inquire, has monitoring and alarming functions, can automatically protect and stop when abnormality occurs, adopts a 'temperature controller+power regulator temperature control' mode in the aspect of temperature accurate control, forms a closed loop control system by matching with a thermocouple, realizes automatic temperature control, configures a conductive temperature controller for curve setting and heating control, and has temperature control precision of +/-1 ℃.
Specifically, the water cooling system comprises a water chiller, and a water pipe of the water chiller is connected with a control valve, a flowmeter and a temperature sensor. The water cooling system can monitor the state of cooling water in real time, and can send out an alarm signal and automatically protect when abnormality occurs.
Specifically, the observation system includes a CCD camera 08; the heating furnace body 09 is provided with an observation window for observing the internal sample, and the CCD camera 08 is placed at the observation window. Wherein, a plurality of observation windows can be arranged, and meanwhile, illumination lamps can be arranged at the observation windows, when the brightness in the inner cavity of the heating furnace body 09 is insufficient, the illumination lamps can be turned on to increase the brightness, so that the photographed pictures are clearer; the CCD camera 08 is in communication connection with a main control computer, the main control computer is in communication connection with the CCD camera 08 through a signal wire, can take pictures at fixed temperature and store, and the frequency can be set.
The irradiation temperature monitoring device can reach 1000 ℃ in the use process, and the vacuum degree can reach 5.0 multiplied by 10 within 1 hour -5 Pa (cold state, after baking), can heat according to the temperature rising curve of settlement, monitor the state of sample through the observation system real time, realize the automatic operation of evacuation, heating and observation process through control system, monitor the condition and easily control, monitor the result more accurate, obtain the melting point temperature more accurate, be applicable to multiple alloy material melting behavior real-time observation and melting point's accurate measurement.
Example 2
Based on embodiment 1, referring to fig. 1 to 6, this embodiment provides a method for using a high vacuum in situ observation device, comprising the steps of:
step 1: starting a cold water machine, a main power supply and a power supply of a power control cabinet, and starting an industrial control computer and a main control computer; opening a deflation valve 05 on the heating furnace body 09, opening the furnace cover 14 through a control program after the slow inflation process of the cavity is finished, placing a sample in a copper clamp and on a workpiece disc 23, contacting the test end of the second temperature thermocouple 26 with the copper clamp, and controlling the lifting structure to close the furnace cover 14 through the control program;
step 2: opening the vortex vacuum pump 21 and the pre-pumping valve 03, closing the pre-pumping valve 03 when the pressure in the vacuum chamber is lower than 5Pa, opening the backing valve 17 and the high-vacuum manual baffle valve 16, and opening the compound molecular pump 18 when the pressure in the chamber and the communication pipeline is lower than 5 Pa; when the vacuum degree of the whole chamber reaches the required requirement, starting a heating control key, and heating according to heating parameters set in advance in a parameter column;
step 3: the photographing software is opened, the exposure degree and photographing frequency of the photo are set, and an auxiliary lighting lamp outside the furnace is opened; before the target photographing starting temperature is not reached, the state of the sample is observed offline in real time; after reaching the target photographing temperature, the system automatically photographs according to the set photographing frequency and records photographing time;
step 4: after the temperature rise is finished, the heater stops working, when the temperature in the heating furnace body 09 is lower than 100 ℃, the high-vacuum manual baffle valve 16 is closed, the compound molecular pump 18 is closed, and when the indicator lamp of the compound molecular pump 18 stops flashing, the backing valve 17 and the vortex vacuum pump 21 are closed;
step 5: opening a deflation valve 05 on the heating furnace body 09, opening a furnace cover 14 when the vacuum degree in the heating furnace body 09 is more than 8X 104Pa, and taking out the sample, thereby completing the experiment;
step 6: and comparing the photo of the time and morphology of the melted sample with the data recording page to obtain the accurate melting temperature of the sample.
Application case
The use of one of the high vacuum in situ observation apparatus of example 1 and one of the high vacuum in situ observation apparatus of example 2 was used to monitor Ag-Li alloy materials of unknown specific melting temperature (theoretical liquidus 472 c, solidus 420 c), which were processed to be smaller than the size of the quartz tube, according to the following operating method:
(1) Starting a water chiller, a main power supply, a power supply of an electric control cabinet, starting an industrial personal computer and a main control computer, and determining that all parts are complete and normal;
(2) Opening a deflation valve 05 on the heating furnace body 09, opening the furnace cover 14 through a control program after the slow inflation process of the cavity is finished, placing an Ag-Li alloy sample in a quartz tube and in a copper clamp, placing the whole into a placing hole 27 of a workpiece disc 23, enabling the test end of a second temperature thermocouple 26 to be in contact with the copper clamp, and controlling a lifting structure to close the furnace cover 14 by a control system;
(3) Opening the vortex vacuum pump 21 and the pre-pumping valve 03, closing the pre-pumping valve 03 when the pressure in the vacuum chamber is lower than 5Pa, opening the backing valve 17 and the high-vacuum manual baffle valve 16, and opening the compound molecular pump 18 when the pressure in the chamber and the communication pipeline is lower than 5 Pa; setting a heating curve, heating from room temperature to 420 ℃ for 50min, then heating to 520 ℃ for 200min, and preserving heat for 30min; the output power was set at 40% and the auto-photographing temperature was set at 420 ℃. When the vacuum degree of the whole chamber meets the required requirement, heating is started, and the data recording page can record the temperature, vacuum degree and other data in the whole experiment process in real time;
(4) The photographing software is opened, the exposure degree (60) and the photographing frequency (1/30 sec) of the photograph are set, an auxiliary lighting lamp outside the furnace is opened, the state of a sample can be observed offline in real time before 420 ℃ is reached, and after the target photographing temperature is reached, the system automatically photographs according to the set photographing frequency and records photographing time;
(5) After the temperature rise is finished, the heater automatically stops working, then the temperature in the furnace is waited for cooling, when the temperature in the furnace is lower than 100 ℃, the high-vacuum manual baffle valve 16 is closed, the compound molecular pump 18 is closed, and when the indicator lamp of the compound molecular pump 18 stops flashing, the backing valve 17 and the vortex vacuum pump 21 are closed;
(6) Slowly opening the air release valve 05 until the vacuum degree in the furnace is 8 multiplied by 10 4 Opening a furnace cover 14 when Pa is above, and taking out a sample to finish the experiment; closing the furnace cover 14 and exhausting air to ensure that the equipment is in a high vacuum state when idle so as to prolong the service life of the equipment;
(7) And comparing the recorded photo of the melting time and morphology of the sample with a data recording page to obtain the accurate melting temperature of the Ag-Li alloy sample at 458 ℃.
The foregoing description of the embodiments has been provided for the purpose of illustrating the general principles of the application, and is not meant to limit the scope of the application, but to limit the application to the particular embodiments, and any modifications, equivalents, improvements, etc. that fall within the spirit and principles of the application are intended to be included within the scope of the application.
Claims (10)
1. The high-vacuum in-situ observation device is characterized by comprising a heating furnace body system, a sample testing platform, a vacuum acquisition system, a control system, a water cooling system and an observation system; the sample testing platform is arranged in the heating furnace body system; the control system is used for realizing automatic operation of vacuumizing, heating and observing processes.
2. The high vacuum in-situ observation device according to claim 1, wherein the heating furnace body system comprises a heating furnace body (09) connected to a rack (06), a heating cylinder is connected inside the heating furnace body (09), a furnace cover (14) is connected to the top of the heating furnace body (09) through a lifting structure, and a temperature measuring structure for measuring the temperature inside the heating furnace body (09) and on a sample testing platform is connected to a furnace bottom (07) of the heating furnace body (09); and the heating furnace body (09) is connected with a release valve (05).
3. A high vacuum in situ observation device according to claim 2, characterized in that the lifting structure comprises a vertical support plate (10) connected to a frame (06), a guide rail (11) is mounted on the vertical support plate (10), a lifting slide block (12) is mounted on the guide rail (11), a connecting plate (13) is connected to the furnace cover (14), and the connecting plate (13) is connected with the lifting slide block (12); the lifting slide block (12) is driven by a motor (22).
4. The high vacuum in-situ observation device according to claim 2, wherein the sample testing platform comprises a support column (24) connected to the interior of the heating furnace body (09), a workpiece disc (23) is connected to the support column (24), and a plurality of placement holes (27) are formed in the workpiece disc (23); the temperature measuring structure comprises a first temperature thermocouple (25) for monitoring the internal temperature of the heating furnace body (09) and a second temperature thermocouple (26) for monitoring the sample testing platform; a through hole (29) for placing a first temperature thermocouple (25) is formed in the center of the workpiece disc (23); each placement hole (27) is correspondingly provided with a small hole (28) for placing a second temperature thermocouple (26).
5. The high vacuum in-situ observation device according to claim 1, wherein the vacuum obtaining system comprises a compound molecular pump (18), a high vacuum manual baffle valve (16) is connected to the compound molecular pump (18), the high vacuum manual baffle valve (16) is connected with a heating furnace body (09), and an ionization gauge (15) is connected at the connection position; the high-vacuum manual baffle valve (16) is connected with the backing valve (17), the backing valve (17) is connected with the first corrugated pipe (19), and the first corrugated pipe (19) is connected with the vortex vacuum pump (21).
6. The high vacuum in-situ observation device according to claim 5, wherein a first three-way adapter (20) is adopted between the vortex vacuum pump (21) and the first corrugated pipe (19), a second corrugated pipe (01) is connected to the first three-way adapter (20), the second corrugated pipe (01) is connected to a pre-pumping valve (03), the pre-pumping valve (03) is connected to the heating furnace body (09) through a second three-way adapter (02), and a resistance gauge (04) is connected to the second three-way adapter (02).
7. The high vacuum in-situ observation device according to claim 1, wherein the control system adopts a PLC+industrial personal computer hardware configuration, and is matched with special labview upper computer software on a main control computer to realize automatic control of the system.
8. The high vacuum in-situ observation device according to claim 1, wherein the water cooling system comprises a water chiller, and a water pipe of the water chiller is connected with a control valve, a flowmeter and a temperature sensor.
9. A high vacuum in situ viewing device as claimed in claim 1, wherein the viewing system comprises a CCD camera (08); an observation window for observing an internal sample is arranged on the heating furnace body (09), and the CCD camera (08) is placed at the observation window.
10. A method of using the high vacuum in situ observation device of any one of claims 1 to 9, comprising the steps of:
step 1: starting a cold water machine, a main power supply and a power supply of a power control cabinet, and starting an industrial control computer and a main control computer; opening a deflation valve (05) on the heating furnace body (09), opening a furnace cover (14) through a control program after the slow inflation process of the cavity is finished, placing a sample in a copper clamp and on a workpiece disc (23), contacting the test end of a second temperature thermocouple (26) with the copper clamp, and controlling a lifting structure to close the furnace cover (14) through the control program;
step 2: opening a vortex vacuum pump (21) and a pre-pumping valve (03), closing the pre-pumping valve (03) when the pressure in the vacuum chamber is lower than 5Pa, opening a backing valve (17) and a high-vacuum manual baffle valve (16), and opening a compound molecular pump (18) when the pressure in the cavity and the communication pipeline is lower than 5 Pa; when the vacuum degree of the whole chamber reaches the required requirement, starting a heating control key, and heating according to heating parameters set in advance in a parameter column;
step 3: the photographing software is opened, the exposure degree and photographing frequency of the photo are set, and an auxiliary lighting lamp outside the furnace is opened; before the target photographing starting temperature is not reached, the state of the sample is observed offline in real time; after reaching the target photographing temperature, the system automatically photographs according to the set photographing frequency and records photographing time;
step 4: after the temperature rise is finished, the heater stops working, when the temperature in the heating furnace body (09) is lower than 100 ℃, the high-vacuum manual baffle valve (16) is closed, then the compound molecular pump (18) is closed, and when the indicator lamp of the compound molecular pump (18) stops flashing, the backing valve (17) and the vortex vacuum pump (21) are closed;
step 5: opening a release valve (05) on the heating furnace body (09), wherein the vacuum degree in the heating furnace body (09) is 8 multiplied by 10 4 When Pa is above, opening a furnace cover (14), taking out a sample, and finishing the experiment;
step 6: and comparing the photo of the time and morphology of the melted sample with the data recording page to obtain the accurate melting temperature of the sample.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311072504.XA CN117092157A (en) | 2023-08-24 | 2023-08-24 | High-vacuum in-situ observation device and use method thereof |
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| CN202311072504.XA CN117092157A (en) | 2023-08-24 | 2023-08-24 | High-vacuum in-situ observation device and use method thereof |
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| CN117092157A true CN117092157A (en) | 2023-11-21 |
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