CN111289439A - Local high-temperature environment device for dynamic infrared spectroscopy technology - Google Patents
Local high-temperature environment device for dynamic infrared spectroscopy technology Download PDFInfo
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- CN111289439A CN111289439A CN202010132661.5A CN202010132661A CN111289439A CN 111289439 A CN111289439 A CN 111289439A CN 202010132661 A CN202010132661 A CN 202010132661A CN 111289439 A CN111289439 A CN 111289439A
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- 238000005516 engineering process Methods 0.000 title claims abstract description 11
- 238000004566 IR spectroscopy Methods 0.000 title claims description 5
- 238000010438 heat treatment Methods 0.000 claims abstract description 70
- 239000000919 ceramic Substances 0.000 claims abstract description 50
- 230000007613 environmental effect Effects 0.000 claims abstract description 24
- 238000002474 experimental method Methods 0.000 claims abstract description 3
- 238000012544 monitoring process Methods 0.000 claims abstract description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 11
- 239000010453 quartz Substances 0.000 claims description 10
- 230000000149 penetrating effect Effects 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 15
- 238000002329 infrared spectrum Methods 0.000 abstract description 13
- 230000008859 change Effects 0.000 abstract description 5
- 238000000034 method Methods 0.000 abstract description 5
- 230000008569 process Effects 0.000 abstract description 5
- 238000012360 testing method Methods 0.000 abstract description 5
- 230000008878 coupling Effects 0.000 abstract description 4
- 238000010168 coupling process Methods 0.000 abstract description 4
- 238000005859 coupling reaction Methods 0.000 abstract description 4
- 238000010249 in-situ analysis Methods 0.000 abstract description 2
- 238000013461 design Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 238000002834 transmittance Methods 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 210000004907 gland Anatomy 0.000 description 1
- 238000012844 infrared spectroscopy analysis Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
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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
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
- G01N21/03—Cuvette constructions
- G01N21/0332—Cuvette constructions with temperature control
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- G—PHYSICS
- G05—CONTROLLING; REGULATING
- G05D—SYSTEMS FOR CONTROLLING OR REGULATING NON-ELECTRIC VARIABLES
- G05D23/00—Control of temperature
- G05D23/19—Control of temperature characterised by the use of electric means
- G05D23/20—Control of temperature characterised by the use of electric means with sensing elements having variation of electric or magnetic properties with change of temperature
- G05D23/22—Control of temperature characterised by the use of electric means with sensing elements having variation of electric or magnetic properties with change of temperature the sensing element being a thermocouple
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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
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
- G01N2021/0106—General arrangement of respective parts
- G01N2021/0112—Apparatus in one mechanical, optical or electronic block
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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
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
- G01N21/03—Cuvette constructions
- G01N2021/0389—Windows
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- Analytical Chemistry (AREA)
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Abstract
The invention belongs to the field of infrared spectrum application, and discloses a local high-temperature environment device for a dynamic infrared spectrum technology, which comprises an environment box upper cover, a high-temperature environment box and an environment box bottom plate, wherein notches for a sample to pass through are arranged at two ends of the high-temperature environment box; the upper cover of the environment box and the high-temperature environment box are respectively fixed with a ceramic heating ring; an electrifying socket of the upper cover of the environment box is inserted into an electrifying socket of the high-temperature environment box to form a closed loop, and the upper ceramic heating ring and the lower ceramic heating ring can be heated simultaneously by electrifying; the environmental box bottom plate is provided with a wire outlet to lead out a line to the external temperature control box; and the thermocouple is arranged on the upper cover of the environment box and used for monitoring the experiment environment temperature and feeding back a temperature signal to the external temperature control box. The invention can realize the force-thermal coupling loading on the material in the infrared spectrum in-situ analysis, simultaneously ensures the local heating and uniform heating of the sample, has high heating speed, stable constant temperature and compact structure, and can better analyze the local structural change rule in the material mechanics test process on line.
Description
Technical Field
The invention belongs to the field of infrared spectrum application, and particularly relates to an environment loading device for a dynamic infrared spectrum technology.
Background
The dynamic infrared spectrum technology is used for carrying out in-situ infrared spectrum analysis on chemical compositions and molecular structures of materials in the process of testing mechanical properties of the materials and is used for measuring the rule that chemical components of the materials change along with the changes of time, temperature and external force. Most of materials analyzed by the dynamic infrared spectroscopy technology are high polymer materials, and are sensitive to temperature, and the local structure of the materials can change correspondingly with the temperature. Therefore, accurate temperature control in a force-thermal coupling loading environment is crucial to infrared spectroscopic analysis of materials.
The existing environmental loading device of the dynamic infrared spectrum technology has some problems, such as: 1. local accurate heating is difficult to realize in the heating environment in the environment cavity; 2. the heating unit of a common environment loading device is arranged at the bottom of an environment box, a sample is heated only at the bottom, the local heating uniformity cannot be guaranteed, and the structural design of the sample surrounding the periphery uniform heating is to be developed.
Disclosure of Invention
The invention aims to solve the technical problem that the existing environment loading device is difficult to ensure accurate heating and uniform heating, and provides a local high-temperature environment device for a dynamic infrared spectrum technology, which can realize force-thermal coupling loading on a material in infrared spectrum in-situ analysis, ensures local heating and uniform heating of a sample, has high heating speed, stable constant temperature and compact structure, and can better analyze the local structural change rule in the material mechanics test process on line.
In order to solve the technical problems, the invention is realized by the following technical scheme:
a local high-temperature environment device for a dynamic infrared spectrum technology comprises an environment box upper cover, a high-temperature environment box and an environment box bottom plate which are sequentially arranged from top to bottom; notches for the sample to pass through are respectively arranged at two ends of the high-temperature environment box;
a first ceramic heating ring and a second ceramic heating ring are respectively fixed on the opposite surfaces of the upper cover of the environment box and the high-temperature environment box, and the first ceramic heating ring and the second ceramic heating ring are correspondingly arranged above and below the sample; a circuit groove and an electrified socket are preset in the upper cover of the environment box, and a circuit of the first ceramic heating ring is led to the electrified socket along the circuit groove; the high-temperature environment box is provided with an electrifying contact pin corresponding to the electrifying socket, the electrifying contact pin is inserted into the electrifying socket to form a closed loop, and the closed loop is electrified to heat the first ceramic heating ring and the second ceramic heating ring simultaneously, so that the local uniform heating of the sample is realized;
the environment box bottom plate is fixedly connected with the high-temperature environment box, and is provided with a wire outlet which is used for penetrating through a connecting lead between the closed loop and the external temperature control box; the thermocouple is installed to environment case upper cover, and the thermocouple is used for monitoring the experiment ambient temperature between environment case upper cover and the high temperature environment case to feedback temperature signal to external temperature control case.
Further, the upper cover of the environment box is provided with a quartz slide.
Furthermore, the first ceramic heating ring and the second ceramic heating ring are fixed on the upper cover of the environment box and the high-temperature environment box through pressing sheets respectively, and the pressing sheets are installed on the upper cover of the environment box and the high-temperature environment box through fastening screws respectively.
Further, the positions of the upper cover of the environment box, the high-temperature environment box and the bottom plate of the environment box, which correspond to the center of the sample, are respectively provided with a light through hole; a light transmitting sheet made of quartz is embedded in the light transmitting hole of the environmental box bottom plate; the light-transmitting hole enables the light beam to directly irradiate the center of the surface of the sample.
Furthermore, the first ceramic heating ring, the second ceramic heating ring and the light through hole are concentric.
Further, the thermocouple is used for feeding back a real-time temperature signal in the device to an external temperature control box, and the external temperature control box controls the first ceramic heating ring and the second ceramic heating ring to be heated to a set target value simultaneously; and after the temperature signal fed back by the thermocouple reaches a set target value, the relay in the external temperature control box automatically regulates and controls to maintain the constant temperature and stability in the device.
The invention has the beneficial effects that:
the local high-temperature environment device for the dynamic infrared spectrum technology is compact in structural design, exquisite and light in structure and light in practical application environment; the heating unit in the device adopts a ceramic heating ring design, so that the local position is accurately heated, and the temperature can reach 300 ℃; the two ceramic heating rings are respectively arranged on the high-temperature environment box and the upper cover of the environment box, and are butted with the electrified socket through the electrified contact pin, so that simultaneous heating is realized, and the effect of uniformly heating the sample is achieved; an armored thermocouple is arranged in the device close to the sample and serves as a temperature sensor, so that accurate measurement and temperature control of the test environment are realized; the upper cover of the environment box, the high-temperature environment box and the bottom plate of the environment box are all provided with light through holes, and are covered with quartz slides and embedded with quartz glass on the bottom plate of the environment box, so that the good light transmission and the good tightness of the device are ensured; the environmental box bottom plate plays a role in heat insulation while leading out a line, a heat insulation layer is not needed, the structure is simple, and the cost is reduced.
Therefore, the invention can realize the accurate regulation and control of the temperature in the material in-situ infrared spectrum analysis process, simultaneously realize the local heating and the uniform heating of the sample, ensure the material force-thermal coupling loading environment by matching with a small mechanical testing machine, analyze the change rule of chemical components in the material loading process on line and meet the deep research on the chemical components and the deformation mechanism of the material.
Drawings
FIG. 1 is a structural assembly view of a localized high temperature environment device provided by an embodiment;
FIG. 2 is an exploded view of a localized high temperature environment apparatus provided by an embodiment;
FIG. 3 is a schematic structural diagram of an upper cover of an environmental chamber in a local high-temperature environment apparatus according to an embodiment.
In the above figures: 1: a thermocouple; 2: quartz slide; 3: an environment box upper cover; 4: a high temperature environment chamber; 5: an environmental chamber floor; 6: an outlet; 7: a first light passing hole; 8: a second light passing hole; 9: a second ceramic heating ring; 10: tabletting; 11: electrifying the pin; 12: a third light passing hole; 13: fastening the threaded hole; 14: a first ceramic heating ring; 15: a line slot; 16: and (6) electrifying the socket.
Detailed Description
In order to further understand the contents, features and effects of the present invention, the following embodiments are illustrated and described in detail with reference to the accompanying drawings:
as shown in fig. 1 and 2, the present embodiment provides a local high temperature environment device for dynamic infrared spectroscopy, the main structure of the device is composed of four layers of structures, namely, a quartz slide 2, an environmental box upper cover 3, a high temperature environmental box 4 and an environmental box bottom plate 5, from top to bottom, and the environmental box upper cover 3, the high temperature environmental box 4 and the environmental box bottom plate 5 are all made of aluminum alloy.
The quartz slide 2 adopts an integral design and can be fixed on the upper cover 3 of the environmental box through a fastening screw, so that the replacement is convenient; the cover is arranged on the upper cover 3 of the environment box to ensure the transmittance of infrared light and the tightness of the equipment.
As shown in fig. 3, a first light through hole 7 is formed in the center of the upper cover 3 of the environmental chamber, and the first light through hole 7 corresponds to the center of the sample, so that the light beam can directly irradiate the center of the surface of the sample. The 3 internal surface central points of environment case upper cover put through the first ceramic heating ring 14 of preforming 10 fixed mounting, and preforming 10 is fixed in environment case upper cover 3 through fastening screw, and 10 central round hole diameters of preforming slightly are lighter than first ceramic heating ring 14, and first ceramic heating ring 14 is fixed and prevent to drop by the 10 glands of preforming. The first ceramic heating ring 14 and the first light through hole 7 are concentric as much as possible, so that the sample is uniformly heated around the center. Line groove 15 is predetermine through milling processing to 3 internal surfaces of environment case upper cover, and two angles departments that environment case upper cover 3 is located line groove 15 one side set up circular telegram socket 16 respectively, and the circuit of first ceramic heating ring 14 leads to circular telegram socket 16 along line groove 15, avoids preforming 10 to damage the circuit. A thermocouple 1 is fixedly installed on the upper cover 3 of the environment box, the thermocouple 1 is matched and fixedly connected with a threaded hole preset in the upper cover 3 of the environment box through an external thread processed by the thermocouple 1, and the lower end of the thermocouple 1 extends into the high-temperature environment box 4 to monitor the experimental environment temperature; the upper end of the quartz slide 2 is connected with an external temperature control box through which temperature signals are fed back.
The two ends of the high-temperature environment box 4 are respectively provided with a notch for the sample to pass through, so that the middle part of the sample is positioned inside the high-temperature environment box 4. The center of the high-temperature environment box 4 is provided with a second light through hole 8, and the second light through hole 8 corresponds to the first light through hole 7 in the vertical position. The central position of the upper surface at the bottom of the high-temperature environment box 4 is fixedly provided with a second ceramic heating ring 9 through a pressing sheet 10, similarly, the pressing sheet 10 is fixed at the bottom of the high-temperature environment box 4 through a fastening screw, the diameter of a central circular hole of the pressing sheet 10 is slightly smaller than that of the second ceramic heating ring 9, and the second ceramic heating ring 9 is fixed by a pressing sheet 10 through a pressing cover and is prevented from falling off. The second ceramic heating ring 9 and the first ceramic heating ring 14 are symmetrical in position and are respectively positioned below and above the middle part of the sample, so that the sample is locally and uniformly heated. Two corners on the same side of the high-temperature environment box 4 are respectively provided with an electrifying pin 11, and the positions of the electrifying pins 11 correspond to the electrifying sockets 16 one by one. The circuit of second ceramic heating ring 9 meets with circular telegram contact pin 11, and circular telegram contact pin 11 inserts the circular telegram socket 16 of environment case upper cover 3, and environment case upper cover 3 is connected the inside closed circuit that forms in back with high temperature environment case 4, guarantees first ceramic heating ring 14 and second ceramic heating ring 9 and heats simultaneously after circular telegram, makes the sample center thermally equivalent.
The environment box bottom plate 5 and the high-temperature environment box 4 are designed in a separated mode, and the environment box bottom plate 5 is fixedly connected with the high-temperature environment box 4 through mounting screws arranged at fastening threaded holes 13 at four corners of the environment box bottom plate. The circuit of second ceramic heating ring 9 divides left and right two strands to insert circular telegram contact pin 11, and circular telegram contact pin 11 interconnecting link stretches out from high temperature environment case 4 bottom, and the wire outlet 6 that 5 lateral parts of rethread environment bottom of the case board set up draws forth and inserts external temperature control box, and environment bottom of the case board 5 plays thermal-insulated effect when drawing forth ceramic heating ring 9 circuit, avoids high temperature damage mechanics loading device and infrared spectrometer. A third light through hole 12 is formed in the center of the environmental box bottom plate 5, and the third light through hole 12 corresponds to the upper and lower positions of the first light through hole 7 and the second light through hole 8; the third light-passing hole 12 is embedded with a light-transmitting sheet made of quartz material, so that the light transmittance of the device is ensured.
The high-temperature loading device is installed in the mechanical loading device, after the external temperature control box sets a target value, the thermocouple 1 feeds back real-time temperature signals in the high-temperature loading device to the external temperature control box, the external temperature control box controls the first ceramic heating ring 14 and the second ceramic heating ring 9 to be heated to the set target value simultaneously, and when the temperature signals fed back by the thermocouple 1 reach the target value, a relay in the external temperature control box automatically regulates and controls to enable the interior of the device to maintain constant temperature and stability.
Although the preferred embodiments of the present invention have been described above with reference to the accompanying drawings, the present invention is not limited to the above-described embodiments, which are merely illustrative and not restrictive, and those skilled in the art can make various changes and modifications within the spirit and scope of the present invention without departing from the spirit and scope of the appended claims.
Claims (6)
1. A local high-temperature environment device for a dynamic infrared spectroscopy technology is characterized by comprising an environment box upper cover, a high-temperature environment box and an environment box bottom plate which are sequentially arranged from top to bottom; notches for the sample to pass through are respectively arranged at two ends of the high-temperature environment box;
a first ceramic heating ring and a second ceramic heating ring are respectively fixed on the opposite surfaces of the upper cover of the environment box and the high-temperature environment box, and the first ceramic heating ring and the second ceramic heating ring are correspondingly arranged above and below the sample; a circuit groove and an electrified socket are preset in the upper cover of the environment box, and a circuit of the first ceramic heating ring is led to the electrified socket along the circuit groove; the high-temperature environment box is provided with an electrifying contact pin corresponding to the electrifying socket, the electrifying contact pin is inserted into the electrifying socket to form a closed loop, and the closed loop is electrified to heat the first ceramic heating ring and the second ceramic heating ring simultaneously, so that the local uniform heating of the sample is realized;
the environment box bottom plate is fixedly connected with the high-temperature environment box, and is provided with a wire outlet which is used for penetrating through a connecting lead between the closed loop and the external temperature control box; the thermocouple is installed to environment case upper cover, and the thermocouple is used for monitoring the experiment ambient temperature between environment case upper cover and the high temperature environment case to feedback temperature signal to external temperature control case.
2. The device according to claim 1, wherein the cover of the environmental chamber is covered with a quartz slide.
3. The device according to claim 1, wherein said first ceramic heating ring and said second ceramic heating ring are fixed to said environmental chamber upper cover and said high temperature environmental chamber by pressing plates, respectively, said pressing plates being mounted to said environmental chamber upper cover and said high temperature environmental chamber by fastening screws, respectively.
4. The device of claim 1, wherein the top cover of the environmental chamber, the top plate of the environmental chamber, and the bottom plate of the environmental chamber are respectively provided with a light hole corresponding to the center of the sample; a light transmitting sheet made of quartz is embedded in the light transmitting hole of the environmental box bottom plate; the light-transmitting hole enables the light beam to directly irradiate the center of the surface of the sample.
5. The device according to claim 4, wherein the first ceramic heating ring and the second ceramic heating ring are concentric with the light hole.
6. The device according to claim 1, wherein the thermocouple is configured to feed back a real-time temperature signal inside the device to an external temperature control box, and the external temperature control box controls the first ceramic heating ring and the second ceramic heating ring to be heated to a predetermined target value simultaneously; and after the temperature signal fed back by the thermocouple reaches a set target value, the relay in the external temperature control box automatically regulates and controls to maintain the constant temperature and stability in the device.
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