CN112485198A - High-low temperature in-situ spectrum reaction tank - Google Patents

High-low temperature in-situ spectrum reaction tank Download PDF

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Publication number
CN112485198A
CN112485198A CN202011336009.1A CN202011336009A CN112485198A CN 112485198 A CN112485198 A CN 112485198A CN 202011336009 A CN202011336009 A CN 202011336009A CN 112485198 A CN112485198 A CN 112485198A
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low temperature
base
sample
groove
window
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黄伟峰
陈兴
范辉
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Huayan Environmental Science Beijing Technology Co ltd
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Huayan Environmental Science Beijing Technology Co ltd
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/01Arrangements or apparatus for facilitating the optical investigation
    • G01N21/03Cuvette constructions
    • G01N21/0332Cuvette constructions with temperature control
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/01Arrangements or apparatus for facilitating the optical investigation
    • G01N21/03Cuvette constructions
    • G01N2021/0325Cells for testing reactions, e.g. containing reagents
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/01Arrangements or apparatus for facilitating the optical investigation
    • G01N21/03Cuvette constructions
    • G01N21/0332Cuvette constructions with temperature control
    • G01N2021/0335Refrigeration of cells; Cold stages
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/01Arrangements or apparatus for facilitating the optical investigation
    • G01N21/03Cuvette constructions
    • G01N2021/0389Windows

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  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Optical Measuring Cells (AREA)

Abstract

The invention discloses a high-low temperature in-situ spectral reaction tank, and relates to the technical field of spectral reaction tanks. The device comprises a base, an optical window, a sample table, a refrigeration unit, a heating unit, a ventilation unit and an electrical test unit; the top wall of the base is provided with a groove, and the optical window covers the groove to form a sealed cavity; the sample platform is positioned in the groove, and a cavity is arranged in the sample platform. The invention has the beneficial effects that: the reaction tank disclosed by the invention realizes the control of high and low temperature environmental fields in a small system through simple structural layout, the temperature can reach a change range from extremely low temperature of 4K to 300 ℃ above zero, and the circuit layout of various gases and liquids is greatly reduced. Meanwhile, in a limited space size, the reaction tank is also provided with an electrode pressing sheet and an SMA joint of a wiring part for electrical test under a variable temperature condition, so that the electrical test requirements under high and low temperatures are met.

Description

High-low temperature in-situ spectrum reaction tank
Technical Field
The invention relates to the technical field of spectral reaction tanks, in particular to a high-low temperature in-situ spectral reaction tank.
Background
The temperature parameter, as an important physical property change parameter, will affect various properties of the material in many aspects. In fact, the behavior of the material will change greatly from ambient temperature to low temperature, and therefore, it is very meaningful to study the mechanism of the change of the temperature parameter to change the electrical, thermal, mechanical and magnetic properties of pure metal, alloy and insulator from the perspective of general engineering. The properties of the material are generally adapted to specific physical equations, which can be used to predict the behavior of the system. They depend on chemical composition, crystal structure, atom and charge interaction, heat treatment or mechanical treatment, etc., and are affected by temperature change. Therefore, when considering the change of a material with temperature, it is very important to understand the mechanism of the relevant characteristics.
The thermal (and electrical) properties of any material are related to the vibration of its atoms around their equilibrium position (in the crystal lattice). The amplitude of these vibrations depends on the temperature and decreases with decreasing temperature. These vibrations may propagate at the speed of sound within the material and are studied as plane waves associated with phonons. If the material is a conductor, the thermal properties also depend on the movement of negative charges (electrons) and positive charges (vacancies). The heat capacity C is then defined as the amount of energy (heat) that must be introduced in a certain amount of material in order to raise its temperature T by 1K. Reversibly, it is the energy 1K extracted from the quantity of material that lowers its temperature. Thus, the thermal capacity of a material is its ability to store or release thermal energy. It is an important attribute in the cooling or preheating process that can be used to estimate the energy (and cost) involved, and to evaluate the heat transfer transient in relation to thermal diffusivity. In addition to these intrinsic variables, the electron transport capacity or the conductivity for metallic conductors or semiconductors is directly related to the temperature. As for a metallic conductor, the charge e is transported by n "free electrons". At ambient temperature, the electron free path e is dominated by electron scattering caused by thermal vibration of the crystal lattice (phonons). At low temperatures, it is limited mainly by scattering of chemical and physical lattice defects (chemical impurities, vacancies, dislocations). Whereas for semiconductors, charge is transported by conduction band electrons and holes in the valence band. Near ambient temperature, lattice vibration dominates and the electrical performance is not affected by impurities. At low temperatures, lattice vibrations are negligible and impurities play an important role in charge transport. Thus, the resistivity of semiconductors is very non-linear, and temperature generally increases with decreasing temperature due to the decrease in electrons in the conduction band. An important application of this property is the use of semiconductors as temperature sensors (thermistors). Therefore, the temperature parameter has very important significance on various properties of the material, and the problem that how to research the change of the temperature parameter on the change of the intrinsic property of the material is also a great problem for researchers.
At present, the market has more equipment aiming at high and low temperature environments, but most of the equipment is concentrated in the creation of the high and low temperature environments of the equipment, namely, only one environmental field equipment with a low temperature environment or a high temperature environment can be provided. For example, patent No. CN203502338U discloses an in-situ infrared spectrum reaction cell, but it can only realize reaction monitoring in high temperature environment.
Meanwhile, the equipment is often too large in size, large in occupied space and too numerous in various lines to be well adapted to various existing spectroscopy instruments. The method not only occupies a limited experimental space when the in-situ is lost, but also is difficult to satisfy the research of various physical properties of laboratory researchers under different temperature change conditions. Because, if the optical spectrum characterization instrument is to be adapted to various currently commercialized optical spectrum characterization instruments, the high and low temperature device is necessarily small in size, and also needs to be very portable, and more importantly, a certain light path is reserved for various optical characterizations, which puts high design requirements on the equipment. In fact, the combination of various in-situ characterization methods with high and low temperature environments is a rapidly developing research field, because different structural characterization methods can be used to research the conformational changes of substances, and it will further provide the possibility of using advanced detection methods to perform on-line monitoring on metastable substances, which is the reason why this kind of in-situ testing technology has gained much attention in multiple cross-scientific fields, such as the field of earth science, the field of materials, and the chemical/physical field.
Disclosure of Invention
The invention aims to solve the technical problem that the in-situ spectral reaction tank in the prior art can only realize reaction monitoring in a high-temperature or low-temperature environment, and provides a high-temperature and low-temperature in-situ spectral reaction tank.
The invention solves the technical problems through the following technical means:
the invention provides a high-low temperature in-situ spectral reaction tank, which comprises a base, an optical window, a sample table, a refrigerating unit, a heating unit, a ventilating unit and an electrical testing unit, wherein the optical window is arranged on the base; the top wall of the base is provided with a groove, and the optical window covers the groove to form a sealed cavity;
the sample table is positioned in the groove, and a cavity is formed in the sample table; the refrigeration unit is a semiconductor refrigeration piece, or comprises a liquid nitrogen inlet, a liquid nitrogen outlet, a first connecting pipe and a second connecting pipe, wherein the liquid nitrogen inlet and the liquid nitrogen outlet are communicated with a cavity of the sample stage;
the heating unit is wrapped on the outer side of the sample table; the ventilation unit comprises an air outlet joint, and the air outlet joint is positioned at one end of the base; the electrical testing unit comprises an electrode pressing sheet and an SMA connector, wherein one end of the electrode pressing sheet is in contact with a sample on the sample table, and the other end of the electrode pressing sheet is connected with the SMA connector.
The working principle is as follows: the sample to be measured is placed on the sample platform, the optical window is covered on the groove, a sealed cavity is formed in the groove, after the installation is completed, the air outlet connector is connected with the vacuumizing device, the sealed cavity is vacuumized, then the reaction tank is placed on the spectroscopy line station, after the optical path is aligned, liquid nitrogen is introduced into the first connecting pipe, and after the liquid nitrogen passes through the cavity in the sample platform, the liquid nitrogen flows out of the second connecting pipe, so that the sample on the sample platform is refrigerated, and relevant data are collected. Stopping introducing the liquid nitrogen, starting the heating unit, heating by the heating unit, and collecting related data. The sample was contacted with the electrode pad and subjected to electrical testing.
Has the advantages that: the reaction tank in the invention realizes the control of high and low temperature environmental fields in a small system through simple structural layout, the temperature can reach the lowest extreme low temperature of 4K and the variation range of 300 ℃ above zero, wherein the liquid helium system can reach 4K at the lowest, the liquid nitrogen system can reach 77K, the semiconductor refrigerating sheet system can reach 50 ℃ below zero, and meanwhile, the circuit layout of various gases and liquids is greatly reduced. Meanwhile, in a limited space size, the reaction tank is also provided with an electrode pressing sheet and an SMA joint of a wiring part for electrical test under a variable temperature condition, so that the electrical test requirements under high and low temperatures are met.
Preferably, the heating unit comprises a heating body and a resistance wire, the resistance wire is wound on the heating body, the heating body is located on the inner bottom wall of the groove of the base, and the heating body is connected with the sample table through a bolt.
Preferably, the heating unit further comprises a thermocouple, one end of the thermocouple is inserted into the heating body, and the other end of the thermocouple extends out of the base.
Has the advantages that: the high temperature and the low temperature are monitored by a thermocouple.
Preferably, the optical window includes upper cover, first sealing washer, window piece and window lid, the upper cover is located the recess top, the upper cover is connected with the base roof, the upper cover is equipped with first through-hole, the sample platform is located first through-hole below, the window piece is located first through-hole top, first sealing washer is located between window piece and the upper cover, the window lid is located window piece top, the window lid can be dismantled with the upper cover and be connected.
Preferably, the electrical test unit further comprises a guide rail, a bearing seat and a support pillar, the guide rail is located on the bottom wall of the groove, the bearing seat is located on a sliding block of the guide rail, one end of the support pillar is rotatably connected with the bearing seat, the axis of the support pillar is perpendicular to the sliding direction of the sliding block on the guide rail, and the sliding block moves to enable the support pillar to be close to or far away from the sample table; one end of the electrode pressing sheet is connected with one end of the supporting column, and the other end of the electrode pressing sheet is in contact with a sample on the sample table.
Has the advantages that: through the removal of guide rail top shoe, adjust the distance between support column and the sample platform to adjust the distance between electrode preforming and the sample platform, the support column is installed on the bearing frame, and the support column can be with the axis of support column at the recess internal rotation, thereby adjusts the position of electrode preforming and the bench sample of sample, thereby carries out electricity test to the sample.
Preferably, one end of the electrode pressing sheet is provided with a second through hole, one end of the supporting column is provided with a corresponding third through hole, bolts are arranged in the second through hole and the third through hole, and nuts are arranged on the bolts.
Has the advantages that: after a sample is placed on the sample table, the position of the electrode pressing piece is adjusted according to the sample, so that one end of the electrode pressing piece is in contact with the sample.
Preferably, the electrode pad includes a fixing end and a probe end, the fixing end and the probe end are integrally formed, the fixing end is connected with one end of the supporting column, and the probe end forms a tip.
Has the advantages that: the volume of the electrode pressing sheet is reduced, and the influence of the electrode pressing sheet on the light path during light path analysis is reduced.
Preferably, the ventilation unit further comprises an air inlet joint, and the air inlet joint and the air outlet joint are respectively located at two ends of the base.
Preferably, the air inlet joint and the air outlet joint are both provided with two-way ball valves.
The working principle of the invention is as follows: placing a sample to be tested on a sample platform, covering an optical window on a groove, forming a sealed cavity in the groove, connecting an air outlet joint with a vacuumizing device after installation is completed, vacuumizing the sealed cavity, then placing a reaction tank on a spectroscopy line station, aligning a light path, taking a liquid nitrogen system as an example, introducing liquid nitrogen from a first connecting pipe, and after the liquid nitrogen passes through a cavity in the sample platform, flowing out from a second connecting pipe, refrigerating the sample on the sample platform, and collecting related data. Stopping introducing the liquid nitrogen, starting the heating unit, heating by the heating unit, and collecting related data. The sample was contacted with the electrode pad and subjected to electrical testing.
The invention has the advantages that: the reaction tank disclosed by the invention realizes the control of high and low temperature environmental fields in a small system through simple structural layout, the temperature can reach a change range from 4K to 300 ℃ above zero, the circuit layout of various gases and liquids is greatly reduced, and the in-situ spectral analysis of samples under high and low temperature conditions is met.
Meanwhile, in a limited space size, the reaction tank is also provided with an electrode pressing sheet and an SMA joint of a wiring part for electrical test under a variable temperature condition, so that the electrical test requirements under high and low temperatures are met.
Through the removal of guide rail top shoe, adjust the distance between support column and the sample platform to adjust the distance between electrode preforming and the sample platform, the support column is installed on the bearing frame, and the support column can be with the axis of support column at the recess internal rotation, thereby adjusts the position of electrode preforming and the bench sample of sample, thereby carries out electricity test to the sample.
Drawings
FIG. 1 is a top view of a high and low temperature in-situ spectroscopy reaction cell according to an embodiment of the present invention;
FIG. 2 is a cross-sectional view taken along the direction A in FIG. 1;
FIG. 3 is a cross-sectional view taken along the direction B in FIG. 1;
in the figure: a base 111; an upper cover 1121; a first seal 1122; a window sheet 1123; a window cover 1124; a sample stage 113; a liquid nitrogen inlet 1141; a liquid nitrogen outlet 1142; a first connection tube 1143; a second connection pipe 1144; heating body 1151; electrode interface 1152; an outlet connector 1161; an air inlet junction 1162; an electrode pad 1171; a fixed end 11711; a probe end 11712; SMA linker 1172; a guide rail 1173; a bearing seat 1174; support post 1175.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It will be understood that when an element is referred to as being "secured to" another element, it can be directly on the other element or intervening elements may also be present. When an element is referred to as being "connected" to another element, it can be directly connected to the other element or intervening elements may also be present.
It is noted that, in this document, relational terms such as first and second, and the like, if any, are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other identical elements in a process, method, article, or apparatus that comprises the element.
A high-low temperature in-situ spectral reaction cell is shown in figures 1-3 and comprises a base 111, an optical window, a sample stage 113, a refrigeration unit, a heating unit, a ventilation unit and an electrical test unit.
The top wall of the base 111 is provided with a groove, and the base 111 is made of 316 stainless steel to protect the reaction tank safely.
As shown in fig. 2 and 3, the optical window includes an upper cover 1121, a first sealing ring 1122, a window sheet 1123 and a window cover 1124, in this embodiment, the window sheet 1123 is made of a pressure-resistant and highly transparent quartz sheet to ensure the transparency of laser or X-ray, the cross section of the window sheet 1123 is circular, the diameter of the window sheet 1123 is not less than 46mm, and the thickness is 0.5 mm. The upper cover 1121 is located above the groove, a hole is formed in the upper cover 1121, a corresponding threaded hole is formed in the top wall of the base 111, the upper cover 1121 is connected with the top wall of the base 111 through a bolt and a nut, a first through hole is formed in the center of the upper cover 1121, the window sheet 1123 is installed on the first through hole, the first sealing ring 1122 is located between the window sheet 1123 and the upper cover 1121, the window sheet 1123 is sealed, and a second sealing ring is arranged between the bottom wall of the upper cover 1121 and the top wall of the base 111. The window cover 1124 is located above the window piece 1123, the window cover 1124 is connected with the upper cover 1121 through bolts and nuts, and a sealed cavity is formed among the upper cover 1121, the window piece 1123 and the groove of the base 111.
In the embodiment, the sample stage 113 is formed in a column shape, the sample stage 113 is fixedly installed in the groove, the sample stage 113 is located right below the window sheet 1123, the sample stage 113 is fixedly installed by welding but not limited to welding, a cavity is arranged in the sample stage 113, and the sample stage 113 is made of 316 stainless steel.
As shown in fig. 1-3, the refrigeration unit is a semiconductor refrigeration piece (not shown), and when the refrigeration unit is a semiconductor refrigeration piece, the semiconductor refrigeration piece is located in the groove and below the sample stage 113.
Or the refrigeration unit comprises a liquid nitrogen inlet 1141, a liquid nitrogen outlet 1142, a first connecting pipe 1143 and a second connecting pipe 1144, the liquid nitrogen inlet 1141 and the liquid nitrogen outlet 1142 are communicated with the cavity of the sample stage 113, one end of the liquid nitrogen inlet 1141 and one end of the liquid nitrogen outlet 1142 are respectively welded on the side wall of the sample stage 113, the other end of the liquid nitrogen inlet 1141 is connected with one end of the first connecting pipe 1143, the other end of the liquid nitrogen outlet 1142 is connected with one end of the second connecting pipe 1144, the other end of the first connecting pipe 1143 penetrates through the side wall of the base 111, and the other end of the second connecting pipe 1144 penetrates through the side.
The first connection pipe 1143 is connected to a liquid nitrogen pump, liquid nitrogen is input through the liquid nitrogen pump, and the input liquid nitrogen is output from the second connection pipe 1144.
The heating unit includes heating member 1151 and resistance wire (not shown), the resistance wire winding is on heating member 1151, pottery (not shown) pipe is established to the cover on the resistance wire, be used for insulating, heating member 1151 is located the inner diapire of 111 recesses of base, heating member 1151 wraps up in the sample platform 113 outside, heating member 1151's material is 316 stainless steel in this embodiment, pass through bolt and nut connection between heating plate and the sample platform 113, make the better laminating of the two together, play better heat conduction effect.
The heating unit further includes a thermocouple (not shown), which is Pt100 in this embodiment, for measuring temperature, one end of the thermocouple is inserted into a sidewall of the heating body 1151 and fixed with vacuum paste, and the other end of the thermocouple passes through the base 111. Also included in this embodiment is electrode interface 1152, electrode interface 1152 is mounted to a side wall of base 111, and the wires for the resistance wire and thermocouple are connected to electrode interface 1152.
The ventilation unit includes an air outlet connector 1161 and an air inlet connector 1162, one end of the air outlet connector 1161 is fixedly connected with one end of the base 111, one end of the air inlet connector 1162 is fixedly connected with the other end of the base 111, the air outlet connector 1161 and the air inlet connector 1162 in this embodiment are both ferrule connectors, and the ferrule connectors and the end portion of the base 111 are sealed through sealing rings. The air outlet connector 1161 is connected to a vacuum pumping device for vacuum pumping of the sealed cavity, or the sealed cavity may be vented through the air inlet connector 1162. In this embodiment, two-way ball valves are installed on both the inlet connector 1162 and the outlet connector 1161.
As shown in fig. 2 and 3, the electrical testing unit includes an electrode pad 1171, an SMA joint 1172, a guide rail 1173, a bearing seat 1174 and a support column 1175, the guide rail 1173 is fixedly installed on the bottom wall of the groove, the bearing seat 1174 is fixedly installed on a slide block of the guide rail 1173, one end of the support column 1175 is rotatably connected with the bearing seat 1174, the axis of the support column 1175 is perpendicular to the sliding direction of the slide block on the guide rail 1173, and the slide block moves to enable the support column 1175 to approach or move away from the sample stage 113.
Electrode pressing piece 1171 includes stiff end 11711 and probe end 11712, stiff end 11711 and probe end 11712 integrated into one piece, electrode pressing piece 1171's fixed and support column 1175's one end is connected, electrode pressing piece 1171's one end is equipped with the second through-hole, support column 1175's one end is equipped with corresponding third through-hole, be equipped with the bolt in second through-hole and the third through-hole, mounting nut on the bolt, through bolt and nut adjustment electrode pressing piece 1171's inclination. The probe end 11712 of the electrode pad 1171 is pointed, reducing the volume of the electrode pad 1171 and reducing the influence of the electrode pad 1171 on the optical path during optical path analysis. The SMA connector 1172 is fixedly installed on the side wall of the base 111 by welding, and the fixed end 11711 of the electrode pressing sheet 1171 is connected with the SMA connector 1172 by a wire. The electrode pad 1171 includes, but is not limited to, the specific pattern described above, and can be connected to probe ends of other shapes.
In this embodiment, the number of the electrode pressing pieces 1171, the number of the SMA joints 1172, the number of the guide rails 1173, the number of the bearing seats 1174, and the number of the support columns 1175 are four, and the four guide rails 1173 are distributed around the sample table 113.
The working principle of the embodiment is as follows: place the sample that awaits measuring on sample platform 113, close optical window lid 1124 on the recess, make the interior sealed cavity that forms of recess, after the installation is accomplished, will give vent to anger and connect 1161 and evacuating device and be connected, carry out the evacuation to sealed cavity, then place the reaction cell on the spectroscopy line station, aim at the light path after, let in the liquid nitrogen in first connecting pipe 1143, the liquid nitrogen is after the cavity in sample platform 113, flow from second connecting pipe 1144, thereby refrigerate the sample on sample platform 113, gather relevant data. Stopping introducing the liquid nitrogen, starting the heating unit, heating by the heating unit, and collecting related data.
The distance between the support column 1175 and the sample platform 113 is adjusted through the movement of the slide block on the guide rail 1173, so that the distance between the electrode pressing sheet 1171 and the sample platform 113 is adjusted, the support column 1175 is installed on the bearing block 1174, and the support column 1175 can rotate in the groove along the axis of the support column 1175, so that the positions of the samples on the electrode pressing sheet 1171 and the sample platform 113 are adjusted, and therefore the samples are subjected to electrical tests at different temperatures.
The beneficial effects of the embodiment are that: the reaction tank in the embodiment realizes the control of high and low temperature environmental fields in a small system through a simple structural layout, the temperature can reach the lowest extreme low temperature of 4K and the variation interval of 300 ℃ above zero, the liquid helium system can reach 4K at the lowest, the liquid nitrogen system can reach 77K, the semiconductor refrigerating sheet system can reach 50 ℃ below zero, and meanwhile, the circuit layout of various gases and liquids is greatly reduced. Meanwhile, in a limited space size, the reaction tank is also provided with an electrode pressing sheet 1171 of a wiring component for electrical test and an SMA joint 1172 under a temperature-changing condition, so that the electrical test requirements under high and low temperatures are met.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.

Claims (10)

1. A high-low temperature in-situ spectrum reaction tank is characterized in that: the device comprises a base, an optical window, a sample table, a refrigerating unit, a heating unit, a ventilating unit and an electrical testing unit; the top wall of the base is provided with a groove, and the optical window covers the groove to form a sealed cavity;
the sample table is positioned in the groove, a cavity is formed in the sample table, the refrigerating unit is a semiconductor refrigerating piece, or the refrigerating unit comprises a liquid nitrogen inlet, a liquid nitrogen outlet, a first connecting pipe and a second connecting pipe, the liquid nitrogen inlet and the liquid nitrogen outlet are communicated with the cavity of the sample table, one end of the first connecting pipe is connected with the liquid nitrogen inlet, the other end of the first connecting pipe extends out of the base, one end of the second connecting pipe is connected with the liquid nitrogen outlet, and the other end of the second connecting pipe extends out of the base;
the heating unit is wrapped on the outer side of the sample table; the ventilation unit comprises an air outlet joint, and the air outlet joint is positioned at one end of the base; the electrical testing unit comprises an electrode pressing sheet and an SMA connector, wherein one end of the electrode pressing sheet is in contact with a sample on the sample table, and the other end of the electrode pressing sheet is connected with the SMA connector.
2. The high-low temperature in-situ spectrum reaction cell of claim 1, wherein: the heating unit comprises a heating body and a resistance wire, the resistance wire is wound on the heating body, the heating body is located on the inner bottom wall of the groove of the base, and the heating body is connected with the sample table through a bolt.
3. The high-low temperature in-situ spectrum reaction cell of claim 2, wherein: the heating unit further comprises a thermocouple, one end of the thermocouple is inserted into the heating body, and the other end of the thermocouple extends out of the base.
4. The high-low temperature in-situ spectrum reaction cell of claim 1, wherein: the optical window comprises an upper cover, a first sealing ring, a window piece and a window cover, wherein the upper cover is located above the groove, the upper cover is connected with the top wall of the base, a first through hole is formed in the upper cover, the sample platform is located below the first through hole, the window piece is located above the first through hole, the first sealing ring is located between the window piece and the upper cover, the window cover is located above the window piece, and the window cover is detachably connected with the upper cover.
5. The high-low temperature in-situ spectrum reaction cell of claim 1, wherein: the electrical testing unit further comprises a guide rail, a bearing seat and a support pillar, the guide rail is positioned on the bottom wall in the groove, the bearing seat is positioned on a sliding block of the guide rail, one end of the support pillar is rotatably connected with the bearing seat, the axis of the support pillar is perpendicular to the sliding direction of the sliding block on the guide rail, and the sliding block moves to enable the support pillar to be close to or far away from the sample table; one end of the electrode pressing sheet is connected with one end of the supporting column, and the other end of the electrode pressing sheet is in contact with a sample on the sample table.
6. The high-low temperature in-situ spectrum reaction cell of claim 5, wherein: one end of the electrode pressing sheet is provided with a second through hole, one end of the supporting column is provided with a corresponding third through hole, bolts are arranged in the second through hole and the third through hole, and nuts are arranged on the bolts.
7. The high-low temperature in-situ spectrum reaction cell of claim 5, wherein: the electrode pressing sheet comprises a fixed end and a probe end, the fixed end and the probe end are integrally formed, the fixed end is connected with one end of the supporting column, and the probe end forms a tip.
8. The high-low temperature in-situ spectrum reaction cell of claim 1, wherein: the ventilation unit further comprises an air inlet connector, and the air inlet connector and the air outlet connector are respectively located at two ends of the base.
9. The high-low temperature in-situ spectrum reaction cell of claim 8, wherein: and the air inlet joint and the air outlet joint are both provided with two-way ball valves.
10. The high-low temperature in-situ spectrum reaction cell of claim 1, wherein: the upper cover is provided with a hole, the top wall of the base is provided with a corresponding threaded hole, and the upper cover is connected with the top wall of the base through a bolt and a nut.
CN202011336009.1A 2020-11-25 2020-11-25 High-low temperature in-situ spectrum reaction tank Pending CN112485198A (en)

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Cited By (7)

* Cited by examiner, † Cited by third party
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CN113030062A (en) * 2021-03-29 2021-06-25 国家纳米科学中心 Electricity-spectrum signal detection device, system device and detection method
CN113075874A (en) * 2021-03-23 2021-07-06 中国科学院精密测量科学与技术创新研究院 Device for improving uncertainty of radiation frequency shift of atomic optical lattice blackbody
CN113125479A (en) * 2021-04-15 2021-07-16 中国科学技术大学 Reaction device for in-situ temperature-changing X-ray scattering characterization
CN114216890A (en) * 2021-11-23 2022-03-22 合肥原位科技有限公司 High-temperature Raman/X-ray diffraction in-situ spectrum testing device
CN115308242A (en) * 2022-08-05 2022-11-08 合肥原位科技有限公司 Ultra-high temperature X-ray diffraction in-situ spectrum testing device
CN115869858A (en) * 2023-02-13 2023-03-31 中国科学技术大学 High-temperature gas-solid in-situ sum frequency spectrum reaction tank
WO2023065673A1 (en) * 2021-10-20 2023-04-27 浙江大学衢州研究院 In-situ spectral analysis cell for gas sensing exploration and application

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113075874A (en) * 2021-03-23 2021-07-06 中国科学院精密测量科学与技术创新研究院 Device for improving uncertainty of radiation frequency shift of atomic optical lattice blackbody
CN113030062A (en) * 2021-03-29 2021-06-25 国家纳米科学中心 Electricity-spectrum signal detection device, system device and detection method
CN113125479A (en) * 2021-04-15 2021-07-16 中国科学技术大学 Reaction device for in-situ temperature-changing X-ray scattering characterization
WO2023065673A1 (en) * 2021-10-20 2023-04-27 浙江大学衢州研究院 In-situ spectral analysis cell for gas sensing exploration and application
CN114216890A (en) * 2021-11-23 2022-03-22 合肥原位科技有限公司 High-temperature Raman/X-ray diffraction in-situ spectrum testing device
CN115308242A (en) * 2022-08-05 2022-11-08 合肥原位科技有限公司 Ultra-high temperature X-ray diffraction in-situ spectrum testing device
CN115869858A (en) * 2023-02-13 2023-03-31 中国科学技术大学 High-temperature gas-solid in-situ sum frequency spectrum reaction tank

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