CN107884437A - It is a kind of to vary convenient and good airproof performance calorimeter sample cell - Google Patents

It is a kind of to vary convenient and good airproof performance calorimeter sample cell Download PDF

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Publication number
CN107884437A
CN107884437A CN201711327071.2A CN201711327071A CN107884437A CN 107884437 A CN107884437 A CN 107884437A CN 201711327071 A CN201711327071 A CN 201711327071A CN 107884437 A CN107884437 A CN 107884437A
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main body
sample cell
cylinder
sample
tank main
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CN107884437B (en
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史全
罗积鹏
尹楠
刘忻
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Dalian Institute of Chemical Physics of CAS
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Dalian Institute of Chemical Physics of CAS
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N25/00Investigating or analyzing materials by the use of thermal means
    • G01N25/20Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity

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Abstract

Convenient and good airproof performance calorimeter sample cell, its maximum operating temperature 600K are varied the invention discloses a kind of, and can facilitate, be fixed firmly in calorimeter.Sample cell specifically includes:Metallic gasket, there is the yardstick and hardness (mechanical strength) of setting;Sample tank main body, cylindrical tube, bottom centre position set a cylinder trap for going deep into cylinder, and to lay thermometer heating unit, cylinder top sets sealing to accept module;Thermocouple sheath, it is symmetrically welded at sample cell side;Hollow hex nut, upper hole set inside annular slot;Solid cylinder, top set hanging hole, and to hang sample cell, bottom sets the annular extension to be interlocked with annular slot.It is that bottom be hexagonal rectangle that wherein module is accepted in sealing, and main body car is into screw thread, the hollow cylinder equipped with the edge of a knife on top.Inventive samples pool structure is compact, novel in design, and sealing is tight, varies conveniently, using flexible.

Description

It is a kind of to vary convenient and good airproof performance calorimeter sample cell
Technical field
It is specially a kind of to vary convenient and good airproof performance adiabatic calorimetry dress the invention belongs to the calorimeter assembly in calorimetry The sample cell put, it is excellent to possess sealing property, and it is convenient that sample is changed, under 600K high temperature also can normal work, sample cell fixation side Just the characteristics of firm.
Background technology
Thermal capacitance is the summation of the forms of motion such as substance system internal crystal framework, electronics energy contribution, is a basis of material Thermal physical property parameter.By the accurate measure of thermal capacitance, the Basic thermodynamics data such as material enthalpy, entropy, Gibbs free energys can be obtained, Understand the structure of matter and phase transformation, and obtain the lattice vibration of material microstructure, transition of electronic energy and understand superconducting phenomenon, Magnetic action mechanism, a kind of method of structural aberration.Therefore, the accurate data of material thermal capacitance is obtained to excavating, designing new material, Optimize the preparation technology of material, promote the understanding of material science and development significant.
Adiabatic calorimetry is that measure material thermal capacitance is most accurate, one of most reliable method, however test take, vary trouble, Operation temperature area is low and narrow, operator need to possess the development and use that the deficiencies of certain professional knowledge limits it, so exploitation behaviour Control is succinct, vary convenience, stable performance, operation temperature area is high and width, the high adiabatic calorimetry device of accuracy are particularly important.And wherein Most critical link is the optimization of sample pool structure, so that it had both possessed reliable sealing, and can realizes quick, the side of sample Just change, while ensure that calorimeter has high accuracy and accuracy in high and wide warm area.
Built in the world in the representational Calorimetry system of adiabatic calorimetry research field including Osaka, Japan university Sorai at present Vertical 13-530K warm areas device (M.Sorai, K.Kaji, Y.Kaneko.An automated adiabatic calorimeter for the temperature range 13K to 530K The heat capacities of benzoic acid from 15K to 305K and of synthetic sapphire from 60to 505K.J.Chem.Thermodyn..1992,24,167-180.);The 50-310K temperature that Tokyo polytechnical university Atake is established Zone device (T.Tanaka, T.Atake, H.Nakayama, T.Eguchi, K.Saito, I.Ikemoto.Heat capacity and an incommensurate phase transition of crystalline bis(4-chlorophenyl) sulfone.J.Chem.Thermodyn..1994,26,1231-1239.);Dutch Utrecht university Van Miltenburg 10-350K warm areas device (J.C.Van Miltenburg, G.J.K.Van the Den Berg, M.J.Van of foundation Bommel.Construction of an adiabatic calorimeter measurements of the molar heat capacity of synthetic sapphire and of n-heptane.J.Chem.Thermodyn..1987, 19,1129-1137.).However, the sample cell of preceding two adiabatic calorimetry devices depends on and nips off capillary method to seal, this Method complex operation, and repeatability, reliability are poor;The instrument of Utrecht university varies trouble, and sample cell and heat screen are tight Close connection, it is unfavorable for controlling heat leak, influences accuracy of instrument.Meanwhile these three calorimeter assembly maximum temperatures are no more than 550K, sternly Ghost image rings its application.
Therefore, there is an urgent need to develop a kind of compact-sized, excellent performance, modern design, high-temperature region adiabatic calorimetry device Sample cell, to meet the active demand of current condensed state matter thermal capacitance property research.
The content of the invention
For the weak point of existing adiabatic calorimetry device, present invention proposition is a kind of to vary convenient and good airproof performance calorimetric Count sample cell, it possesses excellent sealing, can realize that sample is fast, easily changed, highest can under 600K high temperature work Make, while do not damage the accuracy and precision of adiabatic calorimetry device, also sample cell is easily fixed in calorimeter assembly.
The technical scheme is that:It is a kind of to vary convenient and good airproof performance calorimeter sample cell, including:
Module 4, thermocouple sheath 5, hollow hex nut are accepted in metallic gasket 1, sample tank main body 2, cylinder trap 3, sealing 6th, solid cylinder 7;
The sample tank main body 2 is cylindrical tube, including upper lid 15 and bottom 14, in the bottom of sample tank main body 2 Heart position sets a cylinder trap 3 for going deep into cylinder, and to lay thermometer-heating unit, the top of sample tank main body 2 is set Module 4 is accepted in sealing;
The quantity of thermocouple sheath 5 is two, is symmetrically welded at the side of sample tank main body 2;
Hole sets inside annular slot 12 on the hollow hex nut 6;
The top of solid cylinder 7 sets hanging hole 8, for hanging sample cell, the bottom of solid cylinder 7 set with The annular extension 13 that annular slot 12 interlocks;
It is described sealing accept module 4 be lower section be regular hexagon 9, middle part be the screwed main body 10 in outer surface, It is furnished with the hollow cylinder of the edge of a knife 11 in top;The sealing is accepted the complexed metal pad 1 of module 4 and connected with the hollow screw thread of hex nut 6 Connect.
Preferably, the material of metallic gasket 1 is Mohs' hardness 2-3 metal or alloy, and possesses high- and low-temperature resistance, leads Heating rate is high, chemical inertness, the properties such as mechanical strength is big.
Preferably, the metallic gasket 1 is circular, 0.1~2mm of thickness, 4~10mm of diameter.
Preferably, the sample tank main body 2 is high- and low-temperature resistance, high pressure resistant, and thermal conductivity is high, and chemical property is stable, and machinery is strong Cylindrical tube made of big metal or alloy is spent, its inner and outer surfaces plating last layer high- and low-temperature resistance, thermal conductivity is high, chemically The stable metal or alloy of matter.
Preferably, the length of sample tank main body 2 is 40~80mm, 10~40mm of external diameter, 0.5~5mm of thickness;The bottom Lid 14 is 10~40mm of external diameter, 3~15mm of internal diameter, 0.5~5mm of thickness annulus;The upper lid 15 is 10~40mm of external diameter, interior Hole section be 2~10mm of the length of side regular hexagon annulus, 0.5~5mm of its thickness;Serving is thick in the sample tank main body 2 Spend 0.1~1mm.
Preferably, the cylinder trap 3 with the identical material of sample tank main body 2 by being made, top seal, bottom opening;Institute State cylinder trap 3~15mm of diameter, 20~50mm of length.
Preferably, the thermocouple sheath 5 is high- and low-temperature resistance, and thermal conductivity is high, and the big metal or alloy of mechanical strength is made Cylinder, be symmetrically welded at the side of sample tank main body 2;Thermocouple sheath 5 5~25mm of length, the 0.5~3mm of external diameter are thick Spend 0.05~0.5mm.
Preferably, the hollow hex nut 6 is high- and low-temperature resistance, and thermal conductivity is high, the big metal or alloy system of mechanical strength ;2~the 10mm of thickness of hollow hex nut 6,2~10mm of the length of side, nut 4~10mm of internal diameter, pitch 1~2.5mm are described Annular slot 12 0.5~3mm of thickness, 3~8mm of internal diameter.
Preferably, the solid cylinder 7 is manufactured from the same material with hollow hex nut 6;The solid cylinder 7 is grown Spend 5~15mm, diameter 3~8mm, the hanging hole 8 diameter 1~3mm, the annular 0.5~3mm of thickness of extension 13, external diameter 4~ 10mm。
Preferably, it is described sealing accept module 4 be with the identical material of sample tank main body 2 made of hollow cylinder, it is hollow To realize the filling of sample or displacement.
Preferably, the 3~8mm of inner hollow diameter of module 4 is accepted in the sealing;2~10mm of the length of side of the regular hexagon 9 is thick Spend 2~8mm;The main body 10 4~10mm of external diameter, 1~2.5mm of pitch, 5~15mm of length;The length 0.5 of the edge of a knife 11~ 3mm, 30 °~60 ° of inclination angle.
The present invention has following beneficial effect:
(1) sample cell is compact-sized, and design is fine, so that inside and outside differential pressure of the sample in 100MPa in sample cell Under, it will not also leak, possess excellent sealing;
(2) sample can easily be changed by the handling of hollow nut and metallic gasket, operator;
(3) because each several part is in close contact, sample cell can integrally keep good heat transfer, and all parts temperature difference is little In 0.05K, all high thermal capacitance data of accuracy and precision can be obtained;
(4) sample cell can under 600K high temperature normal work;
(5) fixation of the sample cell in whole calorimeter assembly is realized using the lanyard through hanging hole;
(6) in addition, whole sample cell can be loaded and unloaded easily, and it is straight with calorimeter assembly miscellaneous part to turn avoid it Contact.
Brief description of the drawings
Fig. 1 is the structural representation in inventive samples pond.
Fig. 2 is the structural representation that module is accepted in lid and sealing on inventive samples pond.
Fig. 3 is the structural representation of the hollow hex nut of the present invention.
In figure:1st, metallic gasket;2nd, sample tank main body;3rd, cylinder trap;4th, module is accepted in sealing;5th, thermocouple sheath;6、 Hollow hex nut;7th, solid cylinder;8th, hanging hole;9th, regular hexagon;10th, screw thread;11st, the edge of a knife;12nd, annular slot;13rd, ring Shape extension;14th, bottom;15th, upper lid.
Embodiment
The present invention will be described in detail with reference to the accompanying drawings and examples.
Adiabatic calorimetry device reaches the requirement of thermal insulation by eliminating the heat exchange of sample cell and environment, accurate so as to obtain Reliable thermal capacitance data, so sample pool structure is the most important thing of adiabatic calorimetry device design.
It is of the present invention it is a kind of vary convenient and good airproof performance calorimeter sample cell, adiabatic calorimetry device can be met Intrinsic thermal insulation, the degree of accuracy, accuracy are high, and the requirement of reproducible grade, and can realizes the quickly and easily replacing of measurement sample, And still possesses intact sealing property under 600K high temperature.
As Figure 1-3, it is a kind of to vary convenient and good airproof performance calorimeter sample cell, including:
Module 4, thermocouple sheath 5, hollow hex nut are accepted in metallic gasket 1, sample tank main body 2, cylinder trap 3, sealing 6th, solid cylinder 7;
Sample tank main body 2 is cylindrical tube, including upper lid 15 and bottom 14, the bottom centre position of sample tank main body 2 are set The cylinder for going deep into a cylinder trap 3 is put, to lay thermometer-heating unit, the top of sample tank main body 2 sets sealing to accept module 4;
The quantity of thermocouple sheath 5 is two, is symmetrically welded at the side of sample tank main body 2;
Hole sets inside annular slot 12 on hollow hex nut 6;
The top of solid cylinder 7 sets hanging hole 8, and for hanging sample cell, the bottom of solid cylinder 7 is set and annular slot The 12 annular extensions 13 to interlock;
Sealing accept module 4 be lower section be regular hexagon 9, middle part be the screwed main body 10 in outer surface, top Hollow cylinder equipped with the edge of a knife 11;Sealing is accepted the complexed metal pad 1 of module 4 and is threadedly coupled with hollow hex nut 6.
Wherein, the material of metallic gasket 1 is Mohs' hardness 2-3 metal or alloy, and possesses high- and low-temperature resistance, and thermal conductivity is high, Chemical inertness, the properties such as mechanical strength is big.
Metallic gasket 1 is circular, 0.1~2mm of thickness, 4~10mm of diameter.
Sample tank main body 2 is high- and low-temperature resistance, high pressure resistant, and thermal conductivity is high, and chemical property is stable, the big metal of mechanical strength Or cylindrical tube made of alloy, its inner and outer surfaces plating last layer high- and low-temperature resistance, thermal conductivity is high, the stable gold of chemical property Category or alloy.
The length of sample tank main body 2 is 40~80mm, 10~40mm of external diameter, 0.5~5mm of thickness;Bottom 14 be external diameter 10~ 40mm, 3~15mm of internal diameter, 0.5~5mm of thickness annulus;Upper lid 15 is 10~40mm of external diameter, inner hole section be the length of side 2~ The annulus of 10mm regular hexagon, 0.5~5mm of its thickness;0.1~1mm of thickness of coating inside and outside sample tank main body 2.
Cylinder trap 3 with the identical material of sample tank main body 2 by being made, top seal, bottom opening;Cylinder trap diameter 3~ 15mm, 20~50mm of length.
Thermocouple sheath 5 is high- and low-temperature resistance, and thermal conductivity is high, and cylinder made of the big metal or alloy of mechanical strength is right Title is welded on the side of sample tank main body 2;Thermocouple sheath 5 5~25mm of length, 0.5~3mm of external diameter, 0.05~0.5mm of thickness.
Hollow hex nut 6 is high- and low-temperature resistance, and thermal conductivity is high, and the big metal or alloy of mechanical strength is made;Hollow hexagonal Nut 6 2~10mm of thickness, 2~10mm of the length of side, nut 4~10mm of internal diameter, 1~2.5mm of pitch, the thickness 0.5 of annular slot 12~ 3mm, 3~8mm of internal diameter.
Solid cylinder 7 is manufactured from the same material with hollow hex nut 6;5~the 15mm of length of solid cylinder 7, diameter 3 ~8mm, hanging hole 8 diameter 1~3mm, annular extension 13 0.5~3mm of thickness, 4~10mm of external diameter.
Sealing accept module 4 be with the identical material of sample tank main body 2 made of hollow cylinder, it is hollow to realize sample Filling or displacement.
3~the 8mm of inner hollow diameter of module 4 is accepted in sealing;2~10mm of the length of side of regular hexagon 9,2~8mm of thickness;Main body 10 4~10mm of external diameter, 1~2.5mm of pitch, 5~15mm of length;0.5~the 3mm of length of the edge of a knife 11,30 °~60 ° of inclination angle.
The application method in inventive samples pond is described below:
Following steps are used to load and unload sample with the thermal capacitance of measurement of species particularly liquid:
(1) with washes of absolute alcohol sample cell all parts three times, then it is washed with deionized three times;
(2) by the drying of sample cell all parts, drying, after being cooled to room temperature, weigh and average three times;
(3) sample cell all parts and sample are all put into the glove box for filling helium;
(4) hollow cylinder that sample is accepted to module 4 from sealing is added in sample tank main body 2, until reaching sample cell The 3/4 of volume;
(5) hollow hex nut 6 is closely interlocked with solid cylinder 7 by annular slot 12 and annular extension 13;
(6) module 4 is accepted by metallic gasket 1, sealing and hollow hex nut 6 seals whole sample cell, use spanner Apply 20N power, to ensure suitable sealing;
(7) whole sample cell is taken out, weighs average three times again, front and rear average value twice, which subtracts each other, obtains sample matter Amount;
(8) thermometer-heating unit is fixed to cylinder trap 3, thermocouple junction is fixed to thermocouple sheath 5;
(9) sample cell is fixed in calorimeter assembly with the rope by hanging hole 8;
(10) after connecting other wiring of calorimeter assembly or plug wire, thermal capacitance test is started;
(11) after experiment terminates, sample cell is removed, then remove thermometer-heating unit and thermocouple;
(12) open sample cell, take out sample, with absolute ethyl alcohol and deionized water cleaning sample pond all parts in case under Secondary measurement.
The above embodiments merely illustrate the technical concept and features of the present invention, and its object is to allow person skilled in the art Scholar can understand present disclosure and implement according to this, and it is not intended to limit the scope of the present invention.It is all according to the present invention The equivalent change or modification that Spirit Essence is made, it should all be included within the scope of the present invention.

Claims (10)

1. a kind of vary convenient and good airproof performance calorimeter sample cell, it is characterised in that including:
Module (4), thermocouple sheath (5), hollow six are accepted in metallic gasket (1), sample tank main body (2), cylinder trap (3), sealing Angle nut (6), solid cylinder (7);
The sample tank main body (2) is cylindrical tube, including upper lid (15) and bottom (14), sample tank main body (2) bottom Portion center sets a cylinder trap (3) for going deep into cylinder, and sample tank main body (2) top sets sealing to accept module (4);
Thermocouple sheath (5) quantity is two, is symmetrically welded at sample tank main body (2) side;
Hole sets inside annular slot (12) on the hollow hex nut (6);
Solid cylinder (7) top sets hanging hole (8), and for hanging sample cell, solid cylinder (7) bottom is set The annular extension (13) to be interlocked with annular slot (12);
It is described sealing accept module (4) be lower section be regular hexagon (9), middle part be the screwed main body in outer surface (10), top is furnished with the hollow cylinder of the edge of a knife (11);Module (4) complexed metal pad (1) and hollow hexagonal are accepted in the sealing Nut (6) is threadedly coupled.
2. sample cell according to claim 1, it is characterised in that metallic gasket (1) material is Mohs' hardness 2-3's Metal or alloy.
3. sample cell according to claim 1, it is characterised in that the metallic gasket (1) for circle, thickness 0.1~ 2mm, 4~10mm of diameter.
4. sample cell according to claim 1, it is characterised in that sample tank main body (2) length is 40~80mm, outside 10~40mm of footpath, 0.5~5mm of thickness;The bottom (14) is 10~40mm of external diameter, 3~15mm of internal diameter, 0.5~5mm's of thickness Annulus;The upper lid (15) be 10~40mm of external diameter, and inner hole section is the annulus of 2~10mm of length of side regular hexagon, its thickness 0.5~5mm;0.1~1mm of thickness of coating inside and outside the sample tank main body (2).
5. sample cell according to claim 1, it is characterised in that the cylinder trap (3) is by identical with sample tank main body (2) Material be made, top seal, bottom opening;The cylinder trap 3~15mm of diameter, 20~50mm of length.
6. sample cell according to claim 1, it is characterised in that the thermocouple sheath (5) is cylinder, is symmetrically welded In sample tank main body (2) side;Thermocouple sheath (5) 5~25mm of length, 0.5~3mm of external diameter, thickness 0.05~ 0.5mm。
7. sample cell according to claim 1, it is characterised in that hollow hex nut (6) 2~10mm of thickness, side Long 2~10mm, nut 4~10mm of internal diameter, pitch 1~2.5mm, annular slot (12) 0.5~3mm of thickness, internal diameter 3~ 8mm。
8. sample cell according to claim 1, it is characterised in that the solid cylinder (7) and hollow hex nut (6) It is manufactured from the same material;Solid cylinder (7) 5~15mm of length, diameter 3~8mm, hanging hole (8) 1~3mm of diameter, Annular extension (13) 0.5~3mm of thickness, 4~10mm of external diameter.
9. sample cell according to claim 1, it is characterised in that the sealing accepts module (4) and is and sample tank main body (2) hollow cylinder made of identical material.
10. sample cell according to claim 1, it is characterised in that described sealing undertaking module (4) inner hollow diameter 3~ 8mm;2~the 10mm of the length of side, 2~8mm of thickness of the regular hexagon (9);Main body (10) 4~10mm of external diameter, pitch 1~ 2.5mm, 5~15mm of length;The edge of a knife (11) 0.5~3mm of length, 30 °~60 ° of inclination angle.
CN201711327071.2A 2017-12-13 2017-12-13 Calorimeter sample cell convenient to replace and good in sealing performance Active CN107884437B (en)

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Cited By (5)

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Publication number Priority date Publication date Assignee Title
CN110871982A (en) * 2018-09-03 2020-03-10 中国科学院大连化学物理研究所 High temperature calorimeter sample deposits and remove device
CN113514489A (en) * 2020-04-09 2021-10-19 中国科学院大连化学物理研究所 Small sample amount sample pool in medium temperature area
CN113624802A (en) * 2020-05-07 2021-11-09 中国科学院大连化学物理研究所 Calorimeter sample pool for specific heat determination of chemical raw materials
CN114062413A (en) * 2020-08-04 2022-02-18 中国科学院大连化学物理研究所 Sample packaging mode for measuring heat capacity
CN114594125A (en) * 2020-12-07 2022-06-07 中国科学院大连化学物理研究所 High-temperature-resistant and good-sealing-performance solid-liquid dual-purpose sample pool

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Publication number Priority date Publication date Assignee Title
CN110871982A (en) * 2018-09-03 2020-03-10 中国科学院大连化学物理研究所 High temperature calorimeter sample deposits and remove device
CN110871982B (en) * 2018-09-03 2021-01-26 中国科学院大连化学物理研究所 High temperature calorimeter sample deposits and remove device
CN113514489A (en) * 2020-04-09 2021-10-19 中国科学院大连化学物理研究所 Small sample amount sample pool in medium temperature area
CN113624802A (en) * 2020-05-07 2021-11-09 中国科学院大连化学物理研究所 Calorimeter sample pool for specific heat determination of chemical raw materials
CN114062413A (en) * 2020-08-04 2022-02-18 中国科学院大连化学物理研究所 Sample packaging mode for measuring heat capacity
CN114594125A (en) * 2020-12-07 2022-06-07 中国科学院大连化学物理研究所 High-temperature-resistant and good-sealing-performance solid-liquid dual-purpose sample pool

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