阅读说明：本技术 一种高温量热计样品存放及取出装置 (High temperature calorimeter sample deposits and remove device ) 是由 史全 吴冰 于 2018-09-03 设计创作，主要内容包括：本发明涉及量热学中的量热装置,特别涉及一种高温量热计样品存放及取出装置。包括用于存放样品的样品池和用于抓取样品池的坩埚钳,其中坩埚钳包括坩埚钳钳芯及套设于坩埚钳钳芯外侧的钳芯套管模块,坩埚钳钳芯和钳芯套管模块沿轴向可相对移动,坩埚钳钳芯的一端设有用于抓取样品池的坩埚钳钳爪；样品池包括样品池主体及用于密封样品池主体的样品池瓶盖,样品池瓶盖的顶部设有用于坩埚钳抓取的抓取部。本发明中样品池的结构紧凑,设计精细,从而使得样品池内样品在100MPa的内外压差下,也不会发生泄漏,具备优异的密封性；本发明通过坩埚钳对样品池的装卸,操作者可以方便的更换样品。(The invention relates to a calorimetric device in calorimetric science, in particular to a sample storage and taking device of a high-temperature calorimeter. The crucible tongs comprise a crucible tong core and a tong core sleeve module sleeved outside the crucible tong core, wherein the crucible tong core and the tong core sleeve module can move relatively along the axial direction, and one end of the crucible tong core is provided with a crucible tong claw for grabbing the sample cell; the sample cell comprises a sample cell main body and a sample cell bottle cap used for sealing the sample cell main body, and the top of the sample cell bottle cap is provided with a grabbing part used for grabbing the crucible tongs. The sample cell has compact structure and fine design, so that the sample in the sample cell can not leak under the internal and external pressure difference of 100MPa, and has excellent sealing property; according to the invention, the sample cell is assembled and disassembled through the crucible tongs, so that an operator can conveniently replace the sample.)

1. The utility model provides a high temperature calorimeter sample is deposited and remove device, its characterized in that, including the sample cell that is used for depositing the sample with be used for snatching the crucible tongs of sample cell, wherein the crucible tongs include crucible tongs core (10) and cover locate the pincers core sleeve pipe module in crucible tongs core (10) outside, crucible tongs core (10) with pincers core sleeve pipe module is along axial relative movement, the one end of crucible tongs core (10) is equipped with and is used for snatching crucible tongs claw (12) of sample cell.

2. The high-temperature calorimeter sample storage and removal device according to claim 1, wherein the sample cell comprises a sample cell body (1) and a sample cell cover (3) for sealing the sample cell body (1), and a gripping portion for gripping the crucible tongs is arranged at the top of the sample cell cover (3).

3. The high temperature calorimeter sample storage and removal device of claim 2, wherein the gripping portion is a cylinder with a snap on outer surface.

4. The high temperature calorimeter sample storage and removal device of claim 3, wherein the catch is an annular protrusion coaxial with the cylinder.

5. A high temperature calorimeter sample storage and withdrawal device according to claim 3, wherein the upper end of the cylindrical body is penetrated radially by a hanging hole (5).

6. The high-temperature calorimeter sample storage and extraction device according to claim 2, wherein the sample cell main body (1) is a hollow cylinder, a sealing receiving bottle mouth (2) for being in threaded connection with the sample cell bottle cap (3) is arranged at the end part of the sample cell main body (1), and a sealing chamfering knife edge (7) is arranged on the end surface of the sealing receiving bottle mouth (2).

7. The high-temperature calorimeter sample storage and extraction device according to claim 1, wherein the crucible tong core (10) is a cylinder with a hollow structure, a tong claw engagement module (11) is embedded at one end of the crucible tong core (10), the connecting end of the crucible tong claw (12) is located between the crucible tong core (10) and the tong claw engagement module (11) and is fixed by the tong claw engagement module (11), and the outer surface of the other end of the crucible tong core (10) is provided with stripes to form a tong core handle (9).

8. The high-temperature calorimeter sample storage and extraction device according to claim 1, wherein the jaw sleeve module comprises a jaw sleeve (15) and a jaw sleeve opening (18), the jaw sleeve opening (18) is arranged at one end of the jaw sleeve (15) and has a diameter larger than that of the jaw sleeve (15), the jaw sleeve opening (18) is used for accommodating the crucible jaw (12), and the other end of the jaw sleeve (15) is provided with a jaw handle (14).

9. The high temperature calorimeter sample storage and removal device of claim 8, wherein the clamp core sleeve (15) is provided with a sleeve engagement module (16) at one end, and the end of the jaw socket (18) is provided with a sleeve chuck (17) in threaded connection with the sleeve engagement module (16).

10. The high temperature calorimeter sample storage and removal device of claim 1, wherein the sample cell is made of stainless steel alloy material, the crucible tongs core (10) is made of stainless steel material, the tongs core sleeve (15) is made of copper material, and the crucible tongs jaws (12) are made of stainless steel wire.

Technical Field

The invention relates to a calorimetric device in calorimetric science, in particular to a sample storage and taking device of a high-temperature calorimeter.

Background

The heat capacity is the sum of energy contributions of movement forms such as crystal lattices and electrons in a substance system, and is a basic thermophysical parameter of the substance. Through accurate measurement of heat capacity, basic thermodynamic data such as substance enthalpy, entropy, Gibbs free energy and the like can be obtained, the structure and phase change of a substance are known, and the method is also a method for obtaining lattice vibration and electronic energy level transition of a substance microstructure and understanding a superconducting phenomenon, a magnetic action mechanism and structural distortion. Therefore, the accurate data of the heat capacity of the substance is obtained, and the method has important significance for exploring and designing new materials, optimizing the preparation process of the materials and promoting the understanding and development of the science of the substance.

Adiabatic calorimetry is one of the most accurate and reliable methods for measuring the heat capacity of a substance, however, the development and use of the adiabatic calorimetry are limited due to the defects of time consumption, trouble in sample exchange, low and narrow working temperature region, certain professional knowledge required by an operator and the like, so that the adiabatic calorimetry device is particularly important for developing and controlling the adiabatic calorimetry device with simplicity, convenience in sample exchange, stable performance, high and wide working temperature region and high accuracy. The most critical link lies in the optimization of the structure of the sample pool, so that the sample pool has reliable sealing performance, the sample can be quickly and conveniently replaced, and meanwhile, the calorimeter is ensured to have high accuracy and precision in a high and wide temperature region.

Representative calorimetric systems currently in The field of adiabatic thermal research internationally include The 300- ­ 1300K temperature zone apparatus established by Sorai at osaka university, japan (m.sorai, k.kaji, y.kaneko.an automated adiabatic calorimeter for The thermal range 300K to 1300K The heat capacities from 300K to 1300K and synthetic sapphire from 600to1500 k.j.chem.thermodyne.1992, 24, 167-); 300-1500K temperature zone devices established by Atake, Tokyo university of industry, Japan (T.tanaka, T.Atake, H.Nakayama, T.Eguchi, K.Saito, I.Ikemoto.Heatcacity and an incommensurate phase transition of crystalline bis (4-chlorophenyl) sulfuric acid. J.chem.Thermodyn.1994, 26, 1231-1239.); the 100-inch 1500K temperature zone device established by Van Miltenburg, university of Uadenle, the Netherlands (J.C. Van Miltenburg, G.J.K.Van Den Berg, M.J.Van Bommel.Construction of an adhesive sealant meters of the adhesive heat capacity of synthetic sapphire and of n-helium.J.chem.Thermodyn, 1987,19, 1129-inch 1137). However, the sample cells of the first two adiabatic calorimetric devices are sealed by cutting off the capillary tube, and the method is complex to operate and poor in repeatability and reliability; the instrument of the university of uderlan is troublesome to change samples, and the sample cell is tightly connected with the heat insulation screen, which is not beneficial to controlling heat leakage and influences the precision of the instrument. Meanwhile, the maximum temperature of the three calorimeters is not more than 1000K, which seriously influences the application of the calorimeters.

Therefore, there is an urgent need to develop a sample cell of an adiabatic calorimeter with compact structure, excellent performance, novel design and high temperature region to meet the urgent need of the heat capacity property research of the condensed substance.

Disclosure of Invention

Aiming at the defects of the existing adiabatic heat measuring device, the invention aims to provide a sample storage and taking-out device of a high-temperature heat meter, and aims to solve the problems that the existing heat device is complex in operation, poor in repeatability and reliability, and troublesome in sample change, a sample cell is tightly connected with an adiabatic screen, heat leakage is not easy to control, and instrument precision is affected.

In order to achieve the purpose, the invention adopts the following technical scheme:

the utility model provides a high temperature calorimeter sample deposits and remove device, is including the sample cell that is used for depositing the sample and be used for snatching the crucible pincers of sample cell, wherein the crucible pincers include crucible pincers core and cover locate the pincers core sleeve pipe module in the crucible pincers core outside, the crucible pincers core with pincers core sleeve pipe module is along axial relative movement, the one end of crucible pincers core is equipped with and is used for snatching the crucible pincers claw of sample cell.

The sample cell comprises a sample cell main body and a sample cell bottle cap used for sealing the sample cell main body, wherein the top of the sample cell bottle cap is provided with a grabbing part used for grabbing the crucible tongs.

The grabbing part is a cylinder with a buckle on the outer surface.

The buckle is an annular bulge coaxial with the cylinder.

The upper end of the cylinder is provided with a hanging hole along the radial direction.

The sample cell comprises a sample cell body and is characterized in that the sample cell body is a hollow cylinder, a sealed receiving bottle opening in threaded connection with a sample cell bottle cap is arranged at the end part of the sample cell body, and a sealed chamfer cutter edge is arranged on the end face of the sealed receiving bottle opening.

The crucible tongs core is hollow cylinder, crucible tongs core one end is inlayed and is equipped with claw linking module, the link of crucible tongs claw is located the crucible tongs core with between the claw linking module, and it is fixed through claw linking module, the other end surface of crucible tongs core is equipped with the stripe, forms the pincers core handle.

The crucible clamp comprises a clamp core sleeve and a clamp claw sleeve, wherein the clamp claw sleeve comprises a clamp core sleeve and a clamp claw cover opening, the clamp claw cover opening is arranged at one end of the clamp core sleeve, the diameter of the clamp claw cover opening is larger than that of the clamp core sleeve, the clamp claw cover opening is used for containing a crucible clamp claw, and a clamp sleeve handle is arranged at the other end of the clamp core sleeve.

The clamp comprises a clamp core sleeve, a clamp claw sleeve opening, a clamp claw sleeve and a clamp claw sleeve, wherein a sleeve connecting module is arranged at one end of the clamp core sleeve, and a sleeve clamping head in threaded connection with the sleeve connecting module is arranged at the end of the clamp claw sleeve opening.

The sample pool is made of stainless steel alloy materials, the crucible tongs core is made of stainless steel materials, the tongs core sleeve is made of copper materials, and the crucible tongs jaws are made of stainless steel wires.

The invention has the advantages and beneficial effects that:

1. the sample cell has compact structure and fine design, so that the sample in the sample cell can not leak under the internal and external pressure difference of 100MPa, and has excellent sealing property;

2. according to the invention, the sample cell is assembled and disassembled through the crucible tongs, so that an operator can conveniently replace a sample;

3. according to the invention, because all parts are in close contact, the whole sample cell can keep good heat conduction, the temperature difference of all parts is not more than 0.05K, and heat capacity data with high accuracy and precision can be obtained;

4. the sample cell can work normally at the high temperature of 400K-1700K;

5. the sample pool is suspended and fixed in the whole calorimetric device by utilizing the hanging rope penetrating through the hanging hole;

6. the whole sample cell can be conveniently assembled and disassembled, and the abrasion between the sample cell and other parts of a calorimetric device is avoided.

Drawings

FIG. 1 is a schematic view of a sample cell according to the present invention;

FIG. 2 is a schematic structural view of a core of the crucible tongs of the present invention;

FIG. 3 is a schematic view of the structure of the crucible tongs sleeve of the present invention.

In the figure: 1. a sample cell body; 2. sealing and connecting the bottle mouth; 3. a sample cell bottle cap; 4. buckling; 5. a hanging hole; 6. the cylinder is buckled with the neck; 7. sealing the chamfer cutter edge; 8. a central hole of a crucible tongs core; 9. a clamp core handle; 10. a crucible tong core; 11. a jaw engagement module; 12. a crucible tong jaw; 13. a central hole of the clamp core sleeve; 14. the handle of the forceps sleeve; 15. a clamp core sleeve; 16. a casing joining module; 17 casing pipe clamping heads; 18. the jaw is sleeved.

Detailed Description

In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in detail with reference to the accompanying drawings and specific embodiments.

As shown in fig. 1-3, the sample storage and taking-out device for a high temperature calorimeter provided by the invention comprises a sample cell for storing a sample and a crucible clamp for grabbing the sample cell, wherein the crucible clamp comprises a crucible clamp core 10 and a clamp core sleeve module sleeved outside the crucible clamp core 10, the crucible clamp core 10 and the clamp core sleeve module can move relatively along the axial direction, and one end of the crucible clamp core 10 is provided with a crucible clamp claw 12 for grabbing the sample cell.

As shown in fig. 1, the sample cell comprises a sample cell body 1 and a sample cell cover 3 for sealing the sample cell body 1, and a grabbing part for grabbing the crucible tongs is arranged at the top of the sample cell cover 3.

The grabbing part is a cylinder with a buckle on the outer surface, and the buckle is an annular bulge coaxial with the cylinder and used for grabbing the crucible tongs jaw 12. The upper end of the cylinder is provided with a hanging hole 5 along the radial direction for hanging the sample cell.

Sample cell main part 1 is hollow cylinder, and sample cell main part 1's bottom is sealed, and the upper end is equipped with and is used for accepting bottleneck 2 with 3 threaded connection's of sample cell bottle lid sealed, and sealed bottleneck 2 of accepting is cylindric, and the outer circumference is the heliciform, can seal tightly with sample cell bottle lid 3. The top end of the sealing receiving bottle mouth 2 is a sealing chamfer cutter edge 7, so that the sealing property is improved;

the side of sample cell bottle lid 3 is for erectting the type screw thread, improves frictional force, and upper portion is solid cylinder buckle 4, and the lower part of buckle 4 is the cylinder that buckle 4 meets and detains neck 6, and crucible tongs claw 12 of being convenient for inserts, snatchs buckle 4.

As shown in fig. 2, the crucible tongs core 10 is a hollow cylinder, i.e. the cylinder is provided with a central hole 8 of the crucible tongs core, one end of the crucible tongs core 10 is embedded with a tong claw connection module 11, the connection end of the crucible tongs tong claw 12 is located between the crucible tongs core 10 and the tong claw connection module 11 and fixed by the tong claw connection module 11, and the outer surface of the other end of the crucible tongs core 10 is provided with stripes to form a tong core handle 9.

As shown in fig. 3, the jaw sleeve module includes a jaw sleeve 15 and a jaw pocket 18, the jaw pocket 18 is disposed at one end of the jaw sleeve 15 and has a diameter larger than that of the jaw sleeve 15, and the jaw pocket 18 is used for accommodating the crucible jaw 12. The other end of the clamp core sleeve 15 is provided with a clamp sleeve handle 14.

Furthermore, one end of the clamp core sleeve 15 is provided with a sleeve connection module 16, and the end of the jaw sleeve opening 18 is provided with a sleeve chuck 17 in threaded connection with the sleeve connection module 16.

The sample cell is made of stainless steel alloy materials, the crucible tong core 10 is made of stainless steel materials, the tong core sleeve 15 is made of copper materials, and the crucible tong claws 12 are made of stainless steel wires.

The adiabatic heat measuring device meets the requirement of heat insulation by eliminating heat exchange between the sample cell and the environment, so that accurate and reliable heat capacity data are obtained, and the structure of the sample cell is the most important factor in the design of the adiabatic heat measuring device. The sample pool of the high-temperature calorimeter, which is convenient to change samples and good in sealing performance, provided by the invention can meet the requirements of a heat insulation and measurement device on heat insulation, accuracy, good repeatability and the like, can realize quick and convenient replacement of a measurement sample, and still has good sealing performance at a high temperature of 400-1700K.