CN115639238A - Multi-sample cell suspended and high-temperature-resistant fusing electrode device - Google Patents
Multi-sample cell suspended and high-temperature-resistant fusing electrode device Download PDFInfo
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- CN115639238A CN115639238A CN202110811237.8A CN202110811237A CN115639238A CN 115639238 A CN115639238 A CN 115639238A CN 202110811237 A CN202110811237 A CN 202110811237A CN 115639238 A CN115639238 A CN 115639238A
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Abstract
The invention relates to the field of calorimetric devices, in particular to a multi-sample-cell suspended and high-temperature-resistant fused electrode device which comprises an electrode plug, an electrode rod assembly and a sample cell, wherein the electrode plug comprises electrode columns, electrode caps and electrode sleeves, each electrode column is arranged in each electrode sleeve, each electrode cap is arranged at the upper end of each electrode sleeve, the upper ends of the electrode columns penetrate through the electrode sleeves and then expose parts form electrode joints, each electrode rod assembly comprises a plurality of electrode rods, the lower ends of the electrode columns are connected with the corresponding electrode rods, the electrode rods with the same length form a group of electrode rod groups, and the sample cell is suspended at the lower ends of the corresponding electrode rod groups through fuse wires. The invention can simultaneously hang a plurality of sample tanks, realize the quick and convenient replacement of the sample tanks in the high-temperature furnace, greatly improve the experimental efficiency and can work at the high temperature of 1800K to the maximum.
Description
Technical Field
The invention relates to the field of calorimetric devices, in particular to a fusing electrode device which is hung on a plurality of sample cells and is resistant to high temperature.
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 a substance, basic thermodynamic data such as substance enthalpy, entropy and Gibbs free energy can be obtained through accurate measurement of the heat capacity, and then the structure and phase change of the substance are known, and in addition, the method is also a method for obtaining crystal lattice vibration and electron energy level transition of a microstructure of the substance and understanding superconducting phenomena, magnetic action mechanisms and structural distortion. Therefore, obtaining accurate data of the high-temperature heat capacity of the substance has important significance for exploring and designing new materials, optimizing the preparation process of the materials, promoting the understanding and development of the science of the substance and the like.
Drop-in type calorimetry is one of the most accurate and reliable methods for measuring heat capacity of a substance at high temperature, however, the method has the defects of long test time consumption, high temperature, trouble in sample exchange, inconvenience in sample drop, need of certain professional knowledge for an operator and the like, and the defects limit the development and the use of the method, so that a drop-in type calorimetry device which is concise in development and control, convenient in sample exchange, stable in performance, high and wide in working temperature region and high in accuracy is particularly important, and one of the most critical links lies in the optimization of a sample pool drop-in method and structure, so that the drop-in type calorimetry device has good stability, can realize rapid sample drop and convenient replacement of a sample pool, and can ensure that a fusing electrode can be repeatedly used for a long time in a high-temperature environment.
At present, internationally, the representative high temperature calorimetric system in the formula high temperature calorimetric research field includes ice calorimeters, water calorimeters and copper billet calorimeters, however, these several kinds of formula high temperature calorimetric device's fusing electrode can only hang a sample cell at every turn, will cool down again after the experiment at every turn, heat up, the troublesome poeration, low efficiency, and repeatability under the high temperature, the reliability is relatively poor, be unfavorable for controlling the experiment time under the higher temperature environment, open the bell for a long time also leads to heat leak great, furnace easily receives the quench influence, reduce the instrument precision, these three kinds of calorimetric device's fusing electrode highest temperature all is no longer than 1000K in addition, seriously influence its application.
Disclosure of Invention
The invention aims to provide a multi-sample cell hanging and high-temperature-resistant fusing electrode device, which can be used for hanging a plurality of sample cells simultaneously, realizing the quick and convenient replacement of the sample cells in a high-temperature furnace, greatly improving the experimental efficiency, working at the high temperature of 1800K at most, effectively ensuring the precision of a falling tube calorimeter and conveniently positioning the sample cells at the central position in the tube high-temperature furnace.
The purpose of the invention is realized by the following technical scheme:
the utility model provides a hang a plurality of sample cell and high temperature resistance fusing electrode device, includes electrode stopper, electrode rod subassembly and sample cell, and wherein the electrode stopper includes electrode column, electrode cap and electrode sleeve, and in the electrode sleeve was all located to each electrode column, the electrode cap was located the electrode sleeve upper end, and passed on the electrode column the part that exposes behind the electrode sleeve formed electrode joint, the electrode rod subassembly includes a plurality of electrode rods, just the electrode column lower extreme is connected with the electrode rod that corresponds, and the electrode rod that length is the same forms a set of electrode rod group, and the sample cell hangs in the electrode rod group lower extreme that corresponds through the fuse.
And the electrode sleeve and the electrode cap are respectively provided with a through hole for the electrode column to pass through, and the outer side of the electrode column is wrapped by an insulating ceramic layer.
And the exposed metal on the top of the electrode column forms an electrode joint.
The lower end of the electrode column forms a first connecting end, the upper end of the electrode rod forms a second connecting end, and the first connecting end is in threaded connection with the corresponding second connecting end.
The first connecting end is an internal thread end with an internal thread hole, and the second connecting end is an external thread column end.
Clamping grooves are formed in two sides of the electrode cap.
Seen along the axial direction of the electrode columns, the electrode columns are uniformly distributed along the circumferential direction, and the two electrode rods belonging to the same electrode rod group are symmetrically arranged.
The lower ends of the electrode rods are provided with hooks, two ends of the fuse wire are respectively hung on the hooks corresponding to the lower ends of different electrode rods in the electrode rod group, and the upper end of the sample cell is provided with a hanging ring hung on the fuse wire.
Each sample cell is arranged in sequence along the vertical direction.
During testing, the electrode sleeve is in butt joint and insertion with a furnace mouth of the tubular high-temperature furnace.
The invention has the advantages and positive effects that:
1. the fuse wire and the electrode rod groups are designed to realize the suspension of the plurality of sample pools, the fuse wire can be fused at any time by controlling the electrode posts and the electrode rods to be electrified, and the sample pools fall under the action of gravity, so that the sample pools in the high-temperature furnace are replaced more simply and quickly, the experimental efficiency is effectively improved, and the controllability is more flexible.
2. The electrode column and the electrode bar are matched for use, so that a furnace mouth of the tubular high-temperature furnace can be effectively blocked, a large amount of heat leakage in the furnace is avoided, and each part is made of high-temperature-resistant materials, so that the electrode column can be fused and dropped in a 1800K high-temperature environment.
3. The electrode column and the electrode rod are wrapped by the insulating ceramic layer to realize effective insulation, and the lower end of the electrode column is in threaded connection with the upper end of the corresponding electrode rod, so that the electrode rod is convenient to replace.
4. The invention has simple combination and convenient disassembly, and simultaneously avoids the direct contact of the sample cell and other parts in the high-temperature furnace.
Drawings
Figure 1 is a schematic view of the overall structure of the present invention,
figure 2 is a schematic view of the electrode plug structure of figure 1,
fig. 3 is a schematic view of the electrode rod and the sample cell in fig. 1.
Wherein, 1 is an electrode plug, 101 is an electrode column, 1011 is an electrode joint, 1012 is a first connecting end, 102 is an electrode cap, 1021 is a clamping groove, 103 is an electrode sleeve, 2 is an electrode rod, 201 is a first electrode rod group, 202 is a second electrode rod group, 203 is a third electrode rod group, 204 is a second connecting end, 205 is a hook, 3 is a sample cell, and 301 is a fuse.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings.
As shown in fig. 1 to 3, the present invention includes an electrode plug 1, an electrode rod assembly and a sample cell 3, wherein the electrode plug 1 includes an electrode column 101, an electrode cap 102 and an electrode sleeve 103, each electrode column 101 is disposed in the electrode sleeve 103, the electrode cap 102 is disposed at the upper end of the electrode sleeve 103, and the exposed portion of the upper end of the electrode column 101 passing through the electrode sleeve 103 forms an electrode joint 1011, the electrode rod assembly includes a plurality of electrode rods 2, the lower end of the electrode column 101 is connected with the corresponding electrode rod 2, the electrode rods 2 with the same length form a group of electrode rod assemblies, and the sample cell 3 is suspended at the lower end of the corresponding electrode rod assembly through a fusible link 301.
In this embodiment, the electrode column 101 is made of a high temperature resistant metal bar, through holes for the electrode column 101 to pass through are formed in the electrode sleeve 103 and the electrode cap 102, an insulating ceramic layer is wrapped on the outer side of the electrode column 101 and contacts with the electrode sleeve 103 and the electrode cap 102, and an electrode joint 1011 is formed on the top of the electrode column 101 by exposed metal.
As shown in fig. 1 to 3, a first connection end 1012 is formed at the lower end of the electrode column 101, a second connection end 204 is formed at the upper end of the electrode rod 2, and the first connection end 1012 is in threaded connection with the corresponding second connection end 204, in this embodiment, the first connection end 1012 is an internal thread end having an internal thread hole therein, and the second connection end 204 is an external thread column end.
As shown in fig. 2, two sides of the electrode cap 102 are provided with a clamping groove 1021 for fixing the electrode plug 1, the electrode sleeve 103 is of a metal tubular structure, and the upper end of the electrode sleeve is hermetically welded with the electrode cap 102, so that the electrode column 101 can be protected, and the electrode sleeve can be in dynamic sealing with a furnace mouth of a high-temperature furnace.
As shown in fig. 3, in the present embodiment, the electrode assembly includes six electrode rods 2, the shortest two electrode rods 2 form a first electrode rod group 201, the middle two electrode rods 2 form a second electrode rod group 202, the longest two electrode rods 2 form a third electrode rod group 203, the present embodiment includes three sample cells 3 sequentially arranged from top to bottom, and the uppermost sample cell 3 is hung at the lower end of the first electrode rod group 201, the middle sample cell 3 is hung at the lower end of the second electrode rod group 202, and the lowermost sample cell 3 is hung at the lower end of the third electrode rod group 203.
As shown in fig. 3, in this embodiment, the lower end of the electrode rod 2 is provided with a hook 205, two ends of the fuse 301 are respectively hung on the hooks 205 at the lower ends of different electrode rods in the corresponding electrode rod group, and the upper end of the sample cell 3 is provided with a hanging ring hung on the fuse 301.
Seen along the axial direction of the electrode columns 101, the electrode columns 101 are uniformly distributed along the circumferential direction, two electrode rods 2 belonging to the same electrode rod group are symmetrically arranged, and six electrode rods 2 in the embodiment are uniformly distributed along the circumferential direction to form a regular hexagon.
The number of the electrode rods 2 can be set according to actual requirements.
In this embodiment, the electrode cap 102 is made of nickel-based alloy material by turning, the diameter is 30-80 mm, the height is 20-50 mm, 6 holes are formed in the middle and penetrate through the electrode cap 102, the hole diameter is 1-5 mm, and two clamping grooves 1021 are respectively turned on two sides.
In this embodiment, the electrode column 101 is a tungsten wire wrapped by insulating ceramic, the outer diameter of the electrode column 101 is 1 to 5mm, and the inner diameter of the threaded hole at the first connection end 1012 at the lower side of the electrode column 101 is 0.8 to 4.8mm, and the length is 100 to 500mm.
In this embodiment, the electrode column 101 is a tubular structure formed by lathing a nickel-based alloy material, and the electrode column 101 has an inner diameter of 20-70 mm, an outer diameter of 25-75 mm, and a height of 90-400 mm.
In this embodiment, the electrode rods 2 are ceramic-wrapped tungsten wire structures, and have an outer diameter of 0.8-4.8 mm, wherein the shortest first electrode rod group 201 has a length of 100-200 mm, the middle second electrode rod group 202 has a length of 150-250 mm, the longest third electrode rod group 203 has a length of 250-300 mm, and the outer thread diameter of the second connection end 204 on the upper side of the electrode rod 2 is 0.8-4.8 mm.
In this embodiment, the fuse 301 is made of nickel wire with a purity of 99.9%, the wire diameter of the fuse 301 is 0.1-0.5 mm, the length of the fuse 301 is 50-150 mm, and two ends of the fuse 301 are respectively formed by bending into a circle and are hung on the hook 205 corresponding to the lower end of the electric rod 2.
In this embodiment, the sample cell 3 is a hollow bottle made of a nickel-based alloy material, the inner diameter of the sample cell is 10-15 mm, the outer diameter of the sample cell is 15-20 mm, the height of the sample cell is 40-60 mm, the sample cell 3 is located at the center of the fusing electrode and is arranged up, down, and the vertical direction interval between the sample cells 3 is 5-10 mm.
The working principle of the invention is as follows:
the drop-in calorimeter heats a sample cell 3 in a high-temperature furnace at a high temperature, when the temperature reaches a set temperature, 24V direct current is introduced into an electrode column 101 and an electrode rod 2, so that a fuse wire 301 is sequentially fused from bottom to top, the sample cell 3 is sequentially dropped into the calorimeter from bottom to top under the action of gravity, and then data acquisition and high-temperature specific heat measurement are carried out, so that the drop-in calorimeter is one of indispensable important components in the design of the drop-in calorimeter.
The invention specifically adopts the following steps to load and unload the sample cell 3 to measure the temperature of the substance:
(1) The second connecting end 204 at the top end of the electrode rod 2 is connected with the first connecting end 1012 at the lower end of the electrode column 101 by screw threads, and in this embodiment, the electrode rods 2 constituting the first electrode rod group 201, the second electrode rod group 202 and the third electrode rod group 203 are uniformly distributed in a regular hexagon along the axial direction, and the two electrode rods 2 of the same electrode rod group are arranged in a diagonal direction.
(2) The electrode clamping groove 1021 is fixed with the lifting frame of the high-temperature furnace, so that the whole body of the electrode clamping groove 1021 is vertical to the horizontal plane.
(3) Washing the inside and the outside of the sample cell 3 with absolute ethyl alcohol three times respectively, and then washing with deionized water three times;
(4) Drying and drying each part of the sample pool 3, cooling to room temperature, weighing for three times, and taking an average value;
(5) Putting the sample into a sample cell 3, weighing for three times, and taking an average value;
(6) The fuse wire 301 passes through a hanging ring at the top of the sample pool 3;
(7) Respectively hanging two ends of a fuse wire 301 on hooks 205 at the lower ends of corresponding electrode rods 2 to finish the suspension of the sample cell 3, wherein the sample cells 3 are suspended sequentially from top to bottom;
(8) The invention with the suspended sample pool 3 is slowly put into a tubular high-temperature furnace of a drop-in high-temperature calorimeter by a lifting frame, wherein an electrode sleeve 103 is plugged into a furnace mouth, and the electrode cap 102 and the part of the electrode joint 1011 above the electrode cap are exposed;
(9) Respectively clamping electrode clamps connected with a direct-current power supply on the corresponding electrode connectors 101, so that the two electrode connectors 101 corresponding to each electrode group are electrified, and the electrified electrode clamps are not divided into positive and negative electrodes;
(10) Opening the tubular high-temperature furnace to start testing, controlling to close a direct-current power switch when the temperature reaches a set value, and sequentially fusing the fusible links 301, so that the sample pool 3 sequentially falls from bottom to top;
(11) After the sample is dropped, closing the tubular high-temperature furnace, and taking away the six electrode clamps when the temperature in the furnace is reduced to within 200 ℃, and lifting the electrode clamps;
(12) After the temperature is cooled to room temperature, the residual silk left on the hook 205 is cleaned, and the hook can be continuously used next time.
The invention can meet the requirements of the falling-in high-temperature calorimeter on temperature, accuracy, good repeatability and the like, can realize the high-efficiency experiment of measuring the temperature rise of the furnace body for three times at one time, avoids the repeated temperature reduction and rise processes of the furnace body, and still has good functionality at the high temperature of 1800K.
Claims (10)
1. The utility model provides a hang a plurality of sample cell and high temperature resistance fusing electrode device which characterized in that: including electrode stopper (1), electrode rod subassembly and sample cell (3), wherein electrode stopper (1) includes electrode column (101), electrode cap (102) and electrode sleeve (103), and electrode sleeve (103) are all located in each electrode column (101), and electrode cap (102) are located electrode sleeve (103) upper end, and pass on electrode column (101) the part that exposes behind electrode sleeve (103) forms electrode joint (1011), the electrode rod subassembly includes a plurality of electrode rod (2), just electrode column (101) lower extreme is connected with electrode rod (2) that correspond, and electrode rod (2) that length is the same form a set of electrode rod group, and sample cell (3) hang in the electrode rod group lower extreme that corresponds through fuse (301).
2. The high temperature resistant fused electrode device for suspending a plurality of sample cells according to claim 1, wherein: the electrode sleeve (103) and the electrode cap (102) are both provided with through holes for the electrode column (101) to pass through, and the outer side of the electrode column (101) is wrapped with an insulating ceramic layer.
3. The apparatus of claim 1, wherein the apparatus further comprises: the bare metal on the top of the electrode column (101) forms an electrode joint (1011).
4. The apparatus of claim 1, wherein the apparatus further comprises: the lower end of the electrode column (101) forms a first connecting end (1012), the upper end of the electrode rod (2) forms a second connecting end (204), and the first connecting end (1012) is in threaded connection with the corresponding second connecting end (204).
5. The apparatus of claim 4, wherein the apparatus further comprises: the first connecting end (1012) is an internal thread end with an internal thread hole, and the second connecting end (204) is an external thread column end.
6. The apparatus of claim 1, wherein the apparatus further comprises: clamping grooves (1021) are formed in two sides of the electrode cap (102).
7. The apparatus of claim 1, wherein the apparatus further comprises: seen along the axial direction of the electrode columns (101), the electrode columns (101) are uniformly distributed along the circumferential direction, and the two electrode rods (2) belonging to the same electrode rod group are symmetrically arranged.
8. The apparatus of claim 1, wherein the apparatus further comprises: the lower end of the electrode rod (2) is provided with a hook (205), two ends of the fuse wire (301) are respectively hung on the hooks (205) corresponding to the lower ends of different electrode rods in the electrode rod group, and the upper end of the sample cell (3) is provided with a hanging ring hung on the fuse wire (301).
9. The apparatus of claim 1, wherein the apparatus further comprises: the sample cells (3) are arranged in sequence along the vertical direction.
10. The apparatus of claim 1, wherein the apparatus further comprises: during testing, the electrode sleeve (103) is in butt joint and plug-in mounting with a furnace mouth of the tubular high-temperature furnace.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110811237.8A CN115639238A (en) | 2021-07-19 | 2021-07-19 | Multi-sample cell suspended and high-temperature-resistant fusing electrode device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110811237.8A CN115639238A (en) | 2021-07-19 | 2021-07-19 | Multi-sample cell suspended and high-temperature-resistant fusing electrode device |
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| Publication Number | Publication Date |
|---|---|
| CN115639238A true CN115639238A (en) | 2023-01-24 |
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| CN202110811237.8A Pending CN115639238A (en) | 2021-07-19 | 2021-07-19 | Multi-sample cell suspended and high-temperature-resistant fusing electrode device |
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- 2021-07-19 CN CN202110811237.8A patent/CN115639238A/en active Pending
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