CN201425582Y - Differential thermal analysis device of intense magnetic field - Google Patents

Differential thermal analysis device of intense magnetic field Download PDF

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Publication number
CN201425582Y
CN201425582Y CN2009200694483U CN200920069448U CN201425582Y CN 201425582 Y CN201425582 Y CN 201425582Y CN 2009200694483 U CN2009200694483 U CN 2009200694483U CN 200920069448 U CN200920069448 U CN 200920069448U CN 201425582 Y CN201425582 Y CN 201425582Y
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China
Prior art keywords
heating furnace
differential thermal
thermal analysis
dta
sample
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Expired - Fee Related
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CN2009200694483U
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Chinese (zh)
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任忠鸣
李传军
任维丽
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University of Shanghai for Science and Technology
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University of Shanghai for Science and Technology
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Abstract

The utility model relates to a differential thermal analysis device of an intense magnetic field, which comprises a heating furnace. The heating furnace which is a resistance furnace is connected withthe differential thermal analysis device, the differential thermal analysis device which adopts a detachable structure is arranged in a heating furnace cavity, the heating furnace is connected with aprogram temperature controlling instrument, and the differential thermal analysis device is connected with a temperature collecting treatment system. The device can overcome some problems incurred inthe intense magnetic field, and can be used for measuring thermodynamic and dynamical parameters of materials when phase change is incurred on the materials in the intense magnetic field.

Description

High-intensity magnetic field differential thermal analysis (DTA) device
Technical field
The utility model relates to a kind of differential thermal analysis (DTA) device that uses under high-intensity magnetic field, belong to the expansion of thermoanalysis technology in the investigation of materials field.
Background technology
Two more than ten years in the past, along with the kicker magnet technical development is increasingly mature, high-intensity magnetic field is used more and more widely, and high-intensity magnetic field has attracted countries in the world scholar's keen interest to the influence of material preparation process.Many new phenomenons are found in the material preparation process under high-intensity magnetic field, and this makes high-intensity magnetic field become the new means and the method for a kind of control material tissue and performance.Magnetic field can produce many influences to the material preparation process, as, magnetothermal effect, magnetic aligning, magnetic separates, magnetic Archimedes effect etc.Wherein, in material preparation and process, tend to take place various forms of phase transformations, as, fusing is solidified, and separates out, crystallization etc. again.Measure the phase transition parameter under the various conditions under the magnetic field accurately to explaining particularly important that various phenomenons then show under the magnetic field.And differential thermal analysis is a kind of application thermoanalysis technology very widely under normal condition, has obtained significant progress and progress in its century in the past, and many research institutions have all bought commercial differential thermal analyzer and have been used to study various thermal phenomenons.Yet, up to the present, but still be not fit to the thermal-analysis instrumentation under the high-intensity magnetic field, cause the reason of this phenomenon to mainly contain the following aspects: (1) any material all is magnetic, under strong magnetic field action, though weak magnetic substance it all can be subjected to the magnetic force that can experience, the sample that is in the magnetic field often is moved because of stressed variation causes the position, thereby the differential thermal curve of acquisition is changed, be difficult to guarantee result's repeatability.(2) magnetic field is influential to the thermopair output potential, so the thermocouple output signal under the magnetic field must be calibrated.(3) the kicker magnet work space is limited, and the work space of kicker magnet all is a cylindrical cavity both at home and abroad at present, and diameter is generally several centimetres to tens centimetres scope, and traditional commercial thermal analyzer can not be applied under the high-intensity magnetic field.More than these reasons hindered the application of thermal-analysis instrumentation under high-intensity magnetic field.But, prepare this emerging field at electromagnetic material, and the help that needs thermal-analysis instrumentation is to explain and to understand much new phenomenon and results in the magnetic field under.Therefore, be necessary very much to design the apparatus for thermal analysis that is fit to use under the high-intensity magnetic field.
Summary of the invention
The purpose of this utility model provides a kind of high-intensity magnetic field differential thermal analysis (DTA) device, and it can overcome under the high-intensity magnetic field some problems that occur, the thermodynamics and kinetics parameter when being used to measure material and undergoing phase transition under magnetic field.
For achieving the above object, the technical solution adopted in the utility model is as follows:
A kind of high-intensity magnetic field differential thermal analysis (DTA) device, comprise a heating furnace, connect a differential thermal analysis (DTA) device, described heating furnace is a resistance furnace, described differential thermal analysis (DTA) device is placed in the heating furnace chamber with demountable structure, described heating furnace connects a programmed temperature control instrument, and described differential thermal analysis (DTA) device connects a temperature acquisition disposal system.
The structure of above-mentioned heating furnace is: a top has the gas outlet and the stainless steel boiler clothing of lower openings, the resistance wire calandria of coated outside asbestos is equipped with in its inside, and described resistance wire calandria connects described programmed temperature control instrument by the electrode that is installed in the heating furnace top.
The structure of above-mentioned differential thermal analysis (DTA) device is: a bracket base and described heating furnace lower openings coupling, described bracket base has air intake opening, fixedly mount a sample crucible and a reference crucible arranged side by side by supporting alundum tube above the bracket base, sample thermopair under the sample crucible is drawn from the bracket base bottom with the reference thermopair under the reference crucible and is connected described temperature acquisition disposal system, described support alundum tube side is installed a temperature-control heat couple and is drawn from the bracket base bottom, and connects described programmed temperature control instrument.
The said temperature acquisition processing system is that Keithley 2700 temperature collect modules connect a computing machine, and described sample thermopair is connected the input end of described Keithley2700 temperature collect module with the reference thermopair.
Above-mentioned sample crucible arranged side by side and reference crucible are placed in the sample cell, the structure of described sample cell is: the fixedly sleeved diplopore corundum cover in described support alundum tube top, settle sample crucible and reference crucible in its diplopore respectively, the top of described sample thermopair and reference thermopair contacts a platinum support that is placed in sample crucible and reference crucible respectively separately.
Above-mentioned demountable structure is: the top cover of described heating furnace and bottom flange have corresponding each two perforation, described bracket base also has perforation to aim at two perforation of heating furnace top cover and bottom flange, there are two stainless steel slide bars to pass the perforation on heating furnace top cover and the bottom flange and the perforation of bracket base, there is screw thread at these two slide bars two ends, after putting a depression bar, the upper end screws on nut, the lower end also screws on nut, bracket base is compressed by an O-ring seal connect heating furnace bottom flange.
Principle of work:
After sample is put into the sample crucible, cover the corundum lid, heating furnace descends along the stainless steel slide bar, and the sample cell of adorning sample is placed in the heating furnace, then integral body is put into cylinder kicker magnet chamber.The heating furnace electrode is linked to each other with the power lead of programmed temperature control instrument, and the reference thermopair is linked to each other with temperature collect module 2700 with the sample thermopair with compensation lead of thermocouple.Programmed temperature control instrument is by the temperature rate of temperature-control heat couple control heating furnace.Heating furnace in heating or cooling, the thermoelectrical potential of temperature acquisition partial record sample thermopair and reference thermopair, temperature collect module 2700 is a temperature signal with the thermoelectrical potential conversion of signals, machine collecting temperature data obtain differential thermal curve as calculated.
Might influence the problem of thermopair output potential at high-intensity magnetic field, pay special attention to the design of thermocouple location.According to the Nernst effect of thermopair output potential under the magnetic field, work as magnetic direction, when thermocouple wire direction and thermograde direction three are mutually perpendicular, magnetic field will influence the thermopair output potential.Therefore, three pairs of thermocouple wires of the present utility model all are installed in the diplopore alundum tube of vertical direction, and its direction is all parallel with magnetic direction, has so just avoided the influence of high-intensity magnetic field to the thermopair output potential.
Simultaneously, when the differential thermal analysis (DTA) device was in entering kicker magnet, sample might be subjected to magnetic force and occurrence positions moves even break away from the phenomenon of crucible, has designed close-fitting diplopore corundum cover, can obtain repeatability experimental result preferably like this.And the thermopair chieftain contacts well with platinum support 22, has guaranteed the sensitivity transmission of heat flow signal.
The utility model has following conspicuous substantive distinguishing features and advantage compared with prior art:
1. heating furnace, differential thermal analysis (DTA) device and temperature acquisition disposal system, programmed temperature control instrument is separated from each other, heating furnace, differential thermal analysis (DTA) device maximum outside diameter is consistent with the kicker magnet internal diameter, has adapted to the limited work space of high-intensity magnetic field.
2. heating furnace can move up and down along the stainless steel slide bar, has both helped changing sample, also can play positioning action, has guaranteed that heating furnace sealing back sample cell still is in same position in the heating furnace.
3. reference thermopair, sample thermopair and temperature-control heat couple, three pairs of thermocouple wires are all parallel with magnetic direction, avoided the influence of magnetic field to the thermopair output potential.
4. the corundum lid of band biconvex head can be stabilized in sample in the diplopore corundum cover, and sample moves because of being subjected to the magneticaction occurrence positions when having prevented like this that the differential thermal analysis (DTA) device from entering in the kicker magnet, even the phenomenon of disengaging crucible.
Description of drawings
Fig. 1 is the structural representation of an embodiment of the utility model
Fig. 2 is the sample pool structure synoptic diagram of Fig. 1 example
Embodiment
Preferred embodiment accompanying drawings of the utility model is as follows:
As shown in Figure 1, this high-intensity magnetic field differential thermal analysis (DTA) device comprises a heating furnace, connect a differential thermal analysis (DTA) device, described heating furnace is a resistance furnace, described differential thermal analysis (DTA) device is placed in the heating furnace chamber with demountable structure, described heating furnace connects a programmed temperature control instrument, and described differential thermal analysis (DTA) device connects a temperature acquisition disposal system.
Heating furnace 24 is by gas outlet 1, electrode 2, and stainless steel boiler clothing 4, asbestos 5, resistance wire heating unit 6 forms.Gas outlet 1 joins with snorkel, and electrode 2 links to each other with the out-put supply of programmed temperature control instrument 15.Resistance wire heats first 6 coated outside asbestos heat-insulation layers 5, and both place in the immortal steel boiler clothing 4, and resistance wire heating unit 6 is linked to each other with electrode 2.When changing sample, the heating furnace part is pulled upwardly along stainless steel slide bar 3, and sample cell then is exposed outside, on the contrary the heating furnace part fall along stainless steel slide bar 3, sample cell then enters in the burner hearth.
The differential thermal analysis (DTA) device is by stainless steel slide bar 3, sample crucible 7, and reference crucible 8 supports alundum tube 9, reference thermopair 10, sample thermopair 11, temperature-control heat couple 12, O-ring seal 13, bracket base 14, air intake opening 15, corundum lid 19, diplopore corundum cover 20, platinum support 22, diplopore alundum tube 23 is formed.Stainless steel slide bar 3 lower ends and bracket base 14 are fixing, and placed O-ring seal 13 on the bracket base 14, support alundum tube 9, diplopore alundum tube 23 links to each other with bracket base 14, supports and places diplopore corundum cover 19 above the alundum tube 9, lays reference thermopair 10 and sample thermopair 11 in the diplopore alundum tube 22, lay platinum support 21 on it, the thermopair chieftain contacts with platinum support 21 bottoms, can place sample crucible 7 and reference crucible 8 on the platinum support, can place sample 20 in the sample crucible 8.
The temperature acquisition disposal system is made up of integrated module 270018 and computing machine 17 that Keithley instrument company produces.
Principle of work:
When carrying out the differential thermal analysis (DTA) experiment, at first with heating furnace part 1. along 3 pull-ups of stainless steel slide bar, take away corundum lid 19, the sample 21 for preparing is put into sample crucible 7, cover corundum lid 19, fall heating furnace 24, then, with heating furnace 24, differential thermal analysis (DTA) device 25 is placed on correct position in the kicker magnet.With electrode 2, temperature-control heat couple 12 is connected to programmed temperature control instrument 16, air intake opening 15, and gas outlet 1 joins with snorkel.Reference thermopair 10 links to each other with temperature collect module 270018 with sample thermopair 11, and 270018 of temperature collect modules and computing machine 17 join.
After all lines connect, open air intake opening 15, gas outlet 1 is opened programmed temperature control instrument 16 then, and heating furnace is heated up by the program of setting and lowers the temperature.Temperature acquisition part and temperature control part are then gathered and record temperature signal on away from the worktable of kicker magnet.
The utility model is transferred to the thermal-analysis instrumentation outside the magnetic field in the magnetic field, increased analysis and the characterization method under the magnetic field, convenient research worker observes and analyzes various phase transition process under the high-intensity magnetic field, and the utility model is a kind of strong analysis means in the material preparation process under the magnetic field.
This high-intensity magnetic field differential thermal analysis (DTA) device can only be used to measure the nonferromugnetic material phase transition process, and for ferromagnetic material, owing to be subjected to great magnetic force under high-intensity magnetic field, this device also can't be measured it.As a kind of heat analysis method, high-intensity magnetic field differential thermal analysis (DTA) device can be used in the various phase transformations in the material preparation process under the magnetic field of research room temperature to 900 ℃, as fusing, solidifies, and separates out solid-state reaction etc.

Claims (6)

1. high-intensity magnetic field differential thermal analysis (DTA) device, comprise a heating furnace (24), connect a differential thermal analysis (DTA) device (25), it is characterized in that described heating furnace (24) is a resistance furnace, described differential thermal analysis (DTA) device (25) is placed in heating furnace (24) furnace chamber with demountable structure, described heating furnace connects a programmed temperature control instrument (16), and described differential thermal analysis (DTA) device (25) connects a temperature acquisition disposal system.
2. kicker magnet differential thermal analysis (DTA) device according to claim 1, the structure that it is characterized in that described heating furnace (24) is: a top has gas outlet (1) and the stainless steel boiler clothing (4) of lower openings, the resistance wire calandria (6) of coated outside asbestos (5) is equipped with in its inside, and described resistance wire calandria (6) connects described programmed temperature control instrument (16) by the electrode that is installed in heating furnace (24) top.
3. kicker magnet differential thermal analysis (DTA) device according to claim 2, the structure that it is characterized in that described differential thermal analysis (DTA) device (25) is: a bracket base (14) and described heating furnace (24) lower openings coupling, described bracket base (14) has air intake opening (15), fixedly mount a sample crucible (7) and a reference crucible (8) arranged side by side by supporting alundum tube (9) above the bracket base (14), sample thermopair (11) under the sample crucible is drawn from bracket base (14) bottom with the reference thermopair (10) under the reference crucible and is connected described temperature acquisition disposal system, described support alundum tube side is installed a temperature-control heat couple (12) and is drawn from bracket base (14) bottom, and connects described programmed temperature control instrument (16).
4. kicker magnet differential thermal analysis (DTA) device according to claim 3, it is characterized in that described temperature acquisition disposal system is that Keithley 2700 temperature collect modules (18) connect a computing machine (17), described sample thermopair (11) is connected the input end of described Keithley2700 temperature collect module (18) with reference thermopair (10).
5. kicker magnet differential thermal analysis (DTA) device according to claim 3, it is characterized in that described sample crucible (7) arranged side by side and reference crucible (8) are placed in the sample cell, the structure of described sample cell is: the fixedly sleeved diplopore corundum cover in described support alundum tube (9) top (20), the corundum lid (19) that the biconvex head is arranged on it, settle sample crucible (7) and reference crucible (8) in its diplopore respectively, the top of described sample thermopair (11) and reference thermopair (10) contacts a platinum support (22) that is placed in sample crucible (7) and reference crucible (8) respectively separately.
6. kicker magnet differential thermal analysis (DTA) device according to claim 3, it is characterized in that described above-mentioned demountable structure is: the top cover of described heating furnace (24) and bottom flange have corresponding each two perforation, described bracket base (14) also has perforation to aim at two perforation of heating furnace (24) top cover and bottom flange, there are two stainless steel slide bars (3) to pass the perforation on heating furnace (24) top cover and the bottom flange and the perforation of bracket base, there is screw thread at these two slide bars two ends, after putting a depression bar, the upper end screws on nut, the lower end also screws on nut, bracket base (14) is compressed by an O-ring seal (13) connect heating furnace bottom flange.
CN2009200694483U 2009-03-26 2009-03-26 Differential thermal analysis device of intense magnetic field Expired - Fee Related CN201425582Y (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103822936A (en) * 2014-03-05 2014-05-28 叶俊 Molding sand and core sand high-temperature property detection instrument and molding sand and core sand high-temperature property detection method
CN105136851A (en) * 2015-09-22 2015-12-09 中国石油大学(华东) Device and method for measuring heat effect in isothermal hot reaction process of carbonaceous macromolecules
CN108507900A (en) * 2018-06-14 2018-09-07 南通大学 A kind of thermal analyzer and its control method
CN109136507A (en) * 2018-08-30 2019-01-04 上海大学 One kind moving up and down formula heating device
CN111020703A (en) * 2019-12-26 2020-04-17 北京北方华创微电子装备有限公司 High-temperature vacuum furnace and semiconductor processing equipment
CN113667797A (en) * 2021-07-23 2021-11-19 中国科学院宁波材料技术与工程研究所 High-saturation magnetic induction amorphous nanocrystalline material and heat treatment device and method thereof

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103822936A (en) * 2014-03-05 2014-05-28 叶俊 Molding sand and core sand high-temperature property detection instrument and molding sand and core sand high-temperature property detection method
CN105136851A (en) * 2015-09-22 2015-12-09 中国石油大学(华东) Device and method for measuring heat effect in isothermal hot reaction process of carbonaceous macromolecules
CN105136851B (en) * 2015-09-22 2018-06-26 中国石油大学(华东) A kind of device and method for measuring fuel factor in carbonaceous macromolecular isothermal thermal process reactor
CN108507900A (en) * 2018-06-14 2018-09-07 南通大学 A kind of thermal analyzer and its control method
CN109136507A (en) * 2018-08-30 2019-01-04 上海大学 One kind moving up and down formula heating device
CN111020703A (en) * 2019-12-26 2020-04-17 北京北方华创微电子装备有限公司 High-temperature vacuum furnace and semiconductor processing equipment
CN113667797A (en) * 2021-07-23 2021-11-19 中国科学院宁波材料技术与工程研究所 High-saturation magnetic induction amorphous nanocrystalline material and heat treatment device and method thereof

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