CN102565114A - DTA/DSC measuring and heating device - Google Patents

DTA/DSC measuring and heating device Download PDF

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Publication number
CN102565114A
CN102565114A CN2010105825500A CN201010582550A CN102565114A CN 102565114 A CN102565114 A CN 102565114A CN 2010105825500 A CN2010105825500 A CN 2010105825500A CN 201010582550 A CN201010582550 A CN 201010582550A CN 102565114 A CN102565114 A CN 102565114A
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CN
China
Prior art keywords
furnace shell
assembly
combustion chamber
inner ring
dta
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN2010105825500A
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Chinese (zh)
Inventor
倪东华
杨洋
吴亚锋
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
SHANGHAI TECHCOMP JINGKE SCIENCE INSTRUMENT CO Ltd
SHANGHAI CO Ltd OF FINE SCIENTIFIC INSTRUMENTS
Original Assignee
SHANGHAI TECHCOMP JINGKE SCIENCE INSTRUMENT CO Ltd
SHANGHAI CO Ltd OF FINE SCIENTIFIC INSTRUMENTS
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
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Publication date
Application filed by SHANGHAI TECHCOMP JINGKE SCIENCE INSTRUMENT CO Ltd, SHANGHAI CO Ltd OF FINE SCIENTIFIC INSTRUMENTS filed Critical SHANGHAI TECHCOMP JINGKE SCIENCE INSTRUMENT CO Ltd
Priority to CN2010105825500A priority Critical patent/CN102565114A/en
Publication of CN102565114A publication Critical patent/CN102565114A/en
Pending legal-status Critical Current

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Abstract

The invention relates to a DTA/DSC measuring and heating device, which is mainly composed of a middle cover, an inner cap, a furnace shell assembly, a sample stage assembly, a furnace core assembly housing, a furnace core assembly, a furnace core assembly ring washer, a hard hat, a flange clamping ring, a cooling flange, a breather pipe and a pillar. The furnace shell assembly is formed by forcedly connecting a furnace shell, a furnace shell upper inner ring and a furnace shell lower inner ring. A multiloop air-flow channel is formed between the furnace shell, the furnace shell upper inner ring and the furnace shell lower inner ring. The furnace core assembly is formed by using an inorganic binder to bond nickel chromium heating wires and winding the nickel chromium heating wires on an alumina furnace core. By fully preheating a gas which enters into a sample area, the influence of the gas which flows into the sample area on the sample temperature is greatly minimized, temperature stability in the sample test area is guaranteed, and measurement precision is raised. Simultaneously, the device provided by the invention has advantages of simple structure, convenient assembling, excellent heat stability, measurement accuracy and high sensitivity, and is suitable for large-batch production and application.

Description

A kind of DTA/DSC measures and heating arrangement
Technical field
The present invention relates to a kind of thermal measurement and heating arrangement of adding, particularly a kind of DTA/DSC measures and heating arrangement.
Background technology
Add thermal measurement and heating arrangement, what on the DTA/DSC thermal analyzer, use often at present is that a kind of sample holder and heating furnace body are relatively independent; The measurement and the heating arrangement in the straight-through sample measurement of snorkel zone.Its primary structure is with the basic manufacturing materials of stainless steel as heating furnace body; The support column that sample holder is processed by alumina material supports and is independent of body of heater and is fixed on middle position; Snorkel is directly by outer straight-through sample area.There are following problem in the measurement of this structure and heating arrangement: 1. with the manufacturing materials of stainless steel as heating furnace body, its thermal inertia is bigger, and heat conductivity is not fine, causes difficulty to accurate temperature controlling with to the Accurate Analysis of sample.2. the sample holder that the support column of being processed as material by aluminium oxide supports installs and fixes difficulty, and consistance is poor, causes the uncertainty of sample analysis easily.3. snorkel influences the stable of sample area temperature directly by the ventilating mode of outer straight-through sample area.
Summary of the invention
It is good, can accurate temperature controlling and can the DTA/DSC that sample carry out Accurate Analysis be measured and heating arrangement that the technical matters that the present invention will solve provides a kind of heating furnace body heat-conductive characteristic; This device makes the gas that gets into sample area obtain sufficient preheating; Reduced the influence of inflow gas greatly to sample temperature; Guarantee the stable of sample test regional temperature; Improved measuring accuracy, had simple in structure, easy to assembly, good heat stability, accurate, the highly sensitive advantage of measurement simultaneously, be suitable for producing in enormous quantities and using.
For solving the problems of the technologies described above; A kind of DTA/DSC measures and heating arrangement, mainly by middle cover, inner cap, furnace shell assembly, sample stage assembly, combustion chamber assembly outer cover, combustion chamber assembly, combustion chamber assembly ring washer, piece together emit, flange clamping ring, cooling flange, snorkel, pillar constitute; Said sample stage assembly is made up of through laser spot welding sample stage, brace, E type thermocouple wire, and this sample stage assembly is arranged on combustion chamber assembly and furnace shell assembly central authorities; Said combustion chamber assembly outer cover is nested with in combustion chamber assembly and furnace shell assembly outside; Said furnace shell assembly is connected with cooling flange through the flange clamping ring with the combustion chamber assembly, and said cooling flange is fixedly connected with pillar.
Said furnace shell assembly is formed by connecting through being press-fitted inner ring under inner ring, the furnace shell on furnace shell, the furnace shell; Said furnace shell is divided into furnace shell and following furnace shell by a thicker dividing plate with it; Form the first lap gas channel on the said furnace shell between the upper wall of the sidewall of inner ring and last furnace shell, dividing plate; Form the second circle gas channel under the said furnace shell between the lower wall of the sidewall of inner ring and following furnace shell, dividing plate; On said dividing plate, also dig a clear opening is arranged; The said first lap gas channel of this clear opening conducting and the second circle gas channel, thus many circle gas channels formed on the furnace shell, furnace shell under inner ring, the furnace shell between the inner ring; Said snorkel is communicated with the second circle gas channel.
Said combustion chamber assembly is bondd and is wrapped on the aluminium oxide combustion chamber through inorganic binder by the nickel chromium triangle heater strip and processes.
Said apparatus, wherein on furnace shell, the furnace shell under inner ring, the furnace shell inner ring be that 99.99% Ag material is processed by purity.
Said apparatus, wherein the aluminium oxide combustion chamber is that 99% alumina material is processed by purity.
Said apparatus, wherein the nickel chromium triangle heater strip is processed by the nickel-chrome material.
Said apparatus, wherein combustion chamber assembly outer cover is processed by the 1Cr18Ni9Ti material.
Said apparatus, wherein sample stage is processed by the constantan material.
Said apparatus, wherein the flange clamping ring, piece together emit, cooling flange processed by the Ni201 material.
Compared with prior art, advantage of the present invention is:
1, the present invention encloses airflow lines by inner ring under inner ring, the furnace shell on furnace shell, the furnace shell through being press-fitted inner formation of the body of heater that forms more; Make the gas that gets into sample area obtain sufficient preheating; Reduced the influence of inflow gas greatly to sample temperature; Guarantee the stable of sample test regional temperature, improved measuring accuracy; The furnace shell assembly is that to use purity be that 99.99% Ag material is processed through Precision Machining, and the heat-conductive characteristic that it is good and thermal stability can satisfy the demand of this device to the accurate measurement of sample fully.
2, the present invention adopts the technological process of inorganic binder through special processing technology and science to make aluminium oxide combustion chamber, the nickel chromium triangle heater strip formation heating unit that is assembled together effectively reliably, has improved the efficiency of heating surface and thermal stability.
Description of drawings
Fig. 1 is the structural representation of DTA/DSC measurement of the present invention and heating arrangement.
Among the figure: 1. middle cover, 2. inner cap, 3. furnace shell assembly, 3-1. furnace shell, inner ring on the 3-2. furnace shell, inner ring under the 3-3. furnace shell; 4. sample stage assembly, 4-1. sample stage, 4-2. brace, 4-3.E type thermocouple wire, 5. combustion chamber assembly outer cover; 6. combustion chamber assembly, 6-1. aluminium oxide combustion chamber, 6-2. nickel chromium triangle heater strip, 6-3. inorganic binder, 7. combustion chamber assembly ring washer; 8. piece together and emit, 9. flange clamping ring, 10. cooling flange, 11. snorkels, 12. pillars.
Embodiment
Below in conjunction with accompanying drawing the present invention is described further:
As shown in Figure 1, a kind of DTA/DSC measures and heating arrangement, can be applicable to the DTA/DSC thermal analyzer.Under program temperature control, measure temperature difference or the temperature variant state of energy difference between measured matter and the reference substance, with the chemistry or the physical characteristics of amalyzing substances.This DTA/DSC measure and heating arrangement mainly by middle cover 1, inner cap 2, furnace shell assembly 3, sample stage assembly 4, combustion chamber assembly outer cover 5, combustion chamber assembly 6, combustion chamber assembly ring washer 7, piece together emit 8, flange clamping ring 9, cooling flange 10, snorkel 11, pillar 12 constitute; Said sample stage assembly 4 is made up of through laser spot welding sample stage 4-1, brace 4-2, E type thermocouple wire 4-3, and this sample stage assembly 4 is arranged on combustion chamber assembly 6 and furnace shell assembly 3 central authorities; Said combustion chamber assembly outer cover 5 is nested with in combustion chamber assembly 6 and furnace shell assembly 3 outsides; Said furnace shell assembly 3 is connected with cooling flange 10 through flange clamping ring 9 with combustion chamber assembly 6, and said cooling flange 10 is fixedly connected with pillar 12.
Said furnace shell assembly 3 is formed by connecting through being press-fitted inner ring 3-3 under inner ring 3-2, the furnace shell on furnace shell 3-1, the furnace shell; Said furnace shell 3-1 is divided into furnace shell and following furnace shell by a thicker dividing plate with it; Form the first lap gas channel on the said furnace shell between the upper wall of the sidewall of inner ring 3-2 and last furnace shell, dividing plate; Form the second circle gas channel under the said furnace shell between the lower wall of the sidewall of inner ring 3-3 and following furnace shell, dividing plate; On said dividing plate, also dig a clear opening is arranged; The said first lap gas channel of this clear opening conducting and the second circle gas channel, thus many circle gas channels formed on the furnace shell 3-1, furnace shell under inner ring 3-2, the furnace shell between the inner ring 3-3; Said snorkel 11 is communicated with the second circle gas channel.
Said combustion chamber assembly 6 is bondd through inorganic binder 6-3 and is wrapped in aluminium oxide combustion chamber 6-1 by nickel chromium triangle heater strip 6-2 and upward processes.
During instrument test; Nickel chromium triangle heater strip 6-2 in the combustion chamber assembly 6 heating under program temperature control; Heat is passed through aluminium oxide combustion chamber 6-1; Furnace shell assembly 3 mainly forms a temperature province with heat conducting mode in body of heater, again through under the sample stage assembly 4 many to temperature thermocouple to temperature effectively and accurate control has guaranteed the stability and the accuracy of sample test regional temperature; Sample stage 4-1 is a symmetrical structure in the sample stage assembly 4; And be to adopt the good constantan of heat conductivility to process; E type thermocouple wire 4-3 under it also is a symmetrical structure, so just can be at temperature variant energy difference (DSC) and carry out corresponding data processing and analysis through electronic technology and computer technology between temperature variant temperature difference (DTA) or measuring samples and the reference substance between effectively reliable down measuring samples of program temperature control and the reference substance.
Critical component sample stage assembly 4 of the present invention is to be processed through special processing mode by two kinds of materials; The sample stage article platform 4-1 of upper end adopts the constantan material to form through Precision Machining; When guaranteeing that two sample stage have good symmetry; Make it reach suitable flatness and surface smoothness, excellent contact is arranged with it to guarantee the sample vessel; It is very good to connect and compose symmetry by the nickel chromium triangle material through the special brace 4-2 that is processed into, E type thermocouple wire 4-3 axle method and the sample stage 4-1 through the accurate spot welding of laser, and the high thermopair of sensitivity satisfies measurement requirement fully.
Furnace shell assembly 3 of the present invention is that to use purity be that 99.99% Ag material is processed through Precision Machining, and the heat-conductive characteristic that it is good and thermal stability can satisfy the demand of this device to the accurate measurement of sample fully.Enclose airflow line by inner ring 3-3 under inner ring 3-2, the furnace shell on furnace shell 3-1, the furnace shell through being press-fitted the body of heater inside that forms more; Make the gas that gets into sample area obtain sufficient preheating; Reduced the influence of inflow gas greatly to sample temperature; Guarantee the stable of sample test regional temperature, improved measuring accuracy.
Combustion chamber assembly 6 of the present invention is to be processed through special processes by different materials; Wherein aluminium oxide combustion chamber 6-1 adopts purity to form through high temperature sintering after special process shapes up to 99% aluminium oxide again, and intensity and resistance to elevated temperatures can satisfy the demand of heat fully preferably for they.Adopt the technological process of inorganic binder 6-3 through special processing technology and science to make aluminium oxide combustion chamber 6-1, the nickel chromium triangle heater strip 6-2 formation heating unit that is assembled together effectively reliably, improved the efficiency of heating surface and thermal stability.
More than show and described ultimate principle of the present invention and principal character and advantage thereof.The technological personage of the industry should understand; The present invention does not receive the restriction of above-mentioned implementing regulations; That describes in above-mentioned implementing regulations and the instructions just is used to explain principle of the present invention; Under the prerequisite that does not break away from the principle of the invention and scope, the present invention also can have various changes and modifications, and these variations and improvement all belong in the scope of the invention of requirement protection.
The present invention requires protection domain to define with appending claims and other equivalent.

Claims (7)

1. a DTA/DSC measures and heating arrangement, mainly emits (8), flange clamping ring (9), cooling flange (10), snorkel (11), pillar (12) to constitute by middle cover (1), inner cap (2), furnace shell assembly (3), sample stage assembly (4), combustion chamber assembly outer cover (5), combustion chamber assembly (6), combustion chamber assembly ring washer (7), assembly; Said sample stage assembly (4) is made up of through laser spot welding sample stage (4-1), brace (4-2), E type thermocouple wire (4-3), and this sample stage assembly (4) is arranged on combustion chamber assembly (6) and furnace shell assembly (3) central authorities; Said combustion chamber assembly outer cover (5) is nested with in combustion chamber assembly (6) and furnace shell assembly (3) outside; Said furnace shell assembly (3) is connected with cooling flange (10) through flange clamping ring (9) with combustion chamber assembly (6), and said cooling flange (10) is fixedly connected with pillar (12); It is characterized in that:
Said furnace shell assembly (3) is formed by connecting through being press-fitted inner ring (3-3) under inner ring (3-2), the furnace shell on furnace shell (3-1), the furnace shell; Said furnace shell (3-1) is divided into furnace shell and following furnace shell by a thicker dividing plate with it; Form the first lap gas channel between the sidewall of inner ring on the said furnace shell (3-2) and last furnace shell, the upper wall of dividing plate; Form the second circle gas channel between the sidewall of inner ring under the said furnace shell (3-3) and following furnace shell, the lower wall of dividing plate; On said dividing plate, also dig a clear opening is arranged; The said first lap gas channel of this clear opening conducting and the second circle gas channel, thus many circle gas channels formed on the furnace shell (3-1), furnace shell under inner ring (3-2), the furnace shell between the inner ring (3-3); Said snorkel (11) is communicated with the second circle gas channel;
Said combustion chamber assembly (6) is bondd through inorganic binder (6-3) by nickel chromium triangle heater strip (6-2) and is wrapped in aluminium oxide combustion chamber (6-1) and upward processes.
2. DTA/DSC according to claim 1 measures and heating arrangement, it is characterized in that: on said furnace shell (3-1), the furnace shell under inner ring (3-2), the furnace shell inner ring (3-3) be that 99.99% Ag material is processed by purity.
3. DTA/DSC according to claim 1 measures and heating arrangement, it is characterized in that: said aluminium oxide combustion chamber (6-1) is that 99% alumina material is processed by purity.
4. DTA/DSC according to claim 1 measures and heating arrangement, and it is characterized in that: said nickel chromium triangle heater strip (6-2) is processed by the nickel-chrome material.
5. DTA/DSC according to claim 1 measures and heating arrangement, and it is characterized in that: said combustion chamber assembly outer cover (5) is processed by the 1Cr18Ni9Ti material.
6. DTA/DSC according to claim 1 measures and heating arrangement, and it is characterized in that: said sample stage (4-1) is processed by the constantan material.
7. DTA/DSC according to claim 1 measures and heating arrangement, and it is characterized in that: said assembly emits (8), flange clamping ring (9), cooling flange (10) to process by the Ni201 material.
CN2010105825500A 2010-12-10 2010-12-10 DTA/DSC measuring and heating device Pending CN102565114A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN2010105825500A CN102565114A (en) 2010-12-10 2010-12-10 DTA/DSC measuring and heating device

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN2010105825500A CN102565114A (en) 2010-12-10 2010-12-10 DTA/DSC measuring and heating device

Publications (1)

Publication Number Publication Date
CN102565114A true CN102565114A (en) 2012-07-11

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Application Number Title Priority Date Filing Date
CN2010105825500A Pending CN102565114A (en) 2010-12-10 2010-12-10 DTA/DSC measuring and heating device

Country Status (1)

Country Link
CN (1) CN102565114A (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109164128A (en) * 2018-10-29 2019-01-08 中国科学院上海硅酸盐研究所 A kind of furnace body for thermal-analysis instrumentation
CN109490356A (en) * 2017-09-12 2019-03-19 爱斯佩克株式会社 Thermal capacitance measuring device and thermal capacitance measuring method

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109490356A (en) * 2017-09-12 2019-03-19 爱斯佩克株式会社 Thermal capacitance measuring device and thermal capacitance measuring method
CN109490356B (en) * 2017-09-12 2021-09-28 爱斯佩克株式会社 Thermal capacity measuring apparatus and thermal capacity measuring method
CN109164128A (en) * 2018-10-29 2019-01-08 中国科学院上海硅酸盐研究所 A kind of furnace body for thermal-analysis instrumentation

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Application publication date: 20120711