CN104502405B - Differential scanning calorimeter and preparation method thereof - Google Patents
Differential scanning calorimeter and preparation method thereof Download PDFInfo
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- CN104502405B CN104502405B CN201410855358.2A CN201410855358A CN104502405B CN 104502405 B CN104502405 B CN 104502405B CN 201410855358 A CN201410855358 A CN 201410855358A CN 104502405 B CN104502405 B CN 104502405B
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Abstract
The present invention provides a kind of differential scanning calorimeter and preparation method thereof, including uses the subject core part of thick-film technique formation and be arranged at the thermal insulation layer of the subject core portion outboard, and the subject core part includes：Conducting shell；It is set in turn in the first insulating barrier, sensor layer and the second insulating barrier of the conducting shell side；And it is set in turn in the 3rd insulating barrier, zone of heating and the 4th insulating barrier of the conducting shell opposite side；The sensor layer includes symmetrical sample side senser and reference side senser, and the sample side senser and reference side senser is completely covered in second insulating barrier.Integrally formed subject core part is had less thermal capacitance, is realized instrument high sensitivity and less time constant with extraneous using thermal insulation layer isolation heat loss, complete machine.
Description
Technical field
The present invention relates to fields of measurement, and in particular to a kind of differential scanning calorimeter and preparation method thereof.
Background technology
Heat flow flux type differential scanning calorimeter (DSC) its principle be Linear Control temperature by a certain percentage change (as heating,
Cooling or constant temperature), at a temperature of this dynamic change, by certain temperature or the temperature of time interval measurement reference substance and sample
Difference；If instrumental constant of the known apparatus at a temperature of certain, heat flow value at this temperature can be calculated, and then can obtain
The change of continuous heat flow value within the temperature range of dynamic scan.Many heat of specimen material can be analyzed from this change curve
Physical property and its mechanism of production.
In general DSC, in independent resistance-heated furnace, sensor is placed to reference crucible and sample crucible bottom, is come
Both temperature differences of measurement.In DSC measurement, sensitivity, resolution ratio, noise, reappearance etc. are the indexs of performance.It is described heavy
Existing property refers to the uniformity repeatedly of the measurement baseline obtained in the repeated measurement using same temperature program.Reappeared in baseline
Property relatively low (poor) in the case of, even if the measurement using same temperature program is repeated, baseline each time measurement in also send out
Changing, produced in relatively measurement result difficult.On the other hand, in the case of baseline reappearance higher (preferable), easily
Result measuring each time is compared, and can capture the hot change of more detailed sample, also, also improves measurement knot
The reliability of fruit itself.
The factor for influenceing DSC sensitivity is mainly the species of sensor and its position of deployment and structure, while reference
The influence of heat affecting, heater with sample both ends and very important factor, it is fixed feelings in kind of sensor and structure
Under condition, this is into crucial factor.
The key factor for influenceing resolution ratio is the time constant of instrument, and time constant is shorter, and resolution ratio is higher, and the time is normal
Several then relevant with the thermal capacitance of instrument and related to the heat exchange characteristics of reference crucible, sample crucible, thermal capacitance is smaller, and heat exchange is got over
Good, time constant is smaller.
Influence the factor of noise, the heat-transfer character being between each part, and its interference to signal processing system.
The horizontality and reappearance of baseline, mainly influenceed by the heat-transfer character between the symmetry of each part and each part.
The symmetry of reference crucible and sample crucible, the symmetry that they conduct heat to sensor orientation respectively, it is to influence baseline values
With the key factor of reappearance.
Traditional differential scanning calorimeter is made up of heating furnace, sensor, outer thermal insulation layer respectively, is usually designed to cylinder
Shape, heater are longitudinally wound by resistance wire.Reference crucible is symmetrically placed on sensor disc with sample crucible.Sensor
Disc couples with heating furnace, realizes heat transfer heating and cooling.
Found in practice, the specific following shortcoming of this structure：
1st, body of heater thermal capacitance is big, and sensor disc thermal capacitance is big, the characteristics of heat transfer lag be present, therefore, the time constant of instrument
Greatly, the lifting to resolution ratio is unfavorable；
2nd, because sensor direct-coupling is on carrier disc, disc uses the gold of high heat conduction generally for resolution ratio is improved
Category such as silvery is standby, causes the heat transfer between reference and sample to disturb due to the high heat conduction of disc and becomes big, to the sensitive of lifting instrument
Degree is unfavorable factor；
3rd, due to the quality that resistive heater couples with body of heater winding, winding density is generally all in 1mm or so, and sense
The problems such as coupling symmetry of device disc and body of heater, directly influence the horizontality and its reappearance of baseline.
The content of the invention
It is an object of the invention to provide one kind to have less thermal capacitance, realizes instrument high sensitivity and smaller time constant
Differential scanning calorimeter and preparation method thereof.
To solve the above problems, the present invention provides a kind of differential scanning calorimeter, including：
The subject core part formed using thick-film technique；And
It is arranged at the thermal insulation layer of the subject core portion outboard；
Wherein, the subject core part includes：Conducting shell；It is set in turn in the first insulation of the conducting shell side
Layer, sensor layer and the second insulating barrier；And be set in turn in the 3rd insulating barrier of the conducting shell opposite side, zone of heating with
And the 4th insulating barrier；The sensor layer includes symmetrical sample side senser and reference side senser, and described second
The sample side senser and reference side senser is completely covered in insulating barrier.
Optionally, in described differential scanning calorimeter, the conducting shell, the first insulating barrier, the second insulating barrier, the 3rd
Insulating barrier and the 4th insulating barrier are disc-shaped structure, and the area of the conducting shell is more than first insulating barrier, second
Insulating barrier, the 3rd insulating barrier and the 4th insulating barrier.
Optionally, in described differential scanning calorimeter, the zone of heating, sample side senser and reference side sensing
Device is planar double-helix shape structure.
Optionally, in described differential scanning calorimeter, the thermal insulation layer include top thermal insulation layer, bottom thermal insulation layer with
And side wall thermal insulation layer；The top thermal insulation layer is arranged above the conducting shell and surrounds first insulating barrier, sensor layer
And second insulating barrier formed a sample cavity；The bottom thermal insulation layer is arranged at below the conducting shell, and covers the described 4th
Insulating barrier and conducting shell；The side wall thermal insulation layer surrounds the side wall of the conducting shell.
The present invention also provides a kind of preparation method of differential scanning calorimeter, including：
Subject core part is formed using thick-film technique；And
Thermal insulation layer is formed in the subject core portion outboard；
Wherein, the subject core part includes：Conducting shell；It is set in turn in the first insulation of the conducting shell side
Layer, sensor layer and the second insulating barrier；And be set in turn in the 3rd insulating barrier of the conducting shell opposite side, zone of heating with
And the 4th insulating barrier；The sensor layer includes symmetrical sample side senser and reference side senser, and described second
The sample side senser and reference side senser is completely covered in insulating barrier.
Optionally, in the preparation method of described differential scanning calorimeter, described first is insulated using typography
Layer, sensor layer and the second insulating barrier are printed on the conducting shell side successively, and using typography by the 3rd insulating barrier,
Zone of heating and the 4th insulating barrier are printed on the conducting shell opposite side successively, then sinter molding, form the subject core
Part.
Optionally, in the preparation method of described differential scanning calorimeter, Technology for Heating Processing is carried out after sinter molding.
Optionally, in the preparation method of described differential scanning calorimeter, the conducting shell, the first insulating barrier, second
Insulating barrier, the 3rd insulating barrier and the 4th insulating barrier are disc-shaped structure, and the area of the conducting shell is more than described first
Insulating barrier, the second insulating barrier, the area of the 3rd insulating barrier and the 4th insulating barrier.
Optionally, in the preparation method of described differential scanning calorimeter, the zone of heating, sample side senser and
Reference side senser is planar double-helix shape structure.
Optionally, in the preparation method of described differential scanning calorimeter, the thermal insulation layer include top thermal insulation layer, under
Portion's thermal insulation layer and side wall thermal insulation layer；The top thermal insulation layer is arranged above the conducting shell and surrounds first insulation
Layer, sensor layer and the second insulating barrier form a sample cavity；The bottom thermal insulation layer is arranged at below the conducting shell, and is covered
Cover the 4th insulating barrier and conducting shell；The side wall thermal insulation layer surrounds the side wall of the conducting shell.
Compared with prior art, the present invention provides a kind of differential scanning calorimeter, including the master formed using thick-film technique
Body core and the thermal insulation layer for being arranged at the subject core portion outboard, integrally formed subject core part and the external world
Heat loss is completely cut off using thermal insulation layer, complete machine has less thermal capacitance, realizes instrument high sensitivity and less time constant.
Brief description of the drawings
Referring to the drawings, according to following detailed description, the present invention can be more clearly understood.For the sake of clarity, scheme
In each layer of relative thickness and the relative size of given zone be not drawn to draw.In the accompanying drawings：
Fig. 1 is the overall structure diagram of the differential scanning calorimeter of one embodiment of the invention.
Fig. 2 is the structural representation of the differential scanning calorimeter subject core part of one embodiment of the invention.
Embodiment
The description to exemplary embodiment is merely illustrative below, is never used as to the present invention and its application or use
Any restrictions.Techniques well known in the art can be applied to the part for being specifically not shown or describing.
As shown in figure 1, the present invention provides a kind of differential scanning calorimeter, including the subject core formed using thick-film technique
Part and the thermal insulation layer for being arranged at the subject core portion outboard.The subject core part includes：Conducting shell 3；Successively
The first insulating barrier 2, sensor layer and the second insulating barrier 1 of the side of conducting shell 3 are arranged at, second insulating barrier 1 is complete
Sensor layer described in all standing；The 3rd insulating barrier 7, the zone of heating 4 and the 4th for being set in turn in the opposite side of conducting shell 3 are exhausted
Edge layer 8.First insulating barrier 2, sensor layer, the second insulating barrier 1, the 3rd insulating barrier 7, the insulating barrier 8 of zone of heating 4 and the 4th
Be printed on using thick-film technique on the conducting shell 3, re-sinter shaping, integrally formed subject core part with it is extraneous using every
Thermosphere completely cuts off heat loss, and complete machine has less thermal capacitance, realizes instrument high sensitivity and less time constant.
The conducting shell 3 is shaped as disc-shaped, and the area of the conducting shell 3 is more than other layers of subject core part
Area, the influence that the edge effect of heat loss can be avoided to bring.Matrix of the conducting shell 3 as integral core part, simultaneously
As equal thermosphere and refrigeration layer, other each layer stackups, which are printed thereon, to be formed.The material of the conducting shell 3 is silver-based composite wood
Material, the specific heat of the material is small, thermal conductivity factor is high, and the composite-material formula of particular design makes its thermal coefficient of expansion close to insulating barrier
Thermal coefficient of expansion.
The zone of heating 4 is printed as planar double-helix shape using thick-film technique, then sinter molding.It can use alloy platinum material
It is made, the resistance to corrosion of alloy platinum material is preferable, and is used as measuring resistance component material, processing technology comparative maturity.It is described to add
Hot device 4 uses direct current supply, using PID control temperature algorithm；The PID of direct current supply makes the heater 4 of very little specific heat
Temperature control is very accurate.
The sensor layer includes sample side senser 11 and reference side senser 6, the sample side senser 11 with
And reference side senser 6 is symmetrically distributed on first insulating barrier 2, second insulating barrier 1 is covered in the sample side
On sensor 11, the insulating barrier 2 of reference side senser 6 and first.The sensor layer uses platinum sensor (e.g.
Pt100 or Pt1000) or E type film thermocouples connect the thermoelectric pile to be formed.Consider the factor of magnetic field effect, the sample side passes
Sensor 11 and reference side senser 6 are planar double-helix shape structure.
First insulating barrier 2, the second insulating barrier 1, the 3rd insulating barrier 7 and the 4th insulating barrier 8 are to use thick-film technique
It is printed between each layer.In view of the thermal expansion matching problem of each interlayer, first insulating barrier 2, the second insulating barrier the 1, the 3rd
The material of the insulating barrier 8 of insulating barrier 7 and the 4th is the less single-phase alpha-aluminium oxide (α-Al of the coefficient of expansion2O3)。
The thermal insulation layer includes top thermal insulation layer 5, bottom thermal insulation layer 9 and side wall thermal insulation layer 13, to completely cut off heat loss.
The top thermal insulation layer 5 is arranged at the top of conducting shell 3, and it is exhausted to surround first insulating barrier 2, sensor layer and second
Edge layer 1 forms a sample cavity, and sample crucible 12 is arranged at directly over the sample side senser 11, and reference side crucible 10 is arranged at
Directly over reference side senser 6.The bottom thermal insulation layer 9 is arranged at the lower section of conducting shell 3, and covers the 4th insulating barrier
8 and conducting shell 3.The side wall thermal insulation layer 13 surrounds the side wall of the conducting shell 3.The top thermal insulation layer 5, bottom thermal insulation layer
9 and the material of side wall thermal insulation layer 13 be aeroge, heat insulation foam or thermal insulation ceramicses.
The differential scanning calorimeter also includes lid (not shown), to close the sample cavity.The lid with it is described
The shape of sample cavity matches, and cylindric or oval tubular is shaped as in this sample cavity, so the shape of lid mutually should be round
Shape or ellipse.
In the present embodiment, the thickness of the conducting shell 3 between 4~6mm, first insulating barrier 2, the second insulating barrier 1,
The thickness of 3rd insulating barrier 7 and the 4th insulating barrier 8 is between 0.1~0.3mm.Compared with prior art, described in the present embodiment
The subject core part of differential scanning calorimeter is more frivolous.
The present invention also provides a kind of preparation method of differential scanning calorimeter, including：
Subject core part is formed using thick-film technique；And
Thermal insulation layer is formed in the subject core portion outboard；
Wherein, the subject core part includes：Conducting shell 3；It is set in turn in the first insulation of the side of conducting shell 3
The sensor layer is completely covered in layer 2, sensor layer and the second insulating barrier 1, second insulating barrier 1；And set gradually
The 3rd insulating barrier 7, the insulating barrier 8 of zone of heating 4 and the 4th in the opposite side of conducting shell 3.
First insulating barrier 2 is printed and then on the first insulating barrier 2 using thick-film technique on the side of conducting shell 3
Printed sensor layer, the sensor layer include symmetrical sample side senser 11 and reference side senser 6, Ran Houzai
The second insulating barrier 1 is printed thereon.After the 3rd insulating barrier 7 being printed on the opposite side of conducting shell 3 using thick-film technique,
Zone of heating 4 is printed on the 3rd insulating barrier 7 again, the zone of heating 4 is printed as planar double-helix shape, then described in printing thereon
4th insulating barrier 8.Sinter molding together after above layers are completed for printing.
After sinter molding, carry out Technology for Heating Processing, the temperature of the Technology for Heating Processing for example between 500 DEG C~700 DEG C,
So that each insulating barrier, without hole, deformation, the segregation-free uniform with sensor layer composition of zone of heating 4, molding thickness are consistent, and each layer coupling
Conjunction face pore-free, flawless, no stripping, coupling are close uniform.
Found using of the invention with differential scanning calorimeter contrast test of the prior art, for the pure In metals of identical
Sample, much, and time constant greatly reduces for sensitivity of the present invention and good resolution.
Although the present invention is described in detail by exemplary embodiment, those skilled in the art should
The understanding, exemplary embodiment above is merely to illustrate, the scope being not intended to be limiting of the invention.The skill of this area
Art personnel to above example it should be understood that can modify without departing from the scope and spirit of the present invention.This hair
Bright scope is defined by the following claims.
Claims (10)
- A kind of 1. differential scanning calorimeter, it is characterised in that including：The subject core part formed using thick-film technique, the structure that the subject core part is formed in one；AndIt is arranged at the thermal insulation layer of the subject core portion outboard；Wherein, the subject core part includes：Conducting shell；It is set in turn in the first insulating barrier of the conducting shell side, passes Sensor layer and the second insulating barrier；And it is set in turn in the 3rd insulating barrier of the conducting shell opposite side, zone of heating and Four insulating barriers；The sensor layer includes symmetrical sample side senser and reference side senser, second insulation The sample side senser and reference side senser is completely covered in layer.
- 2. differential scanning calorimeter as claimed in claim 1, it is characterised in that the conducting shell, the first insulating barrier, second exhausted Edge layer, the 3rd insulating barrier and the 4th insulating barrier are disc-shaped structure, and the area of the conducting shell is exhausted more than described first Edge layer, the second insulating barrier, the area of the 3rd insulating barrier and the 4th insulating barrier.
- 3. differential scanning calorimeter as claimed in claim 1, it is characterised in that the zone of heating, sample side senser and Reference side senser is planar double-helix shape structure.
- 4. differential scanning calorimeter as claimed in claim 1, it is characterised in that the thermal insulation layer include top thermal insulation layer, under Portion's thermal insulation layer and side wall thermal insulation layer；The top thermal insulation layer is arranged above the conducting shell and surrounds first insulation Layer, sensor layer and the second insulating barrier；The bottom thermal insulation layer is arranged at below the conducting shell, and it is exhausted to cover the described 4th Edge layer and conducting shell；The side wall thermal insulation layer surrounds the side wall of the conducting shell.
- A kind of 5. preparation method of differential scanning calorimeter, it is characterised in that including：Subject core part, the structure that the subject core part is formed in one are formed using thick-film technique；AndThermal insulation layer is formed in the subject core portion outboard；Wherein, the subject core part includes：Conducting shell；It is set in turn in the first insulating barrier of the conducting shell side, passes Sensor layer and the second insulating barrier；And it is set in turn in the 3rd insulating barrier of the conducting shell opposite side, zone of heating and Four insulating barriers；The sensor layer includes symmetrical sample side senser and reference side senser, second insulation The sample side senser and reference side senser is completely covered in layer.
- 6. the preparation method of differential scanning calorimeter as claimed in claim 5, it is characterised in that using typography by described in First insulating barrier, sensor layer and the second insulating barrier are printed on the conducting shell side successively, and using typography by the Three insulating barriers, zone of heating and the 4th insulating barrier are printed on the conducting shell opposite side successively, then sinter molding.
- 7. the preparation method of differential scanning calorimeter as claimed in claim 6, it is characterised in that hot place is carried out after sinter molding Science and engineering skill.
- 8. the preparation method of the differential scanning calorimeter as any one of claim 5 to 7, it is characterised in that the biography Conducting shell, the first insulating barrier, the second insulating barrier, the 3rd insulating barrier and the 4th insulating barrier are disc-shaped structure, and the conduction The area of layer is more than the area of first insulating barrier, the second insulating barrier, the 3rd insulating barrier and the 4th insulating barrier.
- 9. the preparation method of the differential scanning calorimeter as any one of claim 5 to 7, it is characterised in that described to add Thermosphere, sample side senser and reference side senser are planar double-helix shape structure.
- 10. the preparation method of the differential scanning calorimeter as any one of claim 5 to 7, it is characterised in that it is described every Thermosphere includes top thermal insulation layer, bottom thermal insulation layer and side wall thermal insulation layer；The top thermal insulation layer is arranged on the conducting shell Side simultaneously surrounds first insulating barrier, sensor layer and the second insulating barrier；The bottom thermal insulation layer is arranged at the conducting shell Lower section, and cover the 4th insulating barrier and conducting shell；The side wall thermal insulation layer surrounds the side wall of the conducting shell.
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| CN201410855358.2A CN104502405B (en) | 2014-12-31 | 2014-12-31 | Differential scanning calorimeter and preparation method thereof |
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| CN201410855358.2A CN104502405B (en) | 2014-12-31 | 2014-12-31 | Differential scanning calorimeter and preparation method thereof |
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| CN104502405A CN104502405A (en) | 2015-04-08 |
| CN104502405B true CN104502405B (en) | 2018-03-20 |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| DE102018113412A1 (en) * | 2018-06-06 | 2019-12-12 | Netzsch - Gerätebau Gesellschaft mit beschränkter Haftung | Measuring arrangement and method for a thermal analysis of a sample |
| CN109974902B (en) * | 2019-03-29 | 2020-09-11 | 中国计量大学 | Adiabatic acceleration calorimeter with dynamic thermal inertia correction characteristic |
| CN109991271B (en) * | 2019-04-08 | 2022-06-21 | 包头稀土研究院 | Magnetocaloric effect measuring instrument with reference temperature and measuring method |
| CN112179943B (en) * | 2019-07-02 | 2021-12-21 | 天津大学 | Probe for measuring heat conductivity coefficient and preparation method thereof |
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| CN101163950A (en) * | 2005-04-25 | 2008-04-16 | 梅特勒-托利多公开股份有限公司 | Thermoanalytic sensor |
| CN102156148A (en) * | 2010-02-02 | 2011-08-17 | 精工电子纳米科技有限公司 | Differential scanning calorimeter |
| CN103765982A (en) * | 2011-08-30 | 2014-04-30 | 韦巴斯托股份公司 | Electrical heating unit, heating device for vehicle and method for producing heating unit |
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| JP3103963B2 (en) * | 1993-12-14 | 2000-10-30 | セイコーインスツルメンツ株式会社 | How to measure thermal conductivity |
| CA2309152A1 (en) * | 1997-12-02 | 1999-06-10 | Allan L. Smith | Apparatus and method for simultaneous measurement of mass and heat flow changes |
| US6488406B2 (en) * | 2000-03-23 | 2002-12-03 | Ta Instruments-Waters, Llc | Differential scanning calorimeter |
| FR2856794B1 (en) * | 2003-06-25 | 2006-05-05 | Setaram Soc Et D Automatisatio | MEASURING CELL FOR A POWER-COMPENSATED CALORIMETER AND DEVICE COMPRISING TWO SUCH CELLS |
| NL2000080C2 (en) * | 2006-05-23 | 2007-11-26 | Ferro Techniek Holding Bv | Device for heating liquids. |
| CN101487806B (en) * | 2009-02-20 | 2011-06-08 | 中山大学 | DSC meter with visualization function |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101163950A (en) * | 2005-04-25 | 2008-04-16 | 梅特勒-托利多公开股份有限公司 | Thermoanalytic sensor |
| CN102156148A (en) * | 2010-02-02 | 2011-08-17 | 精工电子纳米科技有限公司 | Differential scanning calorimeter |
| CN103765982A (en) * | 2011-08-30 | 2014-04-30 | 韦巴斯托股份公司 | Electrical heating unit, heating device for vehicle and method for producing heating unit |
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Effective date of registration: 20180522 Address after: 200240 room 210, 7 building, 1088 Crane Road, Minhang District, Shanghai. Patentee after: Shanghai platinum Electromechanical Science and Technology Co.,Ltd. Address before: Room 502, room 660, 3, Cangyuan Road, Minhang District, Shanghai Patentee before: Liang Sheng |
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Granted publication date: 20180320 Termination date: 20211231 |