CN104502405A - Differential scanning calorimeter and manufacturing method thereof - Google Patents
Differential scanning calorimeter and manufacturing method thereof Download PDFInfo
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- CN104502405A CN104502405A CN201410855358.2A CN201410855358A CN104502405A CN 104502405 A CN104502405 A CN 104502405A CN 201410855358 A CN201410855358 A CN 201410855358A CN 104502405 A CN104502405 A CN 104502405A
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Abstract
The invention provides a differential scanning calorimeter and a manufacturing method thereof. The differential scanning calorimeter comprises a main body core part formed by using a thick-film technology and a heat insulating layer arranged on the outer side of the main body core part, wherein the main body core part comprises a conducting layer, a first insulating layer, a sensor layer and a second insulating layer which are sequentially arranged on one side of the conducting layer, and a third insulating layer, a heating layer and a fourth insulating layer which are arranged on the other side of the conducting layer; the sensor layer comprises a sample-side sensor and a reference-side sensor which are symmetrically distributed; the second insulating layer completely covers the sample-side sensor and the reference-side sensor. The integrally-formed main body core part is insulated from the outside by using the heat insulating layer, so that the heat loss is reduced, the complete machine is relatively small in heat capacity, and the high sensitivity and the relatively-small time constant of the differential scanning calorimeter are realized.
Description
Technical field
The present invention relates to fields of measurement, be specifically related to a kind of differential scanning calorimeter and preparation method thereof.
Background technology
Heat flow flux type differential scanning calorimeter (DSC) its principle is the change (as heating, cooling or constant temperature) of Linear Control temperature by a certain percentage, at the temperature of this dynamic change, by the temperature difference of uniform temperature or time interval measurement reference substance and sample; If the instrument constant of known apparatus at certain temperature, then can calculate the heat flow value at this temperature, and then the change of the Continuous Heat flow valuve in the temperature range of dynamic scan can be obtained.Many thermophysical propertys and the mechanism of production thereof of specimen material can be analyzed from this change curve.
General DSC, in independently resistance-heated furnace, places bottom sensor to reference crucible and sample crucible, measures both temperature differences.In the measurement of DSC, sensitivity, resolution, noise, reappearance etc. are the indexs of performance.Namely described reappearance refers in the consistance repeatedly using the measurement baseline obtained in the repeated measurement of same temperature program.When baseline reappearance lower (poor), even if repeatedly carry out the measurement using same temperature program, baseline also changes in measuring at each time, produces difficulty when comparing and measuring result.On the other hand, when baseline reappearance higher (better), the result between easily measuring each time compares, and can capture the change of the heat of more detailed sample, and, also improve the reliability of measurement result self.
The factor affecting the sensitivity of DSC is the kind of sensor and the position of deployment thereof and structure mainly, simultaneously reference and the heat affecting at sample two ends, the impact of well heater are also very important factors, in kind of sensor and structure and when determining, this has become crucial factor.
The key factor affecting resolution is the time constant of instrument, and time constant is shorter, and resolution is higher, time constant is then relevant with the thermal capacitance of instrument, and relevant to the heat exchange characteristics of reference crucible, sample crucible, and thermal capacitance is less, heat interchange is better, and time constant is less.
Affect the factor of noise, be the heat transfer characteristic between each parts, and the interference to signal processing system.
The horizontality of baseline and reappearance, primarily of the heat transfer characteristic impact between the symmetry of each parts and each parts.The symmetry of reference crucible and sample crucible, their symmetry of conducting heat respectively to sensor orientation affect baseline values and reproducible key factor.
Traditional differential scanning calorimeter is made up of heating furnace, sensor, outer thermofin respectively, and be usually designed to cylindrical shape, well heater is longitudinally wound around by resistance wire.Reference crucible and sample crucible are symmetrically placed on sensor disc.Sensor disc is coupled with heating furnace, realizes heat transfer heating and cooling.
Find in practice, the concrete following shortcoming of this structure:
1, body of heater thermal capacitance is large, and sensor disc thermal capacitance is large, there is the feature of heat transfer lag, and therefore, the time constant of instrument is large, unfavorable to the lifting of resolution;
2, because sensor direct-coupling is on carrier disc, disc generally for raising resolution and adopts the metal of high heat conduction as standby in silvery, high heat conduction due to disc causes the heat transfer interference between reference and sample to become large, is disadvantageous factor to the sensitivity of lifting instrument;
3, because resistive heater is wound around with body of heater the quality be coupled, density is wound around usually all at about 1mm, and sensor disc and the problems such as symmetry that are coupled of body of heater, directly have influence on horizontality and the reappearance thereof of baseline.
Summary of the invention
The object of the present invention is to provide and a kind of there is less thermal capacitance, realize instrument height sensitivity and the differential scanning calorimeter and preparation method thereof compared with small time constant.
For solving the problem, the invention provides a kind of differential scanning calorimeter, comprising:
Adopt the subject core part that thick-film technique is formed; And
Be arranged at the thermofin of described subject core portion outboard;
Wherein, described subject core part comprises: conducting stratum; Be set in turn in the first insulation course of described conducting stratum side, sensor layer and the second insulation course; And be set in turn in the 3rd insulation course of described conducting stratum opposite side, zone of heating and the 4th insulation course; Described sensor layer comprises symmetrical sample side senser and reference side senser, and described second insulation course covers described sample side senser and reference side senser completely.
Optionally, in described differential scanning calorimeter, described conducting stratum, the first insulation course, the second insulation course, the 3rd insulation course and the 4th insulation course are disc-shaped structure, and the area of described conducting stratum is greater than described first insulation course, the second insulation course, the 3rd insulation course and the 4th insulation course.
Optionally, in described differential scanning calorimeter, described zone of heating, sample side senser and reference side senser are planar double-helix shape structure.
Optionally, in described differential scanning calorimeter, described thermofin comprises top thermofin, bottom thermofin and sidewall thermofin; Described top thermofin to be arranged at above described conducting stratum and to surround described first insulation course, sensor layer and the second insulation course and forms a sample cavity; Described bottom thermofin is arranged at below described conducting stratum, and covers described 4th insulation course and conducting stratum; Described sidewall thermofin surrounds the sidewall of described conducting stratum.
The present invention also provides a kind of method for making of differential scanning calorimeter, comprising:
Thick-film technique is adopted to form subject core part; And
Thermofin is formed at described subject core portion outboard;
Wherein, described subject core part comprises: conducting stratum; Be set in turn in the first insulation course of described conducting stratum side, sensor layer and the second insulation course; And be set in turn in the 3rd insulation course of described conducting stratum opposite side, zone of heating and the 4th insulation course; Described sensor layer comprises symmetrical sample side senser and reference side senser, and described second insulation course covers described sample side senser and reference side senser completely.
Optionally, in the method for making of described differential scanning calorimeter, adopt typography that described first insulation course, sensor layer and the second insulation course are printed on described conducting stratum side successively, and adopt typography that the 3rd insulation course, zone of heating and the 4th insulation course are printed on described conducting stratum opposite side successively, then sinter molding, forms described subject core part.
Optionally, in the method for making of described differential scanning calorimeter, after sinter molding, carry out Technology for Heating Processing.
Optionally, in the method for making of described differential scanning calorimeter, described conducting stratum, the first insulation course, the second insulation course, the 3rd insulation course and the 4th insulation course are disc-shaped structure, and the area of described conducting stratum is greater than the area of described first insulation course, the second insulation course, the 3rd insulation course and the 4th insulation course.
Optionally, in the method for making of described differential scanning calorimeter, described zone of heating, sample side senser and reference side senser are planar double-helix shape structure.
Optionally, in the method for making of described differential scanning calorimeter, described thermofin comprises top thermofin, bottom thermofin and sidewall thermofin; Described top thermofin to be arranged at above described conducting stratum and to surround described first insulation course, sensor layer and the second insulation course and forms a sample cavity; Described bottom thermofin is arranged at below described conducting stratum, and covers described 4th insulation course and conducting stratum; Described sidewall thermofin surrounds the sidewall of described conducting stratum.
Compared with prior art, the invention provides a kind of differential scanning calorimeter, comprise the subject core part adopting thick-film technique to be formed and the thermofin being arranged at described subject core portion outboard, integrated subject core part adopts thermofin to completely cut off thermal loss with extraneous, complete machine has less thermal capacitance, realizes instrument height sensitivity and less time constant.
Accompanying drawing explanation
With reference to accompanying drawing, according to detailed description below, clearly the present invention can be understood.For the sake of clarity, in figure, the relative thickness of each layer and the relative size of given zone are not drawn in proportion.In the accompanying drawings:
Fig. 1 is the one-piece construction schematic 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
Only illustrative to the description of exemplary embodiment below, never as any restriction to the present invention and application or use.Techniques well known in the art can be applied to the part not illustrating especially or describe.
As shown in Figure 1, the invention provides a kind of differential scanning calorimeter, comprise the subject core part adopting thick-film technique to be formed and the thermofin being arranged at described subject core portion outboard.Described subject core part comprises: conducting stratum 3; Be set in turn in the first insulation course 2 of described conducting stratum 3 side, sensor layer and the second insulation course 1, described second insulation course 1 covers described sensor layer completely; Be set in turn in the 3rd insulation course 7 of described conducting stratum 3 opposite side, zone of heating 4 and the 4th insulation course 8.Described first insulation course 2, sensor layer, the second insulation course 1, the 3rd insulation course 7, zone of heating 4 and the 4th insulation course 8 adopt thick-film technique to be printed on described conducting stratum 3, sinter molding again, integrated subject core part adopts thermofin to completely cut off thermal loss with extraneous, complete machine has less thermal capacitance, realizes instrument height sensitivity and less time constant.
The shape of described conducting stratum 3 is disc-shaped, and the area of described conducting stratum 3 is greater than the area of other layers of subject core part, can avoid the impact that the edge effect of thermal loss brings.The matrix of described conducting stratum 3 core as a whole, simultaneously as equal thermosphere and refrigeration layer, other are respectively folded to be printed thereon layer by layer and form.The material of described conducting stratum 3 is silver-based composite material, and the specific heat of this material is little, coefficient of heat conductivity is high, and the composite-material formula of particular design makes its thermal expansivity close to the thermal expansivity of insulation course.
Described zone of heating 4 adopts thick-film technique to be printed as planar double-helix shape, then sinter molding.It can adopt alloy platinum material to make, and the resistance to corrosion of alloy platinum material is better, and as measuring resistance components and parts material, processing technology comparative maturity.Described well heater 4 uses direct current supply, adopts PID control temperature algorithm; The PID of direct current supply makes the control of the temperature of the described well heater 4 of very little specific heat very accurate.
Described sensor layer comprises sample side senser 11 and reference side senser 6, described sample side senser 11 and reference side senser 6 are symmetrically distributed on described first insulation course 2, and described second insulation course 1 covers on described sample side senser 11, reference side senser 6 and the first insulation course 2.The thermoelectric pile that described sensor layer adopts platinum sensor (being such as Pt100 or Pt1000) or the series connection of E type film thermocouple to be formed.Consider the factor of magnetic field effect, described sample side senser 11 and reference side senser 6 are planar double-helix shape structure.
Described first insulation course 2, second insulation course 1, the 3rd insulation course 7 and the 4th insulation course 8 adopt thick-film technique to be printed between each layer.Consider the thermal expansion matching problem of each interlayer, the material of described first insulation course 2, second insulation course 1, the 3rd insulation course 7 and the 4th insulation course 8 is the single-phase alpha-aluminium oxide (α-Al that expansion coefficient is less
2o
3).
Described thermofin comprises top thermofin 5, bottom thermofin 9 and sidewall thermofin 13, in order to isolated thermal loss.Described top thermofin 5 is arranged at above described conducting stratum 3, and surround described first insulation course 2, sensor layer and the second insulation course 1 and form a sample cavity, sample crucible 12 is arranged at directly over described sample side senser 11, and reference side crucible 10 is arranged at directly over reference side senser 6.Described bottom thermofin 9 is arranged at below described conducting stratum 3, and covers described 4th insulation course 8 and conducting stratum 3.Described sidewall thermofin 13 surrounds the sidewall of described conducting stratum 3.The material of described top thermofin 5, bottom thermofin 9 and sidewall thermofin 13 is aerogel, heat insulation foam or thermal insulation ceramics.
Described differential scanning calorimeter also comprises lid (not shown), to close described sample cavity.The mating shapes of described lid and described sample cavity is cylindric or oval tubular in the shape of this sample cavity, so the shape of lid should be circular or oval mutually.
In the present embodiment, the thickness of described conducting stratum 3 is between 4 ~ 6mm, and the thickness of described first insulation course 2, second insulation course 1, the 3rd insulation course 7 and the 4th insulation course 8 is between 0.1 ~ 0.3mm.Compared with prior art, the subject core part of differential scanning calorimeter described in the present embodiment is more frivolous.
The present invention also provides a kind of method for making of differential scanning calorimeter, comprising:
Thick-film technique is adopted to form subject core part; And
Thermofin is formed at described subject core portion outboard;
Wherein, described subject core part comprises: conducting stratum 3; Be set in turn in the first insulation course 2 of described conducting stratum 3 side, sensor layer and the second insulation course 1, described second insulation course 1 covers described sensor layer completely; And be set in turn in the 3rd insulation course 7 of described conducting stratum 3 opposite side, zone of heating 4 and the 4th insulation course 8.
Described conducting stratum 3 side adopt after thick-film technique prints the first insulation course 2, printed sensor layer on the first insulation course 2 again, described sensor layer comprises symmetrical sample side senser 11 and reference side senser 6, and then printing second insulation course 1 on it.After described conducting stratum 3 opposite side uses described 3rd insulation course 7 of thick-film technique printing, then print zone of heating 4 on the 3rd insulation course 7, described zone of heating 4 is printed as planar double-helix shape, then prints described 4th insulation course 8 thereon.Sinter molding together after above-mentioned each layer is completed for printing.
After sinter molding, heat-treat technique, the temperature of described Technology for Heating Processing is such as between 500 DEG C ~ 700 DEG C, to make each insulation course without hole, distortion, zone of heating 4 and sensor layer uniform composition segregation-free, molding thickness are consistent, and each layer coupling surface pore-free, flawless, without peeling off, coupling closely evenly.
Adopt the present invention and differential scanning calorimeter contrast test of the prior art to find, for identical pure In test button, sensitivity of the present invention and resolution much better, and time constant reduces greatly.
Although by exemplary embodiment to invention has been detailed description, it should be appreciated by those skilled in the art, above exemplary embodiment is only to be described, instead of in order to limit the scope of the invention.It should be appreciated by those skilled in the art, can without departing from the scope and spirit of the present invention, above embodiment be modified.Scope of the present invention is limited by claims.
Claims (10)
1. a differential scanning calorimeter, is characterized in that, comprising:
Adopt the subject core part that thick-film technique is formed; And
Be arranged at the thermofin of described subject core portion outboard;
Wherein, described subject core part comprises: conducting stratum; Be set in turn in the first insulation course of described conducting stratum side, sensor layer and the second insulation course; And be set in turn in the 3rd insulation course of described conducting stratum opposite side, zone of heating and the 4th insulation course; Described sensor layer comprises symmetrical sample side senser and reference side senser, and described second insulation course covers described sample side senser and reference side senser completely.
2. differential scanning calorimeter as claimed in claim 1, it is characterized in that, described conducting stratum, the first insulation course, the second insulation course, the 3rd insulation course and the 4th insulation course are disc-shaped structure, and the area of described conducting stratum is greater than the area of described first insulation course, the second insulation course, the 3rd insulation course and the 4th insulation course.
3. differential scanning calorimeter as claimed in claim 1, it is characterized in that, described zone of heating, sample side senser and reference side senser are planar double-helix shape structure.
4. differential scanning calorimeter as claimed in claim 1, it is characterized in that, described thermofin comprises top thermofin, bottom thermofin and sidewall thermofin; Described top thermofin to be arranged at above described conducting stratum and to surround described first insulation course, sensor layer and the second insulation course; Described bottom thermofin is arranged at below described conducting stratum, and covers described 4th insulation course and conducting stratum; Described sidewall thermofin surrounds the sidewall of described conducting stratum.
5. a method for making for differential scanning calorimeter, is characterized in that, comprising:
Thick-film technique is adopted to form subject core part; And
Thermofin is formed at described subject core portion outboard;
Wherein, described subject core part comprises: conducting stratum; Be set in turn in the first insulation course of described conducting stratum side, sensor layer and the second insulation course; And be set in turn in the 3rd insulation course of described conducting stratum opposite side, zone of heating and the 4th insulation course; Described sensor layer comprises symmetrical sample side senser and reference side senser, and described second insulation course covers described sample side senser and reference side senser completely.
6. the method for making of differential scanning calorimeter as claimed in claim 5, it is characterized in that, adopt typography that described first insulation course, sensor layer and the second insulation course are printed on described conducting stratum side successively, and adopt typography that the 3rd insulation course, zone of heating and the 4th insulation course are printed on described conducting stratum opposite side, then sinter molding successively.
7. the method for making of differential scanning calorimeter as claimed in claim 6, is characterized in that, carry out Technology for Heating Processing after sinter molding.
8. the method for making of the differential scanning calorimeter according to any one of claim 5 to 7, it is characterized in that, described conducting stratum, the first insulation course, the second insulation course, the 3rd insulation course and the 4th insulation course are disc-shaped structure, and the area of described conducting stratum is greater than the area of described first insulation course, the second insulation course, the 3rd insulation course and the 4th insulation course.
9. the method for making of the differential scanning calorimeter according to any one of claim 5 to 7, is characterized in that, described zone of heating, sample side senser and reference side senser are planar double-helix shape structure.
10. the method for making of the differential scanning calorimeter according to any one of claim 5 to 7, is characterized in that, described thermofin comprises top thermofin, bottom thermofin and sidewall thermofin; Described top thermofin to be arranged at above described conducting stratum and to surround described first insulation course, sensor layer and the second insulation course; Described bottom thermofin is arranged at below described conducting stratum, and covers described 4th insulation course and conducting stratum; Described sidewall thermofin surrounds the sidewall of described conducting stratum.
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| CN109974902A (en) * | 2019-03-29 | 2019-07-05 | 中国计量大学 | A kind of insulation accelerating calorimeter with dynamic thermal inertia amendment feature |
| CN109991271A (en) * | 2019-04-08 | 2019-07-09 | 包头稀土研究院 | Specimen holder, the magnetothermal effect measuring instrument with reference temperature and measurement method |
| CN110568008A (en) * | 2018-06-06 | 2019-12-13 | 耐驰-仪器制造有限公司 | measuring device and method for the thermal analysis of a sample |
| CN112179943A (en) * | 2019-07-02 | 2021-01-05 | 天津大学 | Probe for measuring heat conductivity coefficient and preparation method thereof |
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| CN104502405B (en) | 2018-03-20 |
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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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