CN112284572A - Thermopile type heat flow sensor for tower structure differential scanning calorimeter - Google Patents
Thermopile type heat flow sensor for tower structure differential scanning calorimeter Download PDFInfo
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- CN112284572A CN112284572A CN202011094994.XA CN202011094994A CN112284572A CN 112284572 A CN112284572 A CN 112284572A CN 202011094994 A CN202011094994 A CN 202011094994A CN 112284572 A CN112284572 A CN 112284572A
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- sensor
- heat flow
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- thermopile
- gold
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- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000000758 substrate Substances 0.000 claims abstract description 29
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000010931 gold Substances 0.000 claims abstract description 15
- 229910052737 gold Inorganic materials 0.000 claims abstract description 15
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 15
- 239000002002 slurry Substances 0.000 claims abstract description 13
- 238000005259 measurement Methods 0.000 claims abstract description 5
- 238000011049 filling Methods 0.000 claims description 3
- 239000000463 material Substances 0.000 abstract description 5
- 230000035945 sensitivity Effects 0.000 abstract description 5
- 239000000919 ceramic Substances 0.000 abstract description 3
- JUWSSMXCCAMYGX-UHFFFAOYSA-N gold platinum Chemical compound [Pt].[Au] JUWSSMXCCAMYGX-UHFFFAOYSA-N 0.000 abstract description 3
- 238000000113 differential scanning calorimetry Methods 0.000 description 6
- 238000001514 detection method Methods 0.000 description 4
- 238000001035 drying Methods 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 238000007639 printing Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 239000011267 electrode slurry Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- DURPTKYDGMDSBL-UHFFFAOYSA-N 1-butoxybutane Chemical compound CCCCOCCCC DURPTKYDGMDSBL-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 238000007790 scraping Methods 0.000 description 1
- 238000007650 screen-printing Methods 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000004513 sizing Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01K—MEASURING TEMPERATURE; MEASURING QUANTITY OF HEAT; THERMALLY-SENSITIVE ELEMENTS NOT OTHERWISE PROVIDED FOR
- G01K17/00—Measuring quantity of heat
- G01K17/06—Measuring quantity of heat conveyed by flowing media, e.g. in heating systems e.g. the quantity of heat in a transporting medium, delivered to or consumed in an expenditure device
- G01K17/08—Measuring quantity of heat conveyed by flowing media, e.g. in heating systems e.g. the quantity of heat in a transporting medium, delivered to or consumed in an expenditure device based upon measurement of temperature difference or of a temperature
- G01K17/10—Measuring quantity of heat conveyed by flowing media, e.g. in heating systems e.g. the quantity of heat in a transporting medium, delivered to or consumed in an expenditure device based upon measurement of temperature difference or of a temperature between an inlet and an outlet point, combined with measurement of rate of flow of the medium if such, by integration during a certain time-interval
- G01K17/12—Indicating product of flow and temperature difference directly or temperature
- G01K17/16—Indicating product of flow and temperature difference directly or temperature using electrical or magnetic means for both measurements
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Combustion & Propulsion (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Measuring Temperature Or Quantity Of Heat (AREA)
Abstract
The invention relates to a thermopile heat flow sensor for a tower-type structure differential scanning calorimeter, and belongs to the technical field of film heat flow sensors. The invention adopts a gold-platinum material to print on a ceramic substrate to form a thermopile. The sensor substrate is characterized in that through holes with equal intervals are distributed in the positions of different radiuses of the sensor substrate in an arc shape, gold and platinum slurry is respectively filled into two adjacent through holes with different radiuses and extends to the upper surface and the lower surface of the substrate, and joints of two materials are distributed between the two adjacent through holes with different radiuses on the upper surface and the lower surface of the sensor. The sensor is formed by connecting 52 pairs of gold-platinum thermocouples in series, and the area of a formed node is 1mm multiplied by 1 mm. The sensor has the advantages that the axial heat flow is measured through the thermopile structure distributed annularly in 3D, the junction density is increased, and the heat flow measurement sensitivity is improved.
Description
Technical Field
The invention belongs to the technical field of film heat flow sensors, and relates to a 3D thermopile type film heat flow sensor for a tower-type structure differential scanning calorimeter.
Background
Differential Scanning Calorimetry (DSC) is an important thermal analyzer, and is characterized by wide temperature range, high resolution and sensitivity, and can be divided into power compensation type and heat flow type according to different measuring methods, and is mainly used for quantifying thermodynamic and kinetic parameters of various materials. Currently, leading DSC producers around the world include german nav instruments, TA instruments in the united states, mettler instruments in switzerland, cetramer instruments in france, Perkin Elmer in the united states, and the like. Among them, only the Perkin Elmer and Shimadzu, Japan, produce power-compensated differential scanning calorimeters, and other thermal analyzer manufacturers are interested in producing heat flow type differential scanning calorimeters.
The heat flow type differential scanning calorimeter is used for measuring the relationship between the heat flow difference of a sample end and a reference end and the temperature or time under the temperature environment and the atmosphere environment with constant flow rate for providing program control for a substance. It has three basic types of disc type, tower type and cylinder type. The tower type DSC has the advantages of shorter heat conduction path than a disc type, smaller system thermal resistance, smaller sample mass than a cylindrical type, and quicker response, and the tower type structure is the trend and mainstream of DSC development.
The heat flow sensor is the most central component of the heat flow type differential scanning calorimeter, and thus the design and characteristics of the heat flow sensor become more important. Aiming at the characteristics that the existing domestic DSC heat flow detection precision is low and the global leading DSC mainly adopts a disc structure, it is necessary to design and prepare a tower-type structure-oriented high-sensitivity heat flow sensor.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides the thermopile heat flow sensor facing the tower-type structure differential scanning calorimeter, which increases the density of hot junction and improves the heat flow detection sensitivity.
The present invention includes a substrate; and through holes with the same size are distributed on arcs with different radiuses at equal intervals by taking the center of the substrate as the center of a circle.
In two adjacent arcs, the through hole of the arc with the larger radius is filled with gold slurry and extends to the upper surface and the lower surface of the sensor to form gold electrodes; and (3) filling platinum slurry into the through hole with the smaller radius, extending to the upper surface and the lower surface of the sensor to form a platinum electrode, and connecting the gold electrode and the platinum electrode on the upper surface and the lower surface of the sensor substrate to form a node so as to realize measurement of heat flow transmitted along the axial direction of the sensor.
The invention has the beneficial effects that:
firstly, according to the 3D thermopile type heat flow sensor, a thermopile structure penetrates through a substrate, and a node is formed on the upper surface and the lower surface of the substrate, so that heat flow measurement is realized by axially transferring along the sensor. And secondly, the positive electrode and the negative electrode of the thermopile are connected end to end through the through holes, so that the density and the number of hot junction points are increased, and the heat flow detection sensitivity is improved.
Drawings
Fig. 1 is a top view of the overall structure of a 3D thermopile heat flow sensor.
Detailed Description
The technical scheme adopted by the invention is as follows:
in terms of sensor structure design: the center of the substrate is taken as the center of a circle, through holes with the same size are distributed on arcs with different radiuses at equal intervals, and in two adjacent arcs, gold slurry is filled in the through holes of the arcs with the larger radiuses and extends to the upper surface and the lower surface of the sensor to form gold electrodes; and (3) filling platinum slurry into the through hole with the smaller radius, extending to the upper surface and the lower surface of the sensor to form a platinum electrode, and connecting the gold electrode and the platinum electrode on the upper surface and the lower surface of the sensor substrate to form a node to form the 3D thermopile type heat flow sensor.
The diameter of the 3D thermopile heat flow sensor substrate is 22mm, the thickness of the substrate is 0.36mm, and the material can be alumina, silicon carbide, aluminum nitride and other ceramics.
The diameters of circular arcs where the through holes are located on the substrate of the 3D thermopile heat flow sensor are respectively 18mm, 15mm, 12mm, 9mm, 6mm and 3mm, and the diameter of each through hole is 1 mm. The area of the formed junction was 1mm × 1mm, and the thickness of the thermode was 10 μm.
The 3D thermopile type heat flow sensor consists of a total of 52 pairs of thermocouples.
When heat flow flows to the sensor perpendicularly, the 3D thermopile type heat flow sensor generates a certain temperature difference delta T on the upper surface and the lower surface of the sensor substrate, and according to the Fourier law:
Φ is the heat flow through the sensor, W; lambda is the thermal conductivity of the sensor substrate material, W/(m.K); a is the cross-sectional area of the sensor substrate, m2(ii) a Δ T is the temperature of the upper and lower surfaces of the sensor substratePoor, K; Δ X is the thickness of the sensor substrate, m.
The 3D thermopile type heat flow sensor, its measured thermoelectromotive force VEMFThe relationship with the temperature difference Δ T is:
VEMF＝n×Sb(T)×ΔT
wherein S isb(T) is the corresponding Seebeck coefficient of the thermocouple at the temperature point T, delta T is the temperature difference between the upper surface and the lower surface of the sensor, and n is the logarithm of the integrated thermocouple node, which is 52 in the invention. According to the invention, through the 3D structural design, the thermocouple node logarithm is increased, the output electromotive force of the heat flow sensor under the same temperature difference and heat flow conditions is improved, and the heat flow detection sensitivity is improved.
In the preparation of the sensor: the invention adopts an electronic printing process to prepare the 3D thermopile type heat flow sensor, and the flow of preparing the heat flow sensor by using the electronic printing process is as follows:
1. substrate cleaning: the ceramic substrate is precisely ground, polished and perforated, ultrasonically cleaned by alcohol and deionized water, then put into an organic solvent butyl ether to remove oil stains, and finally dried by dry nitrogen.
2. Preparing slurry: organic solvents such as acetone and alcohol are added into the gold and platinum slurry in a certain proportion, so that the adhesion force between electrodes and between the electrodes and a substrate is increased.
3. Preparing a screen printing plate: mainly comprises the steps of screen preparation, screen cleaning, coating emulsification, drying and the like.
4. Printing the sizing agent: moving a scraper to scrape and press the platinum pole slurry, leveling the scraped and pressed platinum pole slurry for 10min, and then drying the sensor for 10min at the temperature of 130 ℃; then sintering the mixture in a quartz furnace at 1200 ℃ for 10min, and naturally cooling the mixture to room temperature; and moving a scraper to scrape and press the gold electrode slurry, leveling the gold electrode slurry after scraping and pressing for 10min, then drying the sensor for 10min at the temperature of 130 ℃, then sintering the sensor in a high-temperature tunnel furnace at the temperature of 850 ℃, and preserving heat for 40 min.
The invention is described in further detail below with reference to the accompanying drawings:
as shown in fig. 1, the 3D thermopile heat flow sensor of the present invention comprises:
(1) the thermopiles are annularly distributed on the substrate 1-1 in a 3D shape,
(2) the 3D thermopile structure includes through holes 1-2, gold electrodes 1-3, platinum electrodes 1-4, nodes 1-5, and pins 1-6.
(3) The 3D heat flow sensor thermopile structure consists of 52 pairs of gold platinum thermocouples, which are able to more accurately measure heat flow axially through the substrate.
Thermopiles formed by serially connecting 52 pairs of thermocouples are distributed on the upper and lower surfaces of the sensor through the substrate of the sensor surface. The sensor substrate is provided with 6 groups of circular arc-shaped through holes with different radiuses, wherein the circular arc-shaped through holes are uniformly distributed, the through holes with adjacent radiuses are respectively filled with gold slurry and platinum slurry, extend to the upper surface and the lower surface of the substrate and are connected with the upper surface and the lower surface to form nodes, and measurement of heat flow transmitted along the axial direction of the sensor is realized.
Claims (1)
1. A thermal current sensor of a thermopile facing a tower structure differential scanning calorimeter is characterized in that:
comprises a substrate;
taking the center of the substrate as the center of a circle, and distributing through holes with the same size at equal intervals on arcs with different radiuses;
in two adjacent arcs, the through hole of the arc with the larger radius is filled with gold slurry and extends to the upper surface and the lower surface of the sensor to form gold electrodes; and (3) filling platinum slurry into the through hole with the smaller radius, extending to the upper surface and the lower surface of the sensor to form a platinum electrode, and connecting the gold electrode and the platinum electrode on the upper surface and the lower surface of the sensor substrate to form a node so as to realize measurement of heat flow transmitted along the axial direction of the sensor.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011094994.XA CN112284572A (en) | 2020-10-14 | 2020-10-14 | Thermopile type heat flow sensor for tower structure differential scanning calorimeter |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011094994.XA CN112284572A (en) | 2020-10-14 | 2020-10-14 | Thermopile type heat flow sensor for tower structure differential scanning calorimeter |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112284572A true CN112284572A (en) | 2021-01-29 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011094994.XA Pending CN112284572A (en) | 2020-10-14 | 2020-10-14 | Thermopile type heat flow sensor for tower structure differential scanning calorimeter |
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| Country | Link |
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| CN (1) | CN112284572A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113503981A (en) * | 2021-06-22 | 2021-10-15 | 中国科学院上海硅酸盐研究所 | Interlinked vertical sawtooth type thermopile heat flow sensor and manufacturing method thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4343960A (en) * | 1979-11-20 | 1982-08-10 | Building Research Institute, Ministry Of Construction | Thermopile and process for manufacturing same |
| JP2012255717A (en) * | 2011-06-09 | 2012-12-27 | Etou Denki Kk | Heat flow sensor and manufacturing method of heat flow sensor |
| CN102928460A (en) * | 2012-10-26 | 2013-02-13 | 中国电子科技集团公司第四十八研究所 | Film heat flux sensor and preparation method thereof |
| CN103512682A (en) * | 2013-08-29 | 2014-01-15 | 中国电子科技集团公司第四十八研究所 | Slice array heat-flow sensor |
| CN108562381A (en) * | 2018-03-22 | 2018-09-21 | 中北大学 | Thin film sensor and preparation method thereof for measuring hot-fluid under hot environment |
| CN108975920A (en) * | 2018-03-12 | 2018-12-11 | 中北大学 | A kind of high-temperature heat flux sensor and preparation method thereof based on HTCC |
-
2020
- 2020-10-14 CN CN202011094994.XA patent/CN112284572A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4343960A (en) * | 1979-11-20 | 1982-08-10 | Building Research Institute, Ministry Of Construction | Thermopile and process for manufacturing same |
| JP2012255717A (en) * | 2011-06-09 | 2012-12-27 | Etou Denki Kk | Heat flow sensor and manufacturing method of heat flow sensor |
| CN102928460A (en) * | 2012-10-26 | 2013-02-13 | 中国电子科技集团公司第四十八研究所 | Film heat flux sensor and preparation method thereof |
| CN103512682A (en) * | 2013-08-29 | 2014-01-15 | 中国电子科技集团公司第四十八研究所 | Slice array heat-flow sensor |
| CN108975920A (en) * | 2018-03-12 | 2018-12-11 | 中北大学 | A kind of high-temperature heat flux sensor and preparation method thereof based on HTCC |
| CN108562381A (en) * | 2018-03-22 | 2018-09-21 | 中北大学 | Thin film sensor and preparation method thereof for measuring hot-fluid under hot environment |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113503981A (en) * | 2021-06-22 | 2021-10-15 | 中国科学院上海硅酸盐研究所 | Interlinked vertical sawtooth type thermopile heat flow sensor and manufacturing method thereof |
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Application publication date: 20210129 |
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