CN100559175C - Peltier low temperature differential heat analyzer - Google Patents
Peltier low temperature differential heat analyzer Download PDFInfo
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- CN100559175C CN100559175C CNB2007100447265A CN200710044726A CN100559175C CN 100559175 C CN100559175 C CN 100559175C CN B2007100447265 A CNB2007100447265 A CN B2007100447265A CN 200710044726 A CN200710044726 A CN 200710044726A CN 100559175 C CN100559175 C CN 100559175C
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- crystallizer
- chip
- heat flux
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Abstract
The invention belongs to hot analysis and testing technology field, be specifically related to a kind of Pa Er card low temperature microthermal analyzer.Form by sensor, crystallizer, heat pump chip, packoff, temperature/heat flux measurement mechanism, temperature/heat flux measurement and output control device, analog-digital commutator, data processing equipment, the packoff middle part is hollow, sensor, crystallizer and chip are positioned at packoff, chip is positioned at the packoff bottom, crystallizer is positioned at the chip top, the crystallizer top has groove, is provided with sensor in the groove; Crystallizer one side is provided with sensor, sensor connects temperature/heat flux by lead and measures and output control device, sensor connects temperature/heat flux measurement mechanism by lead, temperature/heat flux measurement mechanism other end connection mode analog-to-digital conversion apparatus, analog-digital commutator connects computing machine, and computing machine connects printer.The present invention has higher measuring accuracy and automaticity, can be used for the crystal nucleation mechanism research of various organic-compound systems such as DNA, protein, high molecular polymer, medicine, and solid-liquid balances each other and studies and crystallization mechanism research.
Description
Technical field
The invention belongs to hot analysis and testing technology field, be specifically related to a kind of Pa Er card low temperature microthermal analyzer.
Background technology
Pa Er card (Peltire) effect is exactly an electric current when flowing through the interface of two kinds of different conductors, will absorb heat from the external world, or emit heat to the external world.The semiconductor heat pump chip is promptly based on this effect, to connect into galvanic couple right when a N-type semiconductor (electron type) and a P-type semiconductor (cavity type), and during energized, energy just can take place to be shifted, flow deflector joint N type and P-type semiconductor produce electronics, hole respectively, electric current is called cold junction by the joint absorption heat that N type element flows to P type element, and electric current becomes the hot junction by the joint release heat that P flows to N type element.But the characteristics of semiconductor heat pump chip are to allow inverse operation under proper condition, and original cold junction becomes the hot junction and heats when current reversal, so just can select to heat or freeze as long as change by the direction of current of element.
The classic method that is used for hot analysis to measure has liquid nitrogen or compression-type refrigeration, and these method Control Circulation are long, hysteresis is serious, wayward, and the cost of equipment height.
Summary of the invention
The object of the present invention is to provide a kind of Peltier low temperature microthermal analyzer that responds fast, is convenient to operate.
The Peltier low temperature microthermal analyzer that the present invention proposes, by sensor, crystallizer 2, chip 4, packoff 5, temperature/heat flux measurement mechanism 6, temperature/heat flux is measured and output control device 7, analog-digital commutator 8, computing machine 9, printer 10 and heat pump 11 are formed, it is characterized in that packoff 5 middle parts are hollow, sensor, crystallizer 2 and chip 4 are positioned at packoff 5, chip 4 is positioned at packoff 5 bottoms, and by heat pipe connection heat pump 11, temperature/heat flux is measured and output control device (7) carries out programmed control to reach the temperature control requirement to the heat pump chip; Crystallizer 2 is positioned at chip 4 tops by heat-conducting glue, and crystallizer 2 tops have two grooves, are respectively equipped with first sensor 1 in the groove; Crystallizer 2 one sides are provided with second sensor 3, second sensor 3 connects temperature/heat flux by lead and measures and output control device 7, first sensor 1 connects temperature/heat flux measurement mechanism 6 by lead, temperature/heat flux measurement mechanism 6 other end connection mode analog-to-digital conversion apparatus 8, analog-digital commutator 8 connects computing machine 9, and computing machine 9 connects printer 10.
Among the present invention, chip 4 adopts the heat pump chip with heat pump 11 combinations.The heat pump chip both can freeze and also can heat, and response fast, and the refrigeration modes of contact is convenient to operation control.Programmed control semiconductor heat pump chip can obtain desirable temperature control effect more accurately, is suitable for accurately controlling temperature.
Among the present invention, sensor adopts a kind of of temperature/heat-flow sensor, heat-flow sensor.
Heat analyze be the research material in heating or cooling procedure physics and a kind of measuring technique of chemical change.Heat analysis method is divided into two kinds, and a kind of is sample and the temperature difference of reference substance and the differential thermal analysis of time relationship under the routine analyzer control temperature; Also having a kind of then is to be input to the energy difference of sample and reference substance and the differential scanning calorimetry of temperature (or time) relation under the routine analyzer control temperature.When the solid-liquid phase change process is separated out crystal, be attended by heat release, this phenomenon is called as " thermal effect ".Thermal effect makes the cooling curve of solution form " flex point " and " platform ", and this " flex point " is the crystal nucleation point.
The formation of crystal is divided into two stages, promptly forms nucleus earlier, and then grows into crystal.Crystallization solution is not called the stable region before reaching capacity as yet, does not have the possibility of crystallization this moment.Solution reach just saturated after, promptly when nucleus formation speed＞rate of crystal growth, be referred to as the range of instability.This section interval is referred to as to be situated between and surely distinguishes before crystallization solution begins to form nucleus and enters the unstable regin.The steady sector width that is situated between is one of fundamental research content of crystallization process, and the data of gained are crystallization operation and the essential parameter of crystallizer design, and crystallization operation must carry out in the steady district that is situated between.The steady sector width of Jie of solution can be used maximum subcooled temperature Δ T
Max=T
2-T
1Represent (T
2-saturation temperature; T
1-nucleation temperature).
The course of work of the present invention is: the thermal signal on crystallizer 2 surfaces transfers electric signal to by second sensor 3, and this electric signal is measured and output control device 7 displays temperatures by temperature/heat flux, and heat pump chip 4 is carried out programmed control to reach the temperature control requirement; The first sensor 1 that is arranged in the sample hose of crystallizer 2 grooves transfers the thermal signal of sample liquid and reference liquid to electric signal, this electric signal is by temperature/heat flux measurement mechanism 6 displays temperatures, be converted into the temperature digital signal by modulus (A/D) conversion equipment 8 again, computing machine 10 programmings are write down and are handled this temperature digital signal.
Measuring accuracy of the present invention depends primarily on the signal to noise ratio (S/N ratio) of electronic sensor and data acquisition, is generally 0.01 ℃ or higher and cost is lower, simple to operate, compact conformation.It can measure in the solid-liquid phase change process crystal nucleation temperature and the solid-liquid temperature that balances each other, the macroscopic property during the research solid-liquid balances each other.Thereby the present invention can be used widely in the research of crystallization metasable state and solid-liquid balance each other research.
The present invention uses the semiconductor heat pump chip refrigeration based on peltier effect; Operating power control program intensification cooling by control heat pump chip; Utilize computer realization to the temperature signal of research object, storage, conversion and the data processing of heat flux signal.The semiconductor heat pump chip based on peltier effect that the present invention uses both can freeze and also can heat, and response is suitable for accurately controlling temperature fast.The present invention has higher measuring accuracy and automaticity, can be used for the crystal nucleation mechanism research of various organic-compound systems such as DNA, protein, high molecular polymer, medicine, and solid-liquid balances each other and studies and crystallization mechanism research.
Description of drawings
Fig. 1 is a block diagram of the present invention.
Fig. 2 concerns over time for the temperature difference between sample liquid in the embodiment of the invention 1 and reference solution.
Number in the figure: 1 is first sensor, and 2 is crystallizer, and 3 is second sensor, and 4 is chip, 5 is packoff, and 6 is temperature/heat flux measurement mechanism, and 7 is that temperature/heat flux is measured and output control device, and 8 is modulus A/D conversion equipment, 9 is computing machine, and 10 is printer, and 11 is heat pump.
Embodiment
Further specify the present invention below by embodiment.
As shown in Figure 1.Following each parts are connected by mode shown in Figure 1, and these those skilled in the art all can smooth implementation.This device is by second sensor 3, crystallizer 2, chip 4, heat pump 11 and temperature/heat flux is measured and output control device 7 connects and composes successively, first sensor 1 adopts Pt100 sonde-type platinum resistance thermometer sensor,, crystallizer adopts 35*18*25mm metallic crystal device, second sensor 3 adopts Pt100 sheet type platinum resistance thermometer sensor,, chip 4 adopts the TEC1-12704T125 semiconductor chilling plate, packoff 5 adopts 100*100*102mm metallic seal groove, temperature/heat flux measurement mechanism 6 adopts XMTH-7000 intelligent digital adjusting apparatus, temperature/heat flux is measured and output control device 7 adopts the TCA-808 programmed controller, modulus A/D conversion equipment 8 adopts the ADAM-4015 module, computing machine 9 adopts P4 processor P C, printer 10 adopts association's 7000 printers, and heat pump 11 adopts nine continent bearing CPU water-cooled heat radiation pumps.
With above-mentioned gained device in order to measure chromatogram standard specimen level PX (P-xylene C
8H
10) the crystal nucleation temperature.Its mensuration process is as follows:
1. the cleaning of crystallizer 2.After crystallizer 2 usefulness acetone are carried out two minutes ultrasonic cleaning, carry out two minutes ultrasonic cleaning with deionized water again.Put into baking oven after cleaning finishes and carry out drying.
2. experiment parameter determines.Consider that the sample liquid in the present embodiment is high-purity PX solution, its solid-liquid balances each other temperature about 13.15 ℃, and the steady district that is situated between is positioned at the scope in following several years of equilibrium temperature, so whole experimental temperature interval is fixed between 20 ℃ to 5 ℃, cooling rate is controlled at 2 ℃/h.
3. the measurement of crystal nucleation temperature.Inject PX and reference solution (absolute ethyl alcohol) respectively to being arranged in crystallizer groove two sample hoses, open whole apparatus for thermal analysis.Temperature sensor is converted into electric signal with the thermal signal of crystallizer surface, measures and output control device displays temperature and the thermoelectric heat pump chip carried out programmed control to reach the required temperature control requirement of experiment by temperature/heat flux; The temperature sensor of being located in the sample hose transfers the thermal signal in PX solution and the reference solution to electric signal, temperature/heat flux measurement mechanism displays temperature, signal is converted into the temperature digital signal by modulus (A/D) conversion equipment, computer programming writes down and handles the temperature digital signal, and the temperature difference that obtains PX and absolute ethyl alcohol two solution at last concerns over time.
4. the temperature difference-time curve map analysis.As shown in Figure 2.Initial point 1 is to 2 of breaks, and it is zero that the temperature difference of PX and ethanol solution changes perseverance in time; Break 2 places, the temperature difference begins to change and increase to gradually peak dot 3 suddenly; The peak dot 3 back temperature difference are decreased to a little 4 gradually, begin constant afterwards again.According to described thermodynamic principles before as can be known, break 2 is the PX crystal nucleation temperature spot that we will measure.
Claims (1)
1, a kind of Peltier low temperature microthermal analyzer, by sensor, crystallizer (2), chip (4), packoff (5), temperature/heat flux measurement mechanism (6), temperature/heat flux is measured and output control device (7), analog-digital commutator (8), computing machine (9), printer (10) and heat pump (11) are formed, it is characterized in that packoff (5) middle part is hollow, sensor, crystallizer (2) and chip (4) are positioned at packoff (5), chip (4) is positioned at packoff (5) bottom, and by heat pipe connection heat pump (11), temperature/heat flux is measured and output control device (7) carries out programmed control to reach the temperature control requirement to chip; Crystallizer (2) is positioned at chip (4) top by heat-conducting glue, and crystallizer (2) top has two grooves, is respectively equipped with first sensor (1) in the groove; Crystallizer (2) outside is provided with second sensor (3), second sensor (3) connects temperature/heat flux by lead and measures and output control device (7), first sensor (1) connects temperature/heat flux measurement mechanism (6) by lead, temperature/heat flux measurement mechanism (6) other end connection mode analog-to-digital conversion apparatus (8), analog-digital commutator (8) connects computing machine (9), and computing machine (9) connects printer (10); Described chip (4) is the semiconductor heat pump chip, and sensor adopts a kind of of temperature/heat-flow sensor, temperature sensor.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100447265A CN100559175C (en) | 2007-08-09 | 2007-08-09 | Peltier low temperature differential heat analyzer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100447265A CN100559175C (en) | 2007-08-09 | 2007-08-09 | Peltier low temperature differential heat analyzer |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101109721A CN101109721A (en) | 2008-01-23 |
| CN100559175C true CN100559175C (en) | 2009-11-11 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2007100447265A Expired - Fee Related CN100559175C (en) | 2007-08-09 | 2007-08-09 | Peltier low temperature differential heat analyzer |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2214005B1 (en) | 2009-02-03 | 2019-09-18 | Mettler-Toledo GmbH | Thermo-Analytical Instrument |
| CN108088871B (en) * | 2018-01-10 | 2024-03-08 | 上海工程技术大学 | Device and method for testing heat storage performance of fiber aggregate |
| CN109129255A (en) * | 2018-10-25 | 2019-01-04 | 天津职业技术师范大学 | Semiconductor Refrigerating suction cup |
| CN112162003B (en) * | 2020-08-24 | 2022-03-29 | 四川大学 | Device and method for measuring width of micro-scale flow system crystal metastable region |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4292837A (en) * | 1979-02-02 | 1981-10-06 | Stanhope-Seta Limited | Liquid testing apparatus |
| CN1354286A (en) * | 2000-11-17 | 2002-06-19 | 中国科学院物理研究所 | Method for implementing monocrystal growth control by using paltie effect |
| WO2003083462A1 (en) * | 2002-03-28 | 2003-10-09 | Palluel Stephane | Method and device for measuring the crystallisation and melting temperatures of a product |
| DE10344611A1 (en) * | 2003-09-25 | 2005-05-04 | Fraunhofer Ges Forschung | Crystallisation solution supersaturation measurement procedure measures temperature by cooling and heating fluid to obtain different temperature change rates |
-
2007
- 2007-08-09 CN CNB2007100447265A patent/CN100559175C/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4292837A (en) * | 1979-02-02 | 1981-10-06 | Stanhope-Seta Limited | Liquid testing apparatus |
| CN1354286A (en) * | 2000-11-17 | 2002-06-19 | 中国科学院物理研究所 | Method for implementing monocrystal growth control by using paltie effect |
| WO2003083462A1 (en) * | 2002-03-28 | 2003-10-09 | Palluel Stephane | Method and device for measuring the crystallisation and melting temperatures of a product |
| DE10344611A1 (en) * | 2003-09-25 | 2005-05-04 | Fraunhofer Ges Forschung | Crystallisation solution supersaturation measurement procedure measures temperature by cooling and heating fluid to obtain different temperature change rates |
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| CN101109721A (en) | 2008-01-23 |
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