CN102759545B - Single group-component differential scanning calorimeter - Google Patents
Single group-component differential scanning calorimeter Download PDFInfo
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- CN102759545B CN102759545B CN201210254888.2A CN201210254888A CN102759545B CN 102759545 B CN102759545 B CN 102759545B CN 201210254888 A CN201210254888 A CN 201210254888A CN 102759545 B CN102759545 B CN 102759545B
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Abstract
The invention belongs to the technical field of thermoanalysis, and discloses a single group-component differential scanning calorimeter, which adopts the single group-component design, and removes a reference unit in the traditional differential scanning calorimeter. The sample unit of the instrument includes an inner crucible and an outer crucible; and the inner and the outer crucibles are made of materials with ultrahigh heat conduction coefficients to guarantee that the two crucibles are provided with uniformly distributed temperature fields during the heating and cooling. Heat flow flowing in or out of a sample can be calculated through the measured temperature between the inner and the outer crucibles, during the measurement, the heat flow is definitely defined, and a big thermal-resistance heat flow passage between the inner and the outer crucibles improves the signal-to-noise ratio of the measurement, so as to improve the accuracy and recurrence rate of the measurement; and the single group-component differential scanning calorimetry is not only suitable for differential scanning calorimeters (DSC), but also suitable for differential thermal analyzers (DTA), thermogravimetry-differential scanning calorimeters (TG-DSC) and thermogravimetry-differential thermal analyzers (TG-DSC).
Description
Technical field
The invention belongs to thermoanalysis technology field, relate to and a kind ofly measure the thermal analyzer of sample thermophysical property along with temperature variation, particularly one list constituent element differential scanning calorimeter.
Background technology
Differential scanning Calorimetric Techniques (Differential Scanning Calorimetry, DSC) refer to: under controlled heating and cooling environment, measure input (output) to measured matter and the energy of reference substance and the relation of temperature, determine ermal physics and the chemical property of tested substance according to this.
Utilize this technology can the ermal physics of quantitative measurment material, chemical property, as: thermal capacitance, phase transition temperature, latent heat etc.
From 1960's, first released the DSC-1 of the said firm by U.S. Perkin-Elmer since, the first backwardations such as many instrument companies (as Du Pont) are proposed the DSC of Multiple Type.Although the DSC that each company releases is various, with regard to its ultimate principle, two large models can be divided into: hot flow type and energy compensation type.
Hot flow type differential scanning calorimetric instrument establishes a heat flux plates below sample unit and reference unit, and when well heater heats under program, heat is delivered to sample and object of reference by heat flux plates.By measuring the hot-fluid and sample temperature that flow into testee and object of reference, then pass through suitable conversion.The ermal physics chemical property of sample just can be expressed out.The major advantage of the method is the shape not requirement to sample.
Energy compensation type differential scanning calorimeter specific heat streaming DSC is many, and two little well heaters are close to below sample reference substance thermal resistance respectively, by regulating the power of these two little well heaters to compensate sample and the temperature difference of object of reference caused by different physical property.
Existing commercial apparatus existing problems and weak point:
The two-disk designs (sample unit and reference unit) of hot flow type differential scanning calorimeter and energy compensation type differential scanning calorimeter has the following disadvantages:
(1). due to the thermal interaction of sample unit and reference unit, cause the hot-fluid measured really can not reflect the physical property change of sample, but by one by the fuzzy information of (smeared).
(2) measuring tempeature of instrument really can not react the true temperature of testee.
Summary of the invention
The object of the invention is for existing hot flow type differential scanning calorimeter and energy compensation type differential scanning calorimeter weak point, and single constituent element differential scanning calorimeter of a kind of reference unit eliminated in conventional differential scanning calorimeter proposed.
The technical problem to be solved in the present invention is: adopt single constituent element to design, and eliminates the reference unit in conventional differential scanning calorimeter.
Main technical schemes of the present invention: single constituent element differential scanning calorimeter, its feature is that this instrument adopts single constituent element to design, and eliminates the reference unit in conventional differential scanning calorimeter; The sample unit of instrument comprises inside and outside two crucibles; Inside and outside two crucibles are prepared by the material of super-high heat-conductive coefficient to ensure that two crucibles have equally distributed temperature field in heating and cooling process.
Usually, the sample unit of instrument of the present invention is by interior, and outer two crucibles form, the internal diameter of outer crucible is 10-20mm, external diameter is 14-24mm, is highly 10-30mm, respectively has a thickness to be that the disc plate of 1-4mm and outer crucible form a closed isothermal body up and down; The internal diameter of interior crucible is 4-10mm, and external diameter is 6-14mm, is highly 5-15mm, respectively has a thickness to be that the disc plate of 1-4mm and interior crucible form a closed isothermal body up and down.
Usually, during measurement, sample is displayed in interior crucible.1-6 thermopair is inserted into the temperature that outer crucible 1/3 – 2/3 highly measures and controls outer crucible, 1-6 thermopair is inserted into interior crucible 1/3 – 2/3 and highly measures and control the temperature of interior crucible, and 1 sample thermopair is inserted into the temperature of sample 0-2/3 elevation carrection sample.
Instrument of the present invention by measure between interior, the temperature of outer crucible, calculates and flows into or flow out the hot-fluid of sample.In the measurements, hot-fluid is through what clearly define, and between interior, the large thermal resistance heat passage between outer crucible improves the signal to noise ratio (S/N ratio) of measurement, thus improves the accuracy and recall factor of measuring.
Single constituent element differential scanning Calorimetric Techniques of the present invention is not only applicable to differential scanning calorimetric instrument (DSC), and is applicable to differential thermal analysis (DTA) instrument (DTA), thermogravimetric-differential scanning calorimetric instrument (TG-DSC), TG-DTA analytical instrument (TG-DSC).
The present invention does not address part and is applicable to prior art.
Accompanying drawing explanation
Accompanying drawing 1 is the structural representation of embodiment of the present invention list constituent element differential scanning calorimeter; Accompanying drawing 2 is heat content and the thermal capacitance curve map of fine aluminium fusing and the process of setting adopting the embodiment of the present invention to measure; Accompanying drawing 3 is the existing hot-fluid of two-disk designs apparatus measures and the curve map of temperature.
In accompanying drawing, 1-outer crucible; 2-sample; Crucible in 3-; 4-thermopair.
Embodiment
Provide specific embodiment of the invention case below, describe the present invention with a nearly step, but it does not limit claim of the present invention.
Case study on implementation 1:
The present embodiment as shown in Figure 1, the sample unit of single constituent element differential scanning calorimeter mainly comprises interior crucible 3, outer crucible 1, and interior crucible 3 and outer crucible 1 are prepared by the material of super-high heat-conductive coefficient to ensure that two crucibles have equally distributed temperature field in heating and cooling process.
The internal diameter of outer crucible 1 is 10mm, and external diameter is 14mm, is highly 14mm, respectively has a thickness to be that the disc plate of 1mm and outer crucible 1 form a closed isothermal body up and down; The internal diameter of interior crucible 3 is 4mm, and external diameter is 6mm, highly for 6mm respectively has a thickness to be that the disc plate of 1mm and interior crucible 3 form a closed isothermal body up and down; Sample 2 is displayed in interior crucible 3.1 thermopair 4 is inserted into the temperature that outer crucible 1/3 is highly measured and controlled outer crucible 1,1 thermopair 4 is inserted into the temperature that interior crucible 1/3 is highly measured and controlled interior crucible 3, and 1 sample thermopair 4 is inserted into the temperature of sample 1/3 elevation carrection sample 2.
Case study on implementation 2:
The internal diameter of the present embodiment outer crucible 1 is 18mm, and external diameter is 22mm, is highly 20mm, respectively has a thickness to be that the disc plate of 2mm and outer crucible 1 form a closed isothermal body up and down; The internal diameter of interior crucible 3 is 10mm, and external diameter is 14mm, highly for 10mm respectively has a thickness to be that the disc plate of 2mm and interior crucible 3 form a closed isothermal body up and down; Sample 2 is displayed in interior crucible 3.6 thermopairs 4 are inserted into the temperature that outer crucible 1/3 is highly measured and controlled outer crucible 1,6 thermopairs 4 are inserted into the temperature that interior crucible 1/3 is highly measured and controlled interior crucible 3, and 1 sample thermopair 4 is inserted into the temperature of sample 1/2 elevation carrection sample 2.
Application Example:
Adopt the heat content of the fusing of the fine aluminium (99.9999wt%) of embodiment of the present invention apparatus measures and process of setting and thermal capacitance to see Fig. 2, as a comparison, adopt the experimental result of two-disk designs to see Fig. 3.Contrast and experiment can find that the present invention can eliminate the measurement result of normal appearance in two-disk designs instrument automatically by the phenomenon of fuzzy (smeard). because instrument of the present invention measures hot-fluid under the condition of maximum thermal resistance, improve the degree of accuracy of measurement.The measurement latent heat of instrument of the present invention and the accuracy rate of thermal capacitance are respectively 1% and 3%.Instrument recall factor is higher than 99%.In table 1.
table 1 fine aluminium measurement data of the present invention
List of references. 1.Hultgren?R,?Desai?P?D?and?Hawkins?D?T,?1973,?
Selected?Values?of?the?Thermodynamic?Properties?of?Elements.?ASM,?Ohio。
Claims (1)
1. a single constituent element differential scanning calorimeter, is characterized in that this instrument adopts single constituent element to design, and eliminates the reference unit in conventional differential scanning calorimeter; By measuring and control the temperature of two crucibles, calculate the hot-fluid flowing into or flow out sample; In the measurements, hot-fluid through the large thermal resistance heat passage that clearly defines to improve the signal to noise ratio (S/N ratio) of measurement; The sample unit of instrument comprises inside and outside two crucibles; Inside and outside two crucibles are prepared by the material of super-high heat-conductive coefficient to ensure that two crucibles have equally distributed temperature field in heating and cooling process; The internal diameter of described outer crucible is 10-20mm, and external diameter is 14-24mm, is highly 10-30mm, respectively has a thickness to be that the disc plate of 1-4mm and outer crucible form a closed isothermal body up and down; The internal diameter of described interior crucible is 4-10mm, and external diameter is 6-14mm, is highly 5-15mm, respectively has a thickness to be that the disc plate of 1-4mm and interior crucible form a closed isothermal body up and down; Sample is displayed in interior crucible, 1-6 thermopair is inserted into the temperature that outer crucible 1/3 – 2/3 highly measures and controls outer crucible, 1-6 thermopair is inserted into interior crucible 1/3 – 2/3 and highly measures and control the temperature of interior crucible, and 1 sample thermopair is inserted into the temperature of sample 0-2/3 elevation carrection sample.
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| US20170102346A1 (en) * | 2015-10-08 | 2017-04-13 | Richard Brown | MEMS Bio-DSC |
| US10466189B2 (en) | 2017-04-21 | 2019-11-05 | Board Of Trustees Of Northern Illinois University | Uniform chilling calorimeter system |
| JP6792040B1 (en) * | 2019-09-25 | 2020-11-25 | ネッチ ゲレーテバウ ゲーエムベーハー | Thermal analyzer, sample holder assembly and thermal analysis method |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE3221548A1 (en) * | 1982-06-08 | 1983-12-08 | Milan Dr.rer.nat. 7808 Waldkirch Smisek | Combustion calorimeter |
| CN101063665A (en) * | 2007-05-31 | 2007-10-31 | 湖南三德科技发展有限公司 | Method for measuring heat productivity of heating substance for calorimeter |
| CN101308107A (en) * | 2007-05-16 | 2008-11-19 | 比亚迪股份有限公司 | Process for determining thermoconductivity |
| CN202133634U (en) * | 2011-04-14 | 2012-02-01 | 中山大学 | Detection device used for testing performance of roof heat insulation module and material |
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| EP1896433A4 (en) * | 2005-05-25 | 2010-06-02 | Ipca Lab Ltd | Novel crystalline forms of (s)-n-(1-carboxy-2-methyl-prop-1-yl)-n-pentanoyl-n-[2'-(1h-tetrazol-5-yl)bi-phenyl-4-ylmethyl]-amine |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE3221548A1 (en) * | 1982-06-08 | 1983-12-08 | Milan Dr.rer.nat. 7808 Waldkirch Smisek | Combustion calorimeter |
| CN101308107A (en) * | 2007-05-16 | 2008-11-19 | 比亚迪股份有限公司 | Process for determining thermoconductivity |
| CN101063665A (en) * | 2007-05-31 | 2007-10-31 | 湖南三德科技发展有限公司 | Method for measuring heat productivity of heating substance for calorimeter |
| CN202133634U (en) * | 2011-04-14 | 2012-02-01 | 中山大学 | Detection device used for testing performance of roof heat insulation module and material |
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