CN104792821B - Miniature calorimeter - Google Patents
Miniature calorimeter Download PDFInfo
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- CN104792821B CN104792821B CN201510216854.8A CN201510216854A CN104792821B CN 104792821 B CN104792821 B CN 104792821B CN 201510216854 A CN201510216854 A CN 201510216854A CN 104792821 B CN104792821 B CN 104792821B
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Abstract
The present invention relates to miniature calorimeter, including calorimeter body, temperature control system and data handling system, calorimeter body includes outter box and inner box, outter box is provided with heat block, thermocouple is provided with inner box, one end of probe of thermocouple is connected with inner box, and another end of probe is connected with sample, and thermometer is additionally provided with outter box or inner box；The temperature sensing end of temperature control system is connected with thermometer, and temperature control end is connected with heat block；The temperature data receiving terminal of data handling system is connected with thermometer, and temperature difference data receiver is connected with thermocouple.This calorimeter only has a sample platform, temperature difference between sample and instrument inner box is obtained by thermocouple, the electrode coefficient drawn then in conjunction with standard sample correction, you can obtain thermal change amount of the sample during gradient of temperature, and then draw out DSC curve.Relative to traditional instrument, structure of the invention is more compact, and size is compact.
Description
Technical field
The present invention relates to the calorimeter for material heat analysis, the miniature calorimeter that particularly a kind of structure is simplified.
Background technology
In material heat analysis field, currently used thermometric analysis method is differential scanning calorimetry (differential
Scanning calorimeter) abbreviation DSC.Its Cleaning Principle is to be put into object of reference and test specimens in one casing slowly
Heating or cooling, during heating-cooling, record test specimens are absorbed with object of reference or exothermic difference, then draw out this
The relation curve of heat difference and temperature, i.e. DSC curve.By analyzing DSC curve, it can be realized that test specimens are in heating-cooling
During whether produce heat absorption or exothermic phenomenon, and can quantitatively determine absorption or liberated heat how much.
The instrument for carrying out heat analysis to material using DSC method is referred to as differential scanning calorimeter, traditional differential scanning
Calorimeter, two example platforms are provided with casing, a platform is used to place sample, and another platform is used to place
Reference sample, two platforms are provided with temperature sensing part.Calorimeter is additionally provided with temperature control system, for controlling casing
Change temperature according to predetermined temperature curve.Data handling system is additionally provided with, by the temperature difference for collecting two example platforms
Data, and according to electrode coefficient, it is poor to be scaled the heat of two kinds of samples, and then draws out DSC curve.Wherein, electrode coefficient
Can be calculated by the thermal capacity of measuring basis material, such as high-purity Single crystal alpha-alumina is as primary standard substance.
Due to needing to set two example platforms in calorimeter, cause that its structure is complex and instrument size is larger.
The content of the invention
The technical problems to be solved by the invention are：A kind of miniature calorimeter is provided, it is provided only with a sample
Platform, and changes of heat flux Drawing of Curve can be realized.Relative to traditional differential scanning calorimeter, its structure is more compact, chi
It is very little compact.
The technical solution adopted by the present invention is：
Miniature calorimeter, including calorimeter body, temperature control system and data handling system, the calorimeter body bag
Outter box made of thermally conductive materials and inner box are included, the outter box is provided with heat block, heat is provided with the inner box
Galvanic couple, described one end of probe of thermocouple are connected with inner box, and another end of probe of thermocouple is connected with sample, the outer box
Thermometer is additionally provided with body or inner box；The temperature control system includes temperature sensing end and temperature control end, the temperature
Degree end of probe is connected with thermometer, and the temperature control end is connected with heat block；The data handling system includes temperature data
Receiving terminal and temperature difference data receiver, the temperature data receiving terminal are connected with thermometer, the temperature difference data receiver
It is connected with thermocouple.
Further, the temperature is calculated as platinum resistance thermometer.
Further, the thermocouple is semiconductor thermocouple.
Further, the outter box is cup-like structure, and outter box top is provided with outer cup lid；The inner box is cup-shaped
Structure, inner box top are provided with interior cup lid.
Further, thermal insulation board is provided with the outter box, the inner box is arranged on thermal insulation board, and inner box with
There is gap between outter box.
Further, the inner box and outter box are copper material, and the thermal insulation board is quartz glass plate.
Further, the temperature control system includes power amplification circuit, digital-to-analogue conversion circuit and the place being linked in sequence
End is managed, the power amplification circuit is also associated with power supply circuit, and the power amplification circuit is connected with heat block；Also include and place
The connected analog-to-digital conversion circuit in end is managed, the analog-to-digital conversion circuit is connected with thermometer；The data handling system includes mutual
The analog-to-digital conversion circuit of connection and processing end, the analog-to-digital conversion circuit are connected with thermometer and thermocouple respectively.
Further, connected between the analog-to-digital conversion circuit and processing end by usb circuit, digital-to-analogue conversion circuit
It is connected between processing end by usb circuit；The analog-to-digital conversion circuit, usb circuit, digital-to-analogue conversion circuit, work(
Rate amplifying circuit, power supply circuit are arranged in a circuit box.
The beneficial effects of the invention are as follows：Using the miniature calorimeter of the present invention, it is provided only with a sample platform,
Temperature difference between sample and instrument inner box is obtained by thermocouple, equipment is drawn then in conjunction with standard sample correction
Electrode coefficient, you can draw out changes of heat flux curve of the sample during gradient of temperature, i.e., traditional DSC is bent
Line.Relative to traditional instrument, structure of the invention is more compact, and size is compact.
Brief description of the drawings
Fig. 1 is a kind of schematic diagram of embodiment of miniature calorimeter of the present invention；
Fig. 2 is the schematic diagram of the miniature calorimeter another kind embodiment of the present invention；
Part reference is in figure：Calorimeter body 1, outter box 11, heat block 111, outer cup lid 112, thermometer
113rd, inner box 12, thermocouple 121, sample 122, interior cup lid 123, thermal insulation board 13, analog-to-digital conversion circuit 21, USB interface
Circuit 22, digital-to-analogue conversion circuit 23, power amplification circuit 24, power supply circuit 25, processing end 26, temperature control system 8, temperature are visited
Survey end 81, temperature control end 82, data handling system 9, temperature data receiving terminal 91, temperature difference data receiver 92.
Embodiment
The present invention is further described with reference to the accompanying drawings and examples：
Miniature calorimeter, including calorimeter body 1, temperature control system 8 and data handling system 9, the calorimeter sheet
Body 1 includes outter box 11 made of thermally conductive materials and inner box 12, and the outter box 11 is provided with heat block 111, described interior
Thermocouple 121 is provided with box body 12, described 121 1 end of probe of thermocouple are connected with inner box 12,121 another spy of thermocouple
Survey end to be connected with sample 122, thermometer 113 is additionally provided with the outter box 11 or inner box 12；The temperature control
System 8 includes temperature sensing end 81 and temperature control end 82, and the temperature sensing end 81 is connected with thermometer 113, the temperature
Control terminal 82 is connected with heat block 111；The data handling system 9 includes temperature data receiving terminal 91 and temperature difference data receiver
End 92, the temperature data receiving terminal 91 is connected with thermometer 113, the temperature difference data receiver 92 and the phase of thermocouple 121
Even.
As shown in Figure 1：The calorimeter of the present invention, its calorimeter body 1 are used to be that the offer of sample 122 one is stable
Heating or cooling environment, temperature control system 8 is used to control calorimeter body 1 to heat up or cool according to preset program, at data
Reason system 9 is used to collect the temperature difference that sample 122 occurs in the temperature-fall period that heats up, and is converted into according to electrode coefficient
Energy change value, and then draw out DSC curve.
Specifically, calorimeter body 1 includes outter box 11 made of thermally conductive materials and inner box 12, such as can be aluminium
Metal, preferably copper metal.
The processing mode of box body is preferably using being integrally formed, e.g. using modes such as moulding by casting, punch formings,
And avoid processing using modes such as welding, bondings, it can so make the material of outter box 11 and inner box 12 as far as possible uniform, so as to
Ensure that its heat conduction is uniform, improve detection accuracy.
Outter box 11 is provided with heat block 111, when heat block 111 works, the temperature of outter box 11 can be allowed to rise, passed through
Radiation or heat transfer also promote the internal temperature of inner box 12 to rise.Sample 122 is arranged inside inner box 12, can be to prevent
Only the temperature change of instrument periphery is formed to sample 122 disturbs, and the temperature ramp de of sample 122 is highly stable,
So as to obtain accurately detecting data.Heat block 111 can be the material for using Electric radiant Heating Film, resistance etc. to carry out controllable heating.
Outter box 11 and inner box 12 can be the arbitrary internal structures with receiving space, such as can be cubes
The box of shape, cylindrical cup etc..Distributed in order to avoid the heat of tray interior space from the outward opening of box body, and shadow
The temperature stability of sample 122 is rung, box body can be designed to less opening, such as the outter box, inner box
The hydrostatic column of closing is shaped as, offers the less opening of size on the downside of hydrostatic column, the opening is used for detected sample
Product 122 pass in and out container, can also be preferably to keep tray interior temperature stabilization by way of setting lid in opening.Example
Such as can be that the outter box 11 is cup-like structure, the top of outter box 11 is provided with outer cup lid 112；The inner box 12 is cup-shaped
Structure, the top of inner box 12 are provided with interior cup lid 123.
The inner box 12 can be placed directly in outter box 11, but may so cause inner box 12 and outter box
The 11 position temperature changes being in contact are faster.
Preferably, can be that thermal insulation board 13 is provided with the outter box 11, the inner box 12 is arranged on thermal insulation board 13
On, and there is gap between inner box 12 and outter box 11.Change no directly contact between inner box 12 and outter box 11
Heat, make the temperature changing process around sample 122 more stable.The material of thermal insulation board 13 can be it is arbitrary have compared with
The material of big thermal resistance, preferably quartz glass plate.
Thermocouple 121 is provided with the inner box 12, the one end of thermocouple 121 is connected with inner box 12, the other end and quilt
Test sample product 122 connect, for detecting the temperature difference between sample 122 and inner box 12.For example, when sample 122 is sent out
During raw neither endothermic nor exothermic, temperature difference is had between sample 122 and inner box 12, this temperature difference is detected by thermocouple 121
Arrive, and be sent to data handling system 9.Can be preferably the thermocouple to improve the accuracy of detection of thermocouple 121
121 be semiconductor thermocouple.
Thermometer 113 is additionally provided with the outter box 11 or inner box 12, thermometer 113 is used to detect current outter box
11 or the temperature of inner box 12, this temperature data be transported to temperature control system 8, temperature is then sent by temperature control system 8
Degree control signal is controlled to the caloric value of heat block 111；Temperature data is also delivered to data handling system 9, temperature data
Arranged with temperature difference data by data handling system 9 and form DSC curve.
Because the temperature of outter box 11 and inner box 12 is generally not fully identical, such as temperature in inner box 12 can be omited
Higher than the temperature of outter box 11, when thermometer 113 is arranged at outter box 111, the detected value of thermometer 113 can be modified
Afterwards as sample 122 residing for ambient temperature actual value.The thermometer 113 can have temperature using thermocouple etc.
The device of detection function, can be preferably that the thermometer 113 is platinum resistance thermometer, it is possible to increase the inspection of thermometer 113
Survey precision.
The temperature control system 8 is used to control heat block 111 to generate heat according to preset program, such as detects sample
Whether 122 there is the heat of transformation in 50~70 DEG C of temperature-rise period, then can be to control heat block using temperature control system 8
111 pairs of calorimeters heat, and the Current Temperatures detected according to thermometer 113, and control heat block 111 increases or decreases
Caloric value, calorimeter temperature is set to be stepped up 70 DEG C from 50 DEG C.Concrete implementation mode can utilize prior art, such as
The modes such as PLC control system, feedback circuit control or computer program control.This instrument can also be placed in freezing environment, such as
In refrigerator-freezer, temperature control system 8 controls heat block 111 to generate heat, and makes the environment temperature of sample 122 slowly reduce.It can survey
DSC curve of the test agent in temperature-fall period.
The data handling system 9 is used for the data that reception processing calorimeter body 1 exports, and it includes temperature data reception
End 91 and temperature difference data receiver 92, the temperature data receiving terminal 91 obtain the Current Temperatures of calorimeter from thermometer 113,
After this temperature is corrected it can be assumed that to be environment temperature residing for sample 122, the temperature difference data receiver 92
Obtain the temperature difference between sample 122 and inner box 12 from thermocouple 121, this temperature difference data can be assumed that for be by
Temperature difference between test sample product 122 and environment, for example, when sample 122 occur heat absorption phase transformation when, then can thermocouple 121 with
One end temperature that sample 122 contacts reduces, and then temperature difference occurs in 121 two end of probe of thermocouple, this temperature difference
The heat absorbed in above-mentioned phase transformation of sample 122 is can obtain after coupling apparatus coefficient conversion.
The method that the implementation of specific data handling system 9 can utilize prior art, such as thermocouple 121 obtain
Difference signals be voltage data, after the voltage data is read by voltmeter, the coupling apparatus system by the way of manual conversion
Number obtains heat difference and is recorded on drawing, can also be designed after circuit board converts voltage signal and passed through according to electrode coefficient
Stylus recorder device is plotted on drawing, or voltage signal is after analog-to-digital conversion circuit by inputting computer, in computer
To generating DSC images after data reduction.Thermometer 113 obtain processes temperature signal mode with it is upper similarly.
More specifically, such as can be power amplification circuit 24, digital-to-analogue that the temperature control system 8 includes being linked in sequence
Conversion circuit 23 and processing end 26, the power amplification circuit 24 are also associated with power supply circuit 25, the power amplification circuit 24
It is connected with heat block 111；Also include the analog-to-digital conversion circuit 21 being connected with processing end 26, the analog-to-digital conversion circuit 21 and temperature
Degree meter 113 is connected；
The data handling system 9 includes analog-to-digital conversion circuit 21 and the processing end 26 being connected with each other, the analog-to-digital conversion
Circuit 21 is connected with thermometer 113 and thermocouple 121 respectively.
As shown in Fig. 2 processing end 26 can be computer, notebook computer, or calculated with corresponding, display function
The equipment such as single-chip microcomputer.
The temperature data of outter box 11 that thermometer 113 detects is formed at data signal arrival by analog-to-digital conversion circuit 21
End 26 is managed, processing end 26 is contrasted according to predetermined temperature curve and the temperature data, and sends relevant temperature control letter
Number, temperature control signals form control through digital-to-analogue conversion circuit 23 and power amplification circuit 24 to the heating amount of heat block 111, make
Outter box 11 changes along predetermined temperature curve.
The heat of outter box 11 gradually passes to inner box 12, make the temperature of sample 122 in inner box 12 it is gradual on
Rise, when reaching a certain phase transition temperature, sample 122 may absorb heat, then now thermocouple 121 and sample 122
With another end of probe temperature difference can occur for the end of probe of connection, and then magnitude of voltage occurs in the signal output part of thermocouple 121.This
Individual magnitude of voltage is transported to processing end 26 by analog-to-digital conversion circuit 21, by the suction for being converted into sample 122 of electrode coefficient
Heat, the temperature data that combination temperature meter 113 is sent, you can draw out DSC curve.
Described electrode coefficient can be calculated by measurement standard sample, for example with the oxygen of monocrystalline three of high-purity
Change two aluminium as standard sample, in existing bibliographic data base, Single crystal alpha-alumina can be inquired in each temperature
Thermal capacity value C.Further according to the principle formula dQ/dt=- Δ T/R=C dT/dt (formula one) of calorimeter.
Wherein R is the thermal resistance of thermocouple 121, and Δ T is the temperature difference of 121 two end of probe of thermocouple, and T pairs of temperature difference Δ
The voltage difference delta E for answering thermocouple 121 to export, i.e. Δ T=Δs E/S (formula two), wherein S are the thermoelectric power of thermocouple 121.
So it can be obtained according to formula one and formula two：
DQ/dt=- Δ T/R=- Δs E/ (RS)=C dT/dt (formula three).
The thermal resistance of thermocouple 121 and the product (RS) of thermoelectric power are exactly the electrode coefficient that we need to measure.By standard
Sample, which is placed in this instrument, carries out heating detection, it is possible to according to the voltage difference delta E of the output of thermocouple 121 and according to data in literature
The thermal capacity C of library inquiry, convolution three calculate electrode coefficient (RS).
Next, when detecting sample 122, as long as by the voltage difference delta E of thermocouple 121, with reference to present apparatus system
Number (RS) can be scaled the heat stream (dQ/dt) of sample 122, it is possible to draw out DSC curve.The time is carried out again
Integration, it is possible to obtain sample and absorbed during phase change or liberated heat.
In order to further improve this calorimeter ease of use, can be the analog-to-digital conversion circuit 21 with processing end 26 it
Between connected by usb circuit 22, connected between digital-to-analogue conversion circuit 23 and processing end 26 by usb circuit 22.
Such embodiment, can by analog-to-digital conversion circuit 21, usb circuit 22 connect, digital-to-analogue conversion circuit 23,
Power amplification circuit 24, power supply circuit 25 are arranged in a circuit box, carry calorimeter body 1 and foregoing circuit box, then match somebody with somebody
DSC detections can be started by closing any one computer.And this calorimeter, structure is more compact in design, and its size of outter box 11 is most
It is small to accomplish about 2 cubic centimetres, it is very convenient to carry.
Claims (7)
1. miniature calorimeter, including calorimeter body (1), temperature control system (8) and data handling system (9), its feature exist
In the calorimeter body (1) includes outter box (11) made of thermally conductive materials and inner box (12), the outter box (11)
Heat block (111) is provided with, thermocouple (121), described (121) end of probe of thermocouple are provided with the inner box (12)
It is connected with inner box (12), thermocouple (121) another end of probe is connected with sample (122), the outter box (11) or interior
Thermometer (113) is additionally provided with box body (12)；The temperature control system (8) includes temperature sensing end (81) and temperature control
Hold (82), the temperature sensing end (81) is connected with thermometer (113), the temperature control end (82) and heat block (111) phase
Even；The data handling system (9) includes temperature data receiving terminal (91) and temperature difference data receiver (92), the temperature number
It is connected according to receiving terminal (91) with thermometer (113), the temperature difference data receiver (92) is connected with thermocouple (121)；It is described
Thermal insulation board (13) is provided with outter box (11), the inner box (12) is arranged on thermal insulation board (13), and inner box (12) with
There is gap between outter box (11).
2. miniature calorimeter as claimed in claim 1, it is characterised in that the thermometer (113) is platinum resistance thermometer.
3. miniature calorimeter as claimed in claim 1, it is characterised in that the thermocouple (121) is semiconductor thermocouple.
4. miniature calorimeter as claimed in claim 1, it is characterised in that the outter box (11) is cup-like structure, outter box
(11) top is provided with outer cup lid (112)；The inner box (12) is cup-like structure, and inner box (12) top is provided with interior cup lid
(123)。
5. miniature calorimeter as claimed in claim 1, it is characterised in that the inner box (12) and outter box (11) are copper material
Matter, the thermal insulation board (13) are quartz glass plate.
6. miniature calorimeter as claimed in claim 1, it is characterised in that the temperature control system (8) includes being linked in sequence
Power amplification circuit (24), digital-to-analogue conversion circuit (23) and processing end (26), the power amplification circuit (24) be also associated with
Power supply circuit (25), the power amplification circuit (24) are connected with heat block (111)；Also include the mould being connected with processing end (26)
Number conversion circuit (21), the analog-to-digital conversion circuit (21) are connected with thermometer (113)；The data handling system (9) includes
The analog-to-digital conversion circuit (21) of interconnection and processing end (26), the analog-to-digital conversion circuit (21) respectively with thermometer (113)
It is connected with thermocouple (121).
7. miniature calorimeter as claimed in claim 6, it is characterised in that the analog-to-digital conversion circuit (21) and processing end (26)
Between by usb circuit (22) connect, pass through usb circuit between digital-to-analogue conversion circuit (23) and processing end (26)
(22) connect；The analog-to-digital conversion circuit (21), usb circuit (22), digital-to-analogue conversion circuit (23), power amplification circuit
(24), power supply circuit (25) is arranged in a circuit box.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510216854.8A CN104792821B (en) | 2015-04-29 | 2015-04-29 | Miniature calorimeter |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510216854.8A CN104792821B (en) | 2015-04-29 | 2015-04-29 | Miniature calorimeter |
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| Publication Number | Publication Date |
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| CN104792821A CN104792821A (en) | 2015-07-22 |
| CN104792821B true CN104792821B (en) | 2018-01-16 |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US20170102346A1 (en) * | 2015-10-08 | 2017-04-13 | Richard Brown | MEMS Bio-DSC |
| CN106872077A (en) * | 2017-03-06 | 2017-06-20 | 中国工程物理研究院材料研究所 | Calorimetric structure and calorimeter assembly |
| JP6682485B2 (en) * | 2017-09-12 | 2020-04-15 | エスペック株式会社 | Heat capacity measuring device and heat capacity measuring method |
| 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 |
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