CN109781769A - A kind of device and measurement method measuring graphene film thermo electric material Electrothermal Properties - Google Patents
A kind of device and measurement method measuring graphene film thermo electric material Electrothermal Properties Download PDFInfo
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- CN109781769A CN109781769A CN201910004843.1A CN201910004843A CN109781769A CN 109781769 A CN109781769 A CN 109781769A CN 201910004843 A CN201910004843 A CN 201910004843A CN 109781769 A CN109781769 A CN 109781769A
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Abstract
The present invention relates to a kind of devices and measurement method for measuring graphene film thermo electric material Electrothermal Properties, belong to the thin Electrothermal Properties field of measuring technique of graphene, solve the problems, such as that existing measuring device is difficult to precise measurement radiant heat transfer accounting.The device of measurement graphene film thermo electric material Electrothermal Properties of the invention, including electric control system, test macro and data collection and processing system；Electric control system is for exporting constant current or constant voltage；Test macro is used to obtain the electric current, voltage and temperature information of graphene film layer sample, and test macro includes Electrothermal Properties thermometric room, and Electrothermal Properties thermometric room is equipped with thermocouple；Data collection and processing system is used to collect electric current, voltage and the temperature information of test macro acquisition and is handled, and obtains the Electrothermal Properties data of graphene film thermo electric material.The present invention realizes the precise measurement of the thin Electrothermal Properties of graphene.
Description
Technical field
The present invention relates to graphene Electrothermal Properties field of measuring technique more particularly to a kind of measurement graphene film electric heating materials
Expect the device and measurement method of Electrothermal Properties.
Background technique
Graphene is a kind of new carbon, and grapheme material has excellent electric conductivity, thermal conductivity, zero defect single layer stone
The thermal coefficient of black alkene is up to 5300W/mK.Graphene is the most thin material being currently known, and has excellent mechanical performance (its
Theoretical Young's modulus reaches 1.0TPa, tensile strength 130GPa), big (the up to 2630m of theoretical specific surface area2/ g), carrier moves
Fast (the 200000cm of shifting rate2/ (V.s)) etc. excellent physicochemical property, research field focuses primarily upon composite material at present, battery electricity
Pole, supercapacitor, energy storage material, catalyst, the fields such as thin-film material.
Traditional thermo electric material is divided into metal material and ceramic material two major classes, and the thermo electric material price of metal material is just
Preferably, easy to process, but that there is also density simultaneously is big, hardness is high, not corrosion-resistant, preparation process not environmentally the disadvantages of.Ceramic material
Heating rate is slow, and possesses very big brittleness.New electrically heating material is especially received with various carbon containing or with various nano materials
Rice material thermo electric material as main component.It is compared to metallic resistance silk, carbon nanomaterial has from a wealth of sources and environmentally friendly, surpasses
Light weight is compared to ceramic material, and rapidly, flexibility is good for carbon nanomaterial heating.Moreover, with various carbon nanometer materials
Material, such as carbon nanotube, the thermo electric material of the preparations such as graphene also have lower starting voltage, higher electric conversion efficiency with
And radiant heat transfer accounting.
In electric heating conversion process, due to the characteristic of material itself, part electric energy is converted to interior energy storage, and rest part passes through
The mode of heat transmitting is transmitted outward.In heat transfer process, there are two types of main modes: first, when heating, film surface temperature
It increases, and will transmit heat in air, then form one in air and flowed due to caused by the difference of own temperature,
Referred to as free convection is the major way of traditional material heat transmitting.The generation wavelength second, carbon material can also be excited in the electric field
In 8-14 μm of electromagnetic wave, i.e. far infrared, energy is transmitted by way of heat radiation.Heat radiation belongs to electricity as visible light
Magnetic wave, the interaction with object also include absorbing, reflecting and penetrate.For solid and liquid, the absorption and reflection of radiation
Occur not being related to the inside of object in body surface.Therefore influence of the surface situation of object to these radiation characteristics is to pass
Important.And for gas, the absorption of radiation and penetrate, is carried out in entire gas volume.In addition, far infrared has pole
Strong penetrates effect, can pass through plastics, glass and ceramic, but the object that can be had polar molecule as water
It absorbs.Due to electric heating conversion process and these characteristics of heat transfer process, especially far infrared penetrate and absorption characteristic, make
Obtain the Electrothermal Properties difficulty of test multiplication of material.In addition, having special optical detection apparatus at present to detect new electrically heating material
The wavelength of the far infrared electromagnetic generated in material diabatic process, but this method only can know that the wave-length coverage and phase of the electromagnetic wave of radiation
To intensity, measurement result accuracy is low, poor reliability, cannot obtain accounting of the far infrared radiation in diabatic process, can not
Simulate different working environments.
Summary of the invention
In view of above-mentioned analysis, the present invention is intended to provide a kind of device for measuring graphene film thermo electric material Electrothermal Properties
And measurement method, to solve the problems, such as that existing measuring device is difficult to precise measurement radiant heat transfer accounting.
The purpose of the present invention is mainly achieved through the following technical solutions:
On the one hand provide it is a kind of measure graphene film thermo electric material Electrothermal Properties device, including electric control system,
Test macro and data collection and processing system；Electric control system is for exporting constant current or constant voltage；Test macro is used
In the electric current, voltage and the temperature information that obtain graphene film layer sample, test macro includes Electrothermal Properties thermometric room, and electric heating is special
Property thermometric room be equipped with thermocouple；Data collection and processing system is used to collect electric current, voltage and the temperature letter of test macro acquisition
It ceases and is handled, obtain the Electrothermal Properties data of graphene film thermo electric material.
Further, the outer surface of Electrothermal Properties thermometric room is equipped with the insulation of isolation Electrothermal Properties thermometric indoor and outdoor heat exchange
Material layer.
Further, the inner surface of insulation material layer is equipped with heat radiation reflectance coating, and film layer is tried when preventing test
The heat radiation that sample generates is transmitted outward.
Further, heat radiation reflectance coating is silver coating.
Further, Electrothermal Properties thermometric room includes top surface, side and bottom surface, and film layer sample is set to bottom surface.
Further, one group of thermocouple, film are equipped in top surface, side, bottom surface and space away from bottom surface certain distance
Layer sample is uniformly provided with four groups of thermocouples.
Further, data collection and processing system includes temperature polling instrument and control and processing unit, temperature polling instrument
For recording the real time temperature of electroheat pair, control is used for real-time display electric current, voltage, temperature information with processing unit.
Further, temperature polling instrument is connect with thermocouple, and temperature polling instrument can record the temperature measuring point of thermocouple simultaneously
Real time temperature.
Further, film layer sample is equipped with heated object, and heated object is Electrothermal Properties thermometric room air or liquid
State fluid.
Further, electric control system and data collection and processing system are respectively equipped with ammeter and voltmeter.
On the other hand, a kind of method measuring graphene film thermo electric material Electrothermal Properties is also provided, above-mentioned measurement is utilized
The device of graphene film thermo electric material Electrothermal Properties measures, comprising the following steps:
Step 1: arrangement Electrothermal Properties thermometric room selects heated object, film layer sample is put into Electrothermal Properties thermometric room
In, it selects the quantity of thermocouple and is arranged by requirement of experiment；
Step 2: connection circuit starts experiment test；Disconnecting circuit after the heating stipulated time cools down the stipulated time, obtains
The voltage of film layer sample, electric current and temperature measuring point temperature in experimentation；
Step 3: voltage, electric current and the temperature measuring point temperature data of processing film layer sample obtain the electric heating of film layer sample
Parameter.
Compared with prior art, the present invention one of at least has the advantages that:
A) device of measurement graphene film thermo electric material Electrothermal Properties provided by the invention, table outside Electrothermal Properties thermometric room
Face is equipped with the insulation material layer of the heat exchange of isolation Electrothermal Properties thermometric indoor and outdoor, and the inner surface of the insulation material layer is equipped with heat
Radiation reflective coating, it is right that the Electrothermal Properties thermometric room of this structure can not only completely cut off the heat that Electrothermal Properties are surveyed inside and outside greenhouse space
Stream, and the external transmitting for the heat radiation that film layer sample generates during heating is reduced to the maximum extent, precise measurement passes
Radiant heat transfer accounting in thermal process, simple and quick, test result is more accurate, reliable.
B) device of measurement graphene film thermo electric material Electrothermal Properties provided by the invention, can be by adjusting Electrothermal Properties
The material of thermometric room forms and the material of heated object, and more accurate measurement graphene film thermo electric material is in different works
Make the Electrothermal Properties that environment is shown, it is with a wide range of applications, and pass through the note of the arrangement of thermocouple and temperature polling instrument
The temperature change of record and control and processing unit real-time monitoring different location, simply, quick, accurately measurement radiant heat transfer accounts for
Than, and then by comparing voltage, electric current, initial heating rate, heating-up time, average heating rate, electric heating conversion efficiency, synthesis
The Electrothermal Properties parameters such as coefficient of heat transfer, radiant heat transfer accounting evaluate the quality of material electric heating performance.
It in the present invention, can also be combined with each other between above-mentioned each technical solution, to realize more preferred assembled schemes.This
Other feature and advantage of invention will illustrate in the following description, also, certain advantages can become from specification it is aobvious and
It is clear to, or understand through the implementation of the invention.The objectives and other advantages of the invention can by specification, claims with
And it is achieved and obtained in specifically noted content in attached drawing.
Detailed description of the invention
Attached drawing is only used for showing the purpose of specific embodiment, and is not to be construed as limiting the invention, in entire attached drawing
In, identical reference symbol indicates identical component.
Fig. 1 is the structural schematic diagram of the measurement graphene film thermo electric material Electrothermal Properties device in embodiment；
Fig. 2 is the arrangement schematic diagram of thermocouple and graphene thin layer specimen in Electrothermal Properties thermometric room in embodiment；
Fig. 3 is the arrangement schematic diagram of thermocouple on graphene film layer sample in embodiment.
Appended drawing reference:
1- electric control system；2- test macro, 21- Electrothermal Properties thermometric room；The top surface 22-；The side 23-；The bottom surface 24-；
25- film layer sample；26- thermocouple；27-；First interface；28- second interface；3- data collection and processing system.
Specific embodiment
Specifically describing the preferred embodiment of the present invention with reference to the accompanying drawing, wherein attached drawing constitutes the application a part, and
Together with embodiments of the present invention for illustrating the principle of the present invention, it is not intended to limit the scope of the present invention.
A specific embodiment of the invention discloses a kind of measurement graphene film electric heating material as shown in Figure 1 to Figure 3
Expect the device of Electrothermal Properties, including electric control system 1, test macro 2 and data collection and processing system 3, electrical control system
System 1 is for exporting constant current or constant voltage；(the following letter of graphene film layer sample 25 when test macro 2 is for obtaining experiment
Claim " film layer sample 25 ") electric current, voltage and temperature information, test macro 2 include Electrothermal Properties thermometric room 21, Electrothermal Properties
Thermometric room 21 is equipped with thermocouple 26；Data collection and processing system 3 is used to collect electric current, voltage and the temperature of the acquisition of test macro 2
Degree information is simultaneously handled, and the Electrothermal Properties data of graphene film thermo electric material are obtained.
In the present embodiment, electric control system 1 includes rectification circuit component, output mode control assembly and output valve adjustment
Component, electric control system 1 can adjust output mode, realize Constant current output or constant voltage output, export the precision of electric current
Up to 1mA, the precision of output voltage reaches 1mV.Data collection and processing system 3 includes temperature polling instrument and control and processing unit,
Temperature polling instrument is connect with thermocouple 26, and temperature polling instrument is used to record the real time temperature of thermocouple 26, control and processing unit
For real-time display electric current, voltage, temperature information.Temperature polling instrument can record the real-time temperature of the temperature measuring point of thermocouple 26 simultaneously
Degree, it is preferable that temperature polling instrument is able to record the real time temperature of 1 to 16 thermocouple, 26 temperature measuring point.1 sum number of electric control system
It is respectively equipped with ammeter and voltmeter with processing system 3 according to collecting, illustratively, control system is equipped with ammeter A1And voltmeter
V1, current value or voltage value are preset, control system exports stable current or voltage, and data collection and processing system 3 is set
There is ammeter A2With voltmeter V2If presetting ammeter A1For fixed value, then voltmeter V2Graphene film when measurement experiment
The voltage change of thermo electric material, if presetting voltmeter V1For fixed value, then ammeter A2Graphene film electricity when measurement experiment
The curent change of hot material.
In the present embodiment, the selection of 21 material of Electrothermal Properties thermometric room and the arrangement of arrangement, thermocouple 26 are of the invention
One of main innovation point, wherein the selection of 21 material of Electrothermal Properties thermometric room and be arranged in consideration being capable of precise measurement graphene
Consider that economical and practicability, thermocouple 26 are handled according to follow-up data under the premise of the Electrothermal Properties of film thermo electric material
Demand selected and arranged.
Electrothermal Properties thermometric room 21 includes top surface 22, side 23 and bottom surface 24, and grapheme material to be tested is placed in electricity
The bottom surface 24 of thermal characteristics thermometric room 21 forms film layer sample 25.It is special that the outer surface of Electrothermal Properties thermometric room 21 is equipped with isolation electric heating
Property thermometric indoor and outdoor heat exchange insulation material layer, the inner surface of insulation material layer is equipped with heat radiation reflectance coating.It is selected in material
It selects, insulation material layer is preferably loose fiber or foam porous material, such as polystyrene plastics foam, plasticized polyurethane parison
Foam, or powder particle heat-insulating material can also be multi-layer vacuum thermal insulation board；Heat radiation reflecting material can for gold,
The paillon or coating of silver, nickel, aluminium etc.；In arrangement, insulation material layer is arranged in outer surface, and inner surface is arranged heat radiation and reflects
Layer, heat insulation layer can be one layer or multilayer, and heat radiation reflecting layer is one layer, it is preferred that two layers of heat-insulating material and one layer of hot spoke
Reflecting material is penetrated, the heat-insulating material of outer layer is polystyrene plastics foam, and the heat-insulating material of internal layer is plasticized polyurethane strand foam, heat
Radiation reflecting layer is silver coating.The insulation of heat exchange inside and outside the setting isolation Electrothermal Properties thermometric room 21 of Electrothermal Properties thermometric room 21
Material layer and heat radiation reflectance coating can prevent the heat radiation that film layer sample 25 generates when test from transmitting outward, test knot
Fruit is more accurate and reliable.
It is equipped in the top surface 22 of Electrothermal Properties thermometric room 21, side 23, bottom surface 24 and space away from bottom surface certain distance
One group of thermocouple 26, film layer sample 25 are uniformly provided with four groups of thermocouples 26, and film layer sample 25 is equipped with the electricity with control system
The first interface 27 and second interface 28 of road connection, test electric current enter from first interface 27, flow out from second interface 28, such as scheme
Shown in 2, the size of film layer sample 25 to be measured can be adjusted according to requirement of experiment, is set in Electrothermal Properties thermometric room 21 position
And quantity and the setting position of thermocouple 26.In the selection of thermocouple 26, it can choose K-type, T-type, J-type, the thermoelectricity such as E type
It is even, K-type thermocouple is used in this embodiment, the arrangement of thermocouple 26 selects quantity and position according to testing requirement, initially
Heating rate, heating-up time, average heating rate use in film layer sample and space away from bottom surface certain distance totally five groups of heat
The data of galvanic couple, and integrate coefficient of heat transfer, electric heating conversion efficiency, radiant heat transfer accounting and then need to use whole thermocouples 26
Temperature data.It can be according to the thermocouple of testing requirement arranging section or whole.
Film layer sample 25 is equipped with heated object, and heated object is air or liquid stream in Electrothermal Properties thermometric room 21
Body.Air in the cavity of Electrothermal Properties thermometric room 21 is one of heated object, in measurement graphene film thermo electric material
Electrothermal Properties when, select the empty chamber air of Electrothermal Properties thermometric room 21 as heated object；And in simulation working environment, such as
The waist for heating human body whens knee etc., according to different test conditions, selects different heated objects, such as selection liquid stream
Body is as heated object, such as pure water, physiological saline etc..
The device of measurement graphene film thermo electric material Electrothermal Properties provided in this embodiment, test object include but unlimited
The film for determining the preparation of graphene film material can such as measure the thin of other carbon material preparations with far infrared radiation feature
Film also can measure the film of other traditional thermo electric material preparations.
Utilize the device measurement graphene film electricity of the measurement graphene film thermo electric material Electrothermal Properties in the present embodiment
The method of hot material Electrothermal Properties, comprising the following steps:
Step 1: Electrothermal Properties thermometric room 21 is arranged according to requirement of experiment, and selects heated object；Graphene electric heating is thin
Film layer sample 25 is put into Electrothermal Properties thermometric room 21, and is selected the quantity of thermocouple 26 and arranged as required.
Step 2: connecting alternating current, sets the mode and parameter value of input, adjusts input pattern control assembly and input value
Adjust component, setting input pattern and input parameter；Connection circuit starts experiment test；Disconnecting circuit after the heating stipulated time,
Cool down the stipulated time, the temperature data of electric current, voltage and each thermocouple 26 when record is tested.Wherein, there are two types of input patterns,
One kind is that control system exports DC stabilization electric current, and another kind is that control system exports direct-flow steady voltage, correspondingly, data are received
Collection obtains the voltage change or curent change situation of film layer sample 25 with processing system 3.
Step 3: voltage, electric current and the temperature measuring point temperature data of processing film layer sample 25 obtain film layer sample 25
Electric heating parameter.Specifically, after experiment, export the voltage of film layer sample 25 in experimentation, electric current, temperature measuring point temperature with
Simultaneously the heating-up time is calculated in the change curve of time, comprehensive coefficient of heat transfer, electric heating conversion efficiency, radiant heat transfer accounting and just
The electric heating parameter such as beginning heating rate and average heating rate, and with the superiority and inferiority of this comparison material.
In the present embodiment, Electrothermal Properties data include initial heating rate, the heating-up time, average heating rate, comprehensive dissipate
Hot coefficient, electric heating conversion efficiency and radiant heat transfer accounting, for different Electrothermal Properties data, processing method also phase not to the utmost
Together, two methods of curve matching, mounted castization calculating are mainly used, specifically: initial heating rate, is averaged at the heating-up time
Heating rate is matched curve to be obtained by the method for nonlinear fitting, and calculate according to its physical significance and experiment demand
It arrives, wherein the heating-up time can be used " GB/T 7287-2008 infrared radiation heater test method ", and initial heating rate is put down
Equal heating rate is according to experiment demand and its physical significance self-defining.Comprehensive coefficient of heat transfer be according to its physical significance, according to
Newtonian Cooling formula linear fit obtains.Electric heating conversion efficiency, radiant heat transfer accounting are by the way that Electrothermal Properties are surveyed Greenhouse model
Change, it can be according to " thermal conduction study " (Beijing Yang Shiming, inscription on pottery select thermal conduction study (fourth edition) [M]: Higher Education Publishing House, 2006.)
In the calculation method in relation to convection current and radiant heat transfer obtain.
Compared with prior art, the device of measurement graphene film thermo electric material Electrothermal Properties provided in this embodiment, electricity
21 outer surface of thermal characteristics thermometric room is equipped with the insulation material layer of the heat exchange inside and outside isolation Electrothermal Properties thermometric room 21, heat-insulating material
The inner surface of layer is equipped with heat radiation reflectance coating, and the Electrothermal Properties thermometric room 21 of this structure can not only completely cut off Electrothermal Properties thermometric
Thermal convection inside and outside 21 space of room, and the heat radiation that film layer sample 25 generates during heating is reduced to the maximum extent
It externally transmits, the radiant heat transfer accounting in precise measurement diabatic process, simple and quick, test result is more accurate, reliable.
In addition, can be by adjusting the material of the material of Electrothermal Properties thermometric room 21 composition and heated object, more accurate measurement stone
The Electrothermal Properties that black alkene film thermo electric material is shown in different working environments, it is with a wide range of applications, and pass through heat
The arrangement of galvanic couple 26 and the record of temperature polling instrument and the temperature change of control and processing unit real-time monitoring different location, letter
Single, quick, accurately measurement radiant heat transfer accounting, and then voltage by comparing, electric current, initial heating rate, are put down at the heating-up time
Equal heating rate, electric heating conversion efficiency integrate the Electrothermal Properties parameters such as coefficient of heat transfer, radiant heat transfer accounting to evaluate material electric heating
The quality of performance.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
In the technical scope disclosed by the present invention, any changes or substitutions that can be easily thought of by anyone skilled in the art,
It should be covered by the protection scope of the present invention.
Claims (10)
1. a kind of device for measuring graphene film thermo electric material Electrothermal Properties, which is characterized in that including electric control system, survey
Test system and data collection and processing system；
The electric control system is for exporting constant current or constant voltage；
The test macro is used to obtain the electric current, voltage and temperature information of graphene film layer sample, the test macro packet
Electrothermal Properties thermometric room is included, Electrothermal Properties thermometric room is equipped with thermocouple；
The data collection and processing system is used to collect electric current, voltage and the temperature information that the test macro obtains and carries out
Processing, obtains the Electrothermal Properties data of graphene film thermo electric material.
2. the device of measurement graphene film thermo electric material Electrothermal Properties according to claim 1, which is characterized in that described
The outer surface of Electrothermal Properties thermometric room is equipped with the insulation material layer of isolation Electrothermal Properties thermometric indoor and outdoor heat exchange.
3. the device of measurement graphene film thermo electric material Electrothermal Properties according to claim 2, which is characterized in that described
The inner surface of insulation material layer is equipped with heat radiation reflectance coating, and the heat radiation that film layer sample generates when preventing test is outside
Transmitting.
4. the device of measurement graphene film thermo electric material Electrothermal Properties according to claim 3, which is characterized in that described
Heat radiation reflectance coating is silver coating.
5. the device of measurement graphene film thermo electric material Electrothermal Properties according to claim 1, which is characterized in that described
Electrothermal Properties thermometric room includes top surface, side and bottom surface, and film layer sample is set to the bottom surface.
6. the device of measurement graphene film thermo electric material Electrothermal Properties according to claim 5, which is characterized in that described
It is equipped with one group of thermocouple in top surface, side, bottom surface and space away from bottom surface certain distance, the film layer sample is uniformly provided with
Four groups of thermocouples.
7. the device of measurement graphene film thermo electric material Electrothermal Properties according to claim 1, which is characterized in that described
Data collection and processing system includes temperature polling instrument and control and processing unit, and the temperature polling instrument is for recording the electricity
The real time temperature of thermocouple, the control are used for real-time display electric current, voltage, temperature information with processing unit.
8. the device of measurement graphene film thermo electric material Electrothermal Properties according to claim 7, which is characterized in that described
Temperature polling instrument is connect with the thermocouple, and the temperature polling instrument can record the real-time of the temperature measuring point of the thermocouple simultaneously
Temperature.
9. measuring the device of graphene film thermo electric material Electrothermal Properties according to claim 2 to 8, which is characterized in that
The film layer sample is equipped with heated object, and the heated object is Electrothermal Properties thermometric room air or fluid liquid.
10. a kind of method for measuring graphene film thermo electric material Electrothermal Properties, which is characterized in that utilize claim 1 to 9 times
The device that graphene film thermo electric material Electrothermal Properties are measured described in one measures, comprising the following steps:
Step 1: arrangement Electrothermal Properties thermometric room selects heated object, film layer sample is put into Electrothermal Properties thermometric room,
It selects the quantity of thermocouple and is arranged by requirement of experiment；
Step 2: connection circuit starts experiment test；Disconnecting circuit after the heating stipulated time cools down the stipulated time, is tested
The voltage of film layer sample, electric current and temperature measuring point temperature in the process；
Step 3: voltage, electric current and the temperature measuring point temperature data of processing film layer sample obtain the electric heating ginseng of film layer sample
Number.
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