CN107621477A - A kind of Harmonic Method hydrogel testing device for measuring thermal conductivity and method - Google Patents

A kind of Harmonic Method hydrogel testing device for measuring thermal conductivity and method Download PDF

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CN107621477A
CN107621477A CN201710786916.8A CN201710786916A CN107621477A CN 107621477 A CN107621477 A CN 107621477A CN 201710786916 A CN201710786916 A CN 201710786916A CN 107621477 A CN107621477 A CN 107621477A
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copper rod
hydrogel
thermal conductivity
heating process
detector
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杨诺
臧剑锋
郭汝磊
唐妮
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Huazhong University of Science and Technology
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Huazhong University of Science and Technology
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Abstract

The invention belongs to material thermal conductivity field of measuring technique, and disclose a kind of Harmonic Method hydrogel testing device for measuring thermal conductivity, including detector, precision resistance case, signal generator, voltage follower and lock-in amplifier, the detector includes container, supporting plate, electrode and METAL HEATING PROCESS silk, the supporting plate is shelved on the top of the container, the electrode is arranged in the supporting plate, and the electrode includes more copper rods, and the lower end of all copper rods is linked together by the METAL HEATING PROCESS silk;Copper rod a connection signal generators, copper rod b and copper rod c are all connected with first voltage follower, copper rod d connection precision resistance casees, the precision resistance case connects second voltage follower and the signal generator respectively, and the first voltage follower is connected with the second voltage follower with the lock-in amplifier.The present invention can accurately, easily measure the thermal conductivity of hydrogel using Harmonic Method.

Description

A kind of Harmonic Method hydrogel testing device for measuring thermal conductivity and method
Technical field
The invention belongs to material thermal conductivity field of measuring technique, more particularly, to a kind of Harmonic Method hydrogel thermal conductivity Test device and method.
Background technology
Hydrogel is the macroscopical macromolecular material being made up of the crosslinking polymer network comprising a large amount of water (70-99wt%) Material.The main component of our human bodies is exactly a kind of hydrogel.Hydrogel has good pliability, reliable in mechanical performance and bio-compatible Etc. characteristic, therefore it is considered as the optimal material for manufacturing flexibility/wearable electronic device of new generation.This respect have it is many have open The example of hair property, such as the stretchable transparent touch-sensitive panel based on aqueous ionomer gel, the intelligence that manipulates based on flexible hydro-gel are led Tip end, the double-network hydrogel optical fiber for strain transducer etc..It is well known that the radiating of electronic device has a strong impact on its property Energy and life-span.The thermal conductivity of hydrogel directly affects its heat dispersion, therefore the thermal conductivity for measuring hydrogel has significantly now Sincere justice.
The present invention is designed based on Harmonic Method (a kind of generally acknowledged thermal conductivity measurements).Early 20th century, Corbino has found after the alternating current that angular frequency is 1 ω is passed through into METAL HEATING PROCESS silk that metal wire both ends can be due to joule first Self-heating effect and produce the alternating voltage that angular frequency is 3 ω, this alternating voltage reflected the METAL HEATING PROCESS silk heat of itself Physical property.Due to used in measurement angular frequency be 3 ω harmonic signal, the method based on this principle be thus referred to as Harmonic Method or The ω methods of person 3.But because 3 ω voltages are very small (being approximately the one thousandth of 1 ω voltages of application), its measurement difficulty is very big, this One technology there is no application for a long time.Afterwards as the development of phase lock amplifying technology, 3 ω voltages are just accurately measured, this One method is also gradually received by people.Phase late 1980s, Cahill et al. propose the test based on the principle first The ω methods of slope -3 of body block of material thermal conductivity.By constantly developing, at present Harmonic Method be successfully applied to body block, liquid with And the measurement of the hot physical property of the material such as film (including thermal conductivity and specific heat capacity).
The basic functional principle of Harmonic Method can be described as follows:A wires are plated in body block sample surfaces, this root gold Category line will be used as heater and thermal detector simultaneously.The alternating current that angular frequency is 1 ω is passed through into this wires, due to joule Heat, the hot-fluid that frequency is 2 ω can be produced inside it.This hot-fluid can be by sample diffusion into environment.The complexity of diffusion It is relevant with the thermal conductivity of sample.Sample thermal conductivity is higher, and heat diffusion is easier, and the temperature rise of metal wire will be lower.Correspond to The hot-fluid fluctuated by 2 ω angular frequency, there is also the component fluctuated by 2 ω for the temperature of METAL HEATING PROCESS silk.In certain temperature model In the range of enclosing, the resistance and temperature line relationship of METAL HEATING PROCESS silk.Therefore there is also fluctuated by 2 ω for the resistance of METAL HEATING PROCESS silk Component.It is 3 ω's that this resistive component and 1 ω electric currents being passed through originally generate angular frequency at METAL HEATING PROCESS silk both ends together Voltage.As seen from the above description, this voltage reflects the temperature fluctuation amplitude of METAL HEATING PROCESS silk, and temperature fluctuation amplitude then reflects The thermal conductivity of sample.Therefore sample can be measured by measuring the amplitude for the voltage that metal wire both ends angular frequency is 3 ω Thermal conductivity.
A kind of Harmonic Method with independent probe is disclosed in Chinese utility model patent specification CN201535761U Thermal physical property of solid material test device.Independent probe is placed between two pieces of identical testing samples and forms Sanming City by this test device Control formula structure.The thermal conductivity that this device can not only measure solid material can also measure change pass of the thermal contact resistance with pressure System.But this method needs sample surfaces smoother to ensure that contact is good, and due to flexible cover layer be present in hot road, Data processing is more complicated.In addition a kind of Harmonic Detection is disclosed in Chinese utility model patent specification CN201041558Y Technology measures liquid thermal conductivity factor and the device of thermal diffusivity.This device arranges certain size and shape inside testing liquid Shape carries the miniature heater strip of insulating barrier, is heated using the cycle weak current with direct-flow offset weight, then according to heat wave The relation of vibration frequency and temperature change determines multiple thermal parameters such as thermal conductivity factor and the thermal diffusivity of liquid simultaneously.But this Device is more complicated, and is not suitable for measuring sample as hydrogel.
Existing Harmonic Method has many advantages.Harmonic Method can measure the diversified forms such as liquid, body block, film first Material, measurement range are wide.Other Harmonic Method due to overall temperature rise is small and METAL HEATING PROCESS silk as detector and thermal detector nor Often tiny, it is insensitive to radiation and convection current, thus largely reduces this two errors that may be brought.But Existing Harmonic Method is unsuitable for measuring the high flexible material of water content as hydrogel, and reason is mainly difficult to plate metal wire In this kind of material surface.Other existing method makes work due to needing metallization traces or making detector with other method Skill is complicated, and cost is higher, and has more requirement to sample.
The content of the invention
For the disadvantages described above or Improvement requirement of prior art, the invention provides a kind of survey of Harmonic Method hydrogel thermal conductivity Device and method is tried, the thermal conductivity of hydrogel can be simply and economically measured using Harmonic Method.
To achieve the above object, according to one aspect of the present invention, there is provided a kind of Harmonic Method hydrogel thermal conductivity test Device, it is characterised in that including detector, precision resistance case, signal generator, voltage follower and lock-in amplifier, wherein:
The detector includes container, supporting plate, electrode and METAL HEATING PROCESS silk, and the supporting plate is shelved on the container Top, the electrode is arranged in the supporting plate, and the electrode includes more copper rods, and institute is stretched into the lower end of every copper rod State in the container, for the Hydrogel contact in container, and the lower end of all copper rods passes through the metal Heater strip links together;
The copper rod of the detector includes copper rod a, copper rod b, copper rod c and copper rod d, copper rod a connection signal generators, copper rod B and copper rod c is all connected with first voltage follower, copper rod d connection precision resistance casees, and the precision resistance case connects the second electricity respectively Follower and the signal generator are pressed, the first voltage follower is mutually put with the second voltage follower with the lock Big device connection.
Preferably, the resistance of part of the METAL HEATING PROCESS silk between copper rod b and copper rod c is the Ω of 5 Ω~150.
Preferably, it is provided with insulating barrier on the METAL HEATING PROCESS silk.
Preferably, the METAL HEATING PROCESS silk is horizontally disposed with, its from container interior bottom surface distance L=(1/3~1/2) H, wherein H is the height of container inner wall.
According to another aspect of the present invention, additionally provide a kind of using the Harmonic Method hydrogel testing device for measuring thermal conductivity The method for measuring hydrogel thermal conductivity, it is characterised in that comprise the following steps:
1) hydrogel is made in container, and METAL HEATING PROCESS flight lead is distinguished at least 5mm from hydrogel upper and lower interface, then After hydrogel plastic, METAL HEATING PROCESS silk is just embedded in hydrogel;
2) lock-in amplifier is set, makes difference of its measurement signal for first voltage follower and second voltage follower, Then Regulate signal generator, to METAL HEATING PROCESS silk on apply angular frequency be 1 ω sinusoidal signal, set lock-in amplifier, make It measures the resistance of 1 ω sinusoidal signal, then adjustment precision resistance box so that the voltage magnitude that lock-in amplifier measurement obtains It is zero, now the resistance of precision resistance case and the resistance of detector are equal, so as to eliminate 1 ω at detector both ends sinusoidal letter Number, to obtain 3 ω sinusoidal signal;
3) sinusoidal signal of Regulate signal generator output so that the 3 ω voltage magnitudes V that lock-in amplifier measurement obtains For 1 ω voltage magnitudes V1/500~1/1000, keep signal generator output sinusoidal signal amplitude it is constant, change not Same frequency, measure 3 ω voltage magnitudes V, obtain 3 ω voltage magnitudes VWith the relation of corresponding signal frequency, so as to utilize with Lower formula obtains thermal conductivity k:
Wherein VIt is the 1 ω signals that detector both ends measure, β is the temperature-coefficient of electrical resistance of METAL HEATING PROCESS silk in detector, R is detector resistance, and l is the length of part of the METAL HEATING PROCESS silk between copper rod b and copper rod c, and slope is 3 ω voltage magnitudes VSlope with taking the section that the linearity is best in the corresponding signal frequency relation after natural logrithm.
Preferably, the frequency for the sinusoidal signal that the signal generator applies is 1~100Hz.
In general, by the contemplated above technical scheme of the present invention compared with prior art, it can obtain down and show Beneficial effect:
1) panel detector structure that the present invention uses is simple, and cost is cheap, therefore can be with disposable.
2) detector of the invention forms the four lines measuring method using four copper rods, can eliminate contact resistance in test circuit Influence, improve measuring accuracy.
3) present invention passes through signal generator (be used to applying electric current that angular frequency is 1 ω to detector), precision resistance case (being used to eliminate the influence that 1 ω current signals measure 3 ω current signals), voltage follower circuit (is used to measurement signal being total to Ground simultaneously increases measuring circuit input resistance, improves measuring accuracy), lock-in amplifier (is used to extract 1 ω and 3 ω voltage signals), The thermal conductivity of hydrogel can be accurately, easily measured using Harmonic Method.
Brief description of the drawings
Fig. 1 is the structural representation of the present invention;
Fig. 2 is the structural representation of detector in the present invention.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, it is right below in conjunction with drawings and Examples The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and It is not used in the restriction present invention.As long as in addition, technical characteristic involved in each embodiment of invention described below Conflict can is not formed each other to be mutually combined.
Reference picture 1, Fig. 2, a kind of Harmonic Method hydrogel testing device for measuring thermal conductivity, including detector, precision resistance case, signal Generator, voltage follower and lock-in amplifier, wherein,
The detector includes container 3, supporting plate 2, electrode 1 and METAL HEATING PROCESS silk 4, and the supporting plate 2 is shelved on described The top of container 3, the electrode 1 are arranged in the supporting plate 2, and the electrode 1 includes more copper rods, under every copper rod End stretch into it is described be arranged in the container 3, for the Hydrogel contact in container 3, and the lower end of all copper rods Linked together by the METAL HEATING PROCESS silk 4;
The copper rod of the detector includes copper rod a, copper rod b, copper rod c and copper rod d, copper rod a connection signal generators, copper rod B and copper rod c is all connected with first voltage follower, copper rod d connection precision resistance casees, and the precision resistance case connects the second electricity respectively Follower and the signal generator are pressed, the first voltage follower is mutually put with the second voltage follower with the lock Big device connection.
Further, the resistance of part of the METAL HEATING PROCESS silk 4 between copper rod b and copper rod c is the Ω of 5 Ω~150.
Further, it is provided with insulating barrier on the METAL HEATING PROCESS silk 4.
Further, the METAL HEATING PROCESS silk 4 is horizontally disposed, its from container 3 inner bottom surface distance L=(1/3~1/2) H, its Middle H is the height of the inwall of container 3.
The invention provides a kind of device that hydrogel thermal conductivity is tested using Harmonic Method, the device includes:Disposable thermal Conductance detector, the surface of metal wire integrally deposits one layer of very thin dielectric film (ratio in the disposable thermal conductance detector The thick silica insulation film such as 100nm, but can also not have to this layer of dielectric film of deposition for nonconducting hydrogel sample). Because panel detector structure is simple, cost is cheap, therefore can be with disposable.
The signal generator of the present invention is used to apply electric current of the angular frequency for 1 ω to detector, and precision resistance case is for disappearing Except the influence that 1 ω current signals are measured 3 ω current signals, voltage follower circuit is used to measurement signal being total to ground and increases survey Circuit input resistance to be measured, improves measuring accuracy, lock-in amplifier is used to extract 1 ω and 3 ω voltage signals, in addition, for convenience, A universal meter can also individually be added again to measure 1 ω signals.
The METAL HEATING PROCESS silk 4 of the detector of the present invention uses 10~40um of diameter, 20~100mm of length platinum filament, length Selection principle be make METAL HEATING PROCESS silk 4 two harmonic measuring points (i.e. resistance between copper rod b and copper rod c) be in 5~150 Ω it Between, if hydrogel is conductive, needs to deposit a very thin layer insulating on its surface, be platinum filament from the main reason for platinum filament Chemical property is stable, and good linearity in the relation of resistance and temperature, and four copper rods form the four lines measuring method, can eliminate test electricity The influence of contact resistance in road, measuring accuracy is improved, if hydrogel is conductive, it is also desirable to insulating barrier is made on copper rod, but is not had There is the requirement such as thickness, supporting plate 2 is used to install copper rod, can extend into copper rod and hold in the container 3 of hydrogel sample, container 3 For holding hydrogel.Four copper rods are fixed in supporting plate 2, and the level of METAL HEATING PROCESS silk 4 is welded on four copper rods, supporting plate 2 are fixed on container 3.
According to another aspect of the present invention, additionally provide a kind of using the Harmonic Method hydrogel testing device for measuring thermal conductivity The method for measuring hydrogel thermal conductivity, comprises the following steps:
1) hydrogel is made in container 3, and METAL HEATING PROCESS silk 4 is distinguished at least 5mm apart from hydrogel upper and lower interface, Then after hydrogel plastic, METAL HEATING PROCESS silk 4 is just embedded in hydrogel;
2) 2) lock-in amplifier is set, make difference of its measurement signal for first voltage follower and second voltage follower Value, then Regulate signal generator, to METAL HEATING PROCESS silk 4 on apply the sinusoidal signal that angular frequency is 1 ω, set lock mutually to amplify Device, it is set to measure the resistance of 1 ω sinusoidal signal, then adjustment precision resistance box so that the electricity that lock-in amplifier measurement obtains Pressure amplitude value is zero, and now the resistance of precision resistance case and the resistance of detector are equal, so as to eliminate 1 ω at detector both ends just String signal, to obtain 3 ω sinusoidal signal;
3) sinusoidal signal of Regulate signal generator output so that the 3 ω voltage magnitudes V that lock-in amplifier measurement obtains For 1 ω voltage magnitudes V1/500~1/1000, keep signal generator output sinusoidal signal amplitude it is constant, change not Same frequency, measure 3 ω voltage magnitudes V, obtain 3 ω voltage magnitudes VWith the relation of corresponding signal frequency, so as to utilize with Lower formula obtains thermal conductivity k:
Wherein VIt is the 1 ω signals that detector both ends measure, β is the resistance temperature system of METAL HEATING PROCESS silk 4 in detector Number, R is detector resistance, and l is the length of part of the METAL HEATING PROCESS silk 4 between copper rod b and copper rod c, and slope is 3 ω voltages Amplitude VSlope with taking the section that the linearity is best in the corresponding signal frequency relation after natural logrithm.
Further, the frequency for the sinusoidal signal that the signal generator applies is 1~100Hz.
As it will be easily appreciated by one skilled in the art that the foregoing is merely illustrative of the preferred embodiments of the present invention, not to The limitation present invention, all any modification, equivalent and improvement made within the spirit and principles of the invention etc., all should be included Within protection scope of the present invention.

Claims (6)

1. a kind of Harmonic Method hydrogel testing device for measuring thermal conductivity, it is characterised in that including detector, precision resistance case, signal hair Raw device, voltage follower and lock-in amplifier, wherein:
The detector includes container, supporting plate, electrode and METAL HEATING PROCESS silk, and the supporting plate is shelved on the top of the container End, the electrode are arranged in the supporting plate, and the electrode includes more copper rods, described in the lower end of every copper rod is stretched into In container, for the Hydrogel contact in container, and the lower end of all copper rods is connected to by the METAL HEATING PROCESS silk Together;
The copper rod of the detector includes copper rod a, copper rod b, copper rod c and copper rod d, copper rod a connection signal generators, copper rod b and Copper rod c is all connected with first voltage follower, copper rod d connection precision resistance casees, and the precision resistance case connects second voltage respectively Follower and the signal generator, the first voltage follower mutually amplify with the second voltage follower with the lock Device connects.
2. a kind of Harmonic Method hydrogel testing device for measuring thermal conductivity according to claim 1, it is characterised in that the metal adds The resistance of part of the heated filament between copper rod b and copper rod c is the Ω of 5 Ω~150.
3. a kind of Harmonic Method hydrogel testing device for measuring thermal conductivity according to claim 1, it is characterised in that the metal adds Insulating barrier is provided with heated filament.
4. a kind of Harmonic Method hydrogel testing device for measuring thermal conductivity according to claim 1, it is characterised in that the metal adds Heated filament is horizontally disposed with, and, from container interior bottom surface distance L=(1/3~1/2) H, wherein H is the height of container inner wall for it.
5. one kind uses any Harmonic Method hydrogel testing device for measuring thermal conductivity measurement hydrogel thermal conductivity in Claims 1 to 4 The method of rate, it is characterised in that comprise the following steps:
1) hydrogel is made in container, and METAL HEATING PROCESS flight lead is distinguished at least 5mm from hydrogel upper and lower interface, then water-setting After glue plastic, METAL HEATING PROCESS silk is just embedded in hydrogel;
2) lock-in amplifier is set, makes difference of its measurement signal for first voltage follower and second voltage follower, then Regulate signal generator, to METAL HEATING PROCESS silk on apply angular frequency be 1 ω sinusoidal signal, set lock-in amplifier, make its survey 1 ω sinusoidal signal is measured, then the resistance of adjustment precision resistance box so that the voltage magnitude that lock-in amplifier measurement obtains is Zero, now the resistance of precision resistance case and the resistance of detector are equal, so as to eliminate 1 ω at detector both ends sinusoidal signal, To obtain 3 ω sinusoidal signal;
3) sinusoidal signal of Regulate signal generator output so that the 3 ω voltage magnitudes V that lock-in amplifier measurement obtainsFor 1 ω Voltage magnitude V1/500~1/1000, keep signal generator output sinusoidal signal amplitude it is constant, change different frequencies Rate, measure 3 ω voltage magnitudes V, obtain 3 ω voltage magnitudes VWith the relation of signal frequency, so as to using below equation obtain Thermal conductivity k:
<mrow> <mi>k</mi> <mo>=</mo> <mo>-</mo> <mfrac> <mrow> <msubsup> <mi>V</mi> <mrow> <mn>1</mn> <mi>&amp;omega;</mi> </mrow> <mn>3</mn> </msubsup> <mi>&amp;beta;</mi> </mrow> <mrow> <mn>8</mn> <mi>&amp;pi;</mi> <mi>R</mi> <mi>l</mi> <mo>&amp;CenterDot;</mo> <mi>s</mi> <mi>l</mi> <mi>o</mi> <mi>p</mi> <mi>e</mi> </mrow> </mfrac> </mrow>
Wherein VIt is the 1 ω signals that detector both ends measure, β is the temperature-coefficient of electrical resistance of METAL HEATING PROCESS silk in detector, and R is to visit Device resistance is surveyed, l is the length of part of the METAL HEATING PROCESS silk between copper rod b and copper rod c, and slope is 3 ω voltage magnitudes VWith Take the slope in the section that the linearity is best in the corresponding signal frequency relation after natural logrithm.
6. according to the method for claim 5, it is characterised in that the frequency for the sinusoidal signal that the signal generator applies is 1~100Hz.
CN201710786916.8A 2017-09-04 2017-09-04 A kind of Harmonic Method hydrogel testing device for measuring thermal conductivity and method Pending CN107621477A (en)

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CN110044957A (en) * 2019-04-24 2019-07-23 南京大学 Measuring circuit, measuring system and thermal physical property parameter measurement method
CN113702422A (en) * 2021-08-26 2021-11-26 西安交通大学 Device and method for measuring fluid thermal conductivity by double-section platinum wire method
CN113820355A (en) * 2021-08-31 2021-12-21 东南大学 3 omega test bed and test method thereof

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CN110044957A (en) * 2019-04-24 2019-07-23 南京大学 Measuring circuit, measuring system and thermal physical property parameter measurement method
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Application publication date: 20180123