CN105954319B - The device and method that energy-saving heat-insulating material thermal conductivity scene is accurately tested - Google Patents
The device and method that energy-saving heat-insulating material thermal conductivity scene is accurately tested Download PDFInfo
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Abstract
The present invention provides a kind of energy-saving heat-insulating material thermal conductivity device and method that scene is accurately tested, and belongs to energy-saving heat-insulating material thermal characteristics technical field of measurement and test.The device includes self-adaptation type thermal response detector, electrical signal collection module and data processing module.In-site measurement is carried out to energy-saving heat-insulating material using the device, obtains the fundamental voltage (V of sample1ω)yWith third harmonic voltage (V3ω)y；Using thermal response temperature measuring unit temperature-coefficient of electrical resistance β, core strip length l, the substrate thermal conductivity k demarcated before usingsAnd fundamental voltage (the V of sample1ω)yWith third harmonic voltage (V3ω)yCalculate the thermal conductivity of sample.The device and method can overcome the defects of stability of former experimental system signal is not high, measurement resistance accuracy is not high, differential signal is bad, ensure that the scene of heat-barrier material thermal conductivity is accurate and measure.
Description
Technical field
The present invention relates to energy-saving heat-insulating material thermal characteristics technical field of measurement and test, particularly relate to a kind of energy-saving heat-insulating material thermal conductivity
The device and method that rate scene is accurately tested.
Background technology
Heat-barrier material is a kind of energy-saving material playing apparent inhibition to convection current heat transfer.Heat-barrier material utilizes internal holes
The air (thermal conductivity only 0.026W/m K) being limited in shape structure forms the lower material entirety of thermal conductivity, heat-insulated to reach
Energy-efficient effect.Due to having preferable heat-insulated, cold insulation characteristic, heat-barrier material is widely used in building, metallurgy, chemical industry, electricity
The all trades and professions such as power, oil, machinery, military project, communications and transportation, storage.It is seized of highly important in Chinese national economy
Effect.From the food and clothing of people live row all occupy to modern advanced industrial such as aerospace, electronics, atomic energy etc. it is highly important
Status.
Thermal conductivity is one particularly important thermal physical property parameter of porous heat insulation material, represents porous material to a certain extent
Energy-efficient performance.Therefore, scene is obtained, accurate thermal conductivity has important guidance to make the design and evaluation of porous material
With.Usually there is certain deviation and cannot be satisfied in existing thermal characteristics test method and instrument when being tested towards heat-barrier material
The actual demand of on-the-spot test.The precision when measuring heat-insulating material is still to be improved with Hot-strip Method for heat-pole method.Flicker method and photo-thermal
Although it is accurate that bounce technique measures, there is certain requirement to measured material, be not suitable for the on-the-spot test of insulating porous material.Generally acknowledge
Thermal characteristic measurement be accurately protection hot plate method and Adsorbent By Using Transient Plane Source Technique.But protection hot plate method measurement period compared with
It is long, it is desirable that sample size is larger, cannot achieve the test at scene.Adsorbent By Using Transient Plane Source Technique needs replacing not when testing different materials
Same detector, and the triviality of test must be increased in advance by processing such as material cutting, surface polishings.Harmonic Detection method
It is advantageous compared with other methods in terms of minute yardstick material thermal characteristic measurement, but for heat-barrier material measure when, existing detection
Device cannot achieve live in-situ test, and existing experimental circuit can not ensure the accurate test of the extremely low sample of thermal conductivity.
The prior art (ZL200910242362.0) uses Harmonic Detection technical testing thermal conductivity, the device to measure solid material
It is between independent probe is clipped in two pieces of identical samples to be tested when material, this operating feature cannot achieve energy-saving heat-insulating material
The live in-situ test of (especially construction material).In addition, electrical signal collection system used in the prior art does not take original signal
It is filtered, the type selecting of the critical pieces such as power supply and difference amplifier is rougher, and resistance terminal is " two collimation methods "
Test, these factors will influence the precision measured.
Invention content
The technical problem to be solved in the present invention is to provide the devices that a kind of energy-saving heat-insulating material thermal conductivity scene is accurately tested
And method.
The device includes that self-adaptation type thermal response detector, electrical signal collection module and data processing module, electric signal are adopted
Collection module is connect with the respective end of adaptive thermal response detector, for generating heated current, measuring and recording under multiple frequencies
Third harmonic voltage among thermal response temperature measuring unit between two pads and natural logrithm frequency data and fundamental voltage average value；Number
According to processing module be used for using under multiple frequencies among thermal response temperature measuring unit between two pads third harmonic voltage with it is naturally right
Number frequency data and fundamental voltage average value, calculate the thermal conductivity of sample to be tested.
Wherein, self-adaptation type thermal response detector includes substrate, thermal response temperature measuring unit, abrasion-proof insulating protective film, first
Current feed part, the second current feed part, first voltage lead part and second voltage lead part, substrate are used to support thermal response survey
Warm unit and abrasion-proof insulating protective film, thermal response temperature measuring unit are attached by three kinds of Van der Waals force, diffusion attachment, mechanical snap effects
It on the top surface of substrate, according to the heated core component for increasing principle as temperature-sensitive of metallic resistance, is sandwiched in abrasion-proof insulating protection
Between film and substrate, the first current feed part, the second current feed part, first voltage lead part and the welding of second voltage lead part
In on four pads of thermal response temperature measuring unit end, abrasion-proof insulating protective film is covered in the other side of thermal response temperature measuring unit, resistance to
Insulating protective film is ground, thermal response temperature measuring unit surface is overlying on, for slowing down and frictional dissipation when sample engaged test, extension heat
Respond the service life of temperature measuring unit；
Electrical signal collection module includes signal generator, the first high-precision meter amplifier, the amplification of the second high-precision meter
Device, high precision DC power supply, lock-in amplifier, adjustable resistance, the first current feed end, the second current feed end, first voltage
Lead end and second voltage lead end, the first current feed part are connect with signal generator by the first current feed end, and second
Current feed part is connected to the ground with adjustable resistance by the second current feed end, first voltage lead part and first voltage lead end
Electrical connection, second voltage lead part are electrically connected with second voltage lead end, and the first high-precision meter amplifier contains eight ports,
Middle second port-IN and third port+IN is respectively connected to first voltage lead part and second voltage lead part, the 4th port-
Vs, the 7th port+Vs, the 8th port REF are respectively connected to the cathode port, positive port and ground terminal of high precision DC power supply
Mouthful；6th port OUTPUT exports the first differential wave to the first differential wave input terminal A of lock-in amplifier；Second high-precision
Instrument amplifier contains eight ports, and wherein second port-IN and third port+IN are respectively connected to the both ends of adjustable resistance, the
Four port-Vs, the 7th port+Vs, the 8th port REF are respectively connected to the cathode port of high precision DC power supply, positive port
And grounding ports；6th port OUTPUT exports the second differential wave to the second differential wave input terminal B of lock-in amplifier；Lock
The third input terminal of phase amplifier is connected to the first output end of signal generator.
Thermal response temperature measuring unit is that metal faciola side connects four bond pad shapes, wherein metal faciola length is in 8~40mm ranges
Interior, for width in 8~100 μ ms, thermal response temperature measuring unit is that chromium/platinum, chrome gold or chromium/nickel clad, composite bed thickness are
10nm/200nm。
Substrate is BK7 optical glass or PMMA acrylic boards, and the polished processing of substrate meets 10 angstroms of surface roughness, parallel
5 rads of degree, the thickness of matrix is within the scope of 1~3mm.
First current feed part, the second current feed part, first voltage lead part and second voltage lead part are enamel-cover copper
Line, abrasion-proof insulating protective film are silicon nitride.
Self-adaptation type thermal response detector is made by following methods：First, substrate is placed in deionized water, through ultrasonic wave
Cleaning 15 minutes；Then, substrate is placed in painting AZ6130 photoresists, 2000 revs/min of glue spreader rotating speed, gluing on gluing machine
Thickness is 2.4 μm, and type used is positive photoresist；It is dried 10 minutes under 95 DEG C of environment after substrate gluing；Reapply uv-exposure 15 seconds
After use tetramethylammonium hydroxide：Water=1:4 developing liquid developings show four pad structure figures of spill thermal response temperature measuring unit
Case；Wherein, it is 10 in vacuum degree if BK7 substrate of glass-7Torr, Ar flow are 8sccm, and pressure is first under the conditions of being 2mTorr
Magnetron sputtering 10nm chromium laminating layer and 200nm metal layers afterwards, if PMMA substrates, using chemical vapor deposition 10nm chromium laminating layers
And 200nm metal layers；In next step, it if BK7 substrate of glass, is removed photoresist stripping with acetone soak mode, by being cleaned by ultrasonic, drying
Afterwards, it is high-visible to connect four bond pad shapes for metal faciola side；If PMMA substrates, are removed photoresist using dilute alkaline soln；In next step, with resistance to height
Warm insulating tape covers four pad positions of thermal response temperature measuring unit, and Si is deposited by chemical gas-phase deposition method3N4Protection
Layer, main technologic parameters：Environment temperature is 100 DEG C, pressure 900mT, SiH4With NH3The flow of gas be respectively 300sccm with
200sccm often plates 50nm and shuts down postcooling 5 minutes, recycled by 6 times, form the Si of 300nm thickness3N4Film；Heat will be attached with
The substrate for responding temperature measuring unit and abrasion-proof insulating protective film is polished by cutting, if BK7 substrates, then in thermal response temperature measuring unit
Four pads on weld the first current feed part, the second current feed part, first voltage lead part and second voltage lead part,
If PMMA substrates, the first current feed part, the second current feed part, first voltage lead are connected by the way of elargol bonding
Part and second voltage lead part.
Electrical signal collection module power output end be arranged the first filter capacitor, the second filter capacitor, third filter capacitor,
4th filter capacitor, the 5th filter capacitor, the 6th filter capacitor, the 7th filter capacitor, the 8th filter capacitor, the 9th filtered electrical
Appearance, the tenth filter capacitor, the 11st filter capacitor and the 12nd filter capacitor, wherein the first filter capacitor, the second filtered electrical
Appearance, the 7th filter capacitor, the 8th filter capacitor are the filter capacitor of capacitance 10pF types.Third filter capacitor C3, the 4th
Filter capacitor C4, the 9th filter capacitor C9, the tenth filter capacitor C10 are the filter capacitor of 1 μ F types of capacitance.5th filtering
Capacitance C5, the 6th filter capacitor C6, the 11st filter capacitor C11, the 12nd filter capacitor C12 are 100 μ F types of capacitance
Filter capacitor.
Using the method that the device carries out test heat-barrier material thermal conductivity, it is as follows：
Step A carries out in-site measurement using above-mentioned apparatus to heat-barrier material to be measured, obtains the fundamental wave electricity of heat-barrier material to be measured
Press (V1ω)yWith third harmonic voltage (V3ω)y；
Wherein, if detected materials are solid-state, the abrasion-proof insulating protective film side of self-adaptation type thermal response detector is directly pasted
In detected materials surface；If detected materials are liquid or powder, sample directly dripped with suction pipe on abrasion-proof insulating protective film, sample
Product cover subject to full thermal response temperature measuring unit, start next step；
By the first current feed part of adaptive thermal response detector, the second current feed part respectively with the first current feed
End, the electrical connection of the second current feed end, first voltage lead part, second voltage lead part and first voltage lead end, the second electricity
Voltage lead wires end is electrically connected；Thermal response temperature measuring unit is heated at first current feed end, the second current feed end；
Manually adjust adjustable resistance knob, until lock-in amplifier differential wave in 0.0004mV hereinafter, recording this
When resistance value be thermal response detector leveling resistance R0；
Increase signal generator output power, adaptive thermal response detector under predeterminated frequency is recorded by lock-in amplifier
First voltage lead part and second voltage lead part between fundamental voltage (V1ω)y, third harmonic voltage (V3ω)y；
Step B, using (V achieved above1ω)y、(V3ω)yAnd thermal response detector uses the preceding resistance temperature demarcated
The thermal conductivity k of degree factor beta, core strip length l, substrates, the thermal conductivity of sample is calculated using formula (1)；
In formula, kyThermal conductivity (the Wm of-heat-barrier material to be measured-1·K-1)；
ksThermal conductivity (the Wm of-substrate-1·K-1)；
Temperature-coefficient of electrical resistance (the K of β-thermal response detector-1)；
L-thermal response metal detector faciola length (m)；
V1ω- fundamental voltage (V)；
R0- thermal response detector leveling resistance (Ω)；
λ"—V3ωThe inverse of~ln ω slopes.
The above-mentioned technical proposal of the present invention has the beneficial effect that：
(1) it uses self-adaptation type thermal response detector directly to touch the testing scheme of heat-barrier material, it is special to overcome previous heat
The problem of detector of system safety testing device cannot be satisfied on-the-spot test ensures the scene in situ for realizing energy-saving heat-insulating material thermal conductivity
It measures；
(2) it uses a series of measures to improve and optimize electrical signal collection module, including selects high precision DC power supply (power supply
Voltage regulation factor≤0.5%, ripple are less than peak value≤10mV), increase by 6 pairs of capacitances and carry out at high frequencies and low frequency spur signal filtering
Reason selects high-precision meter amplifier, and being changed to four-wire method to adjustable resistance end measures.Former experimental system signal can be overcome
Stability is not high, measures the defects of resistance accuracy is not high, differential signal is bad, ensure that the accurate survey of heat-barrier material thermal conductivity
Amount.
Description of the drawings
Fig. 1 is the schematic device that the energy-saving heat-insulating material thermal conductivity scene of the present invention is accurately tested；
Fig. 2 is the knot of self-adaptation type thermal response detector in on-the-spot test energy-saving heat-insulating material thermal conductivity device shown in Fig. 1
Structure schematic diagram；
Fig. 3 is the operation of self-adaptation type thermal response detector on-the-spot test liquid or powder energy-saving heat-insulating material shown in Fig. 1
Figure；
Fig. 4 is self-adaptation type thermal response detector shown in Fig. 2, Fig. 3 along the sectional view in the faces A-A.
Wherein：11- substrates；12- thermal response temperature measuring units；13- abrasion-proof insulating protective films；1a- the first current feed parts；
1d- the second current feed parts；1b- first voltage lead parts；1c- second voltage lead parts；21- signal generators；22- first is high
Precision instrument amplifier；23- the second high-precision meter amplifiers；24- high precision DC power supplies；25- lock-in amplifiers；R1- can
Adjust resistance；The first current feeds of 2a- end；The second current feeds of 2d- end；2b- first voltage lead ends；2c- second voltage leads
End；The first filter capacitors of C1-；The second filter capacitors of C2-；C3- third filter capacitors；The 4th filter capacitors of C4-；C5- the 5th is filtered
Wave capacitance；The 6th filter capacitors of C6-；The 7th filter capacitors of C7-；The 8th filter capacitors of C8-；The 9th filter capacitors of C9-；
The tenth filter capacitors of C10-；The 11st filter capacitors of C11-；The 12nd filter capacitors of C12-.
Specific implementation mode
To keep the technical problem to be solved in the present invention, technical solution and advantage clearer, below in conjunction with attached drawing and tool
Body embodiment is described in detail.
The present invention provides a kind of energy-saving heat-insulating material thermal conductivity device and method that scene is accurately tested.
First, the present invention provides the devices that a kind of energy-saving heat-insulating material thermal conductivity scene is accurately tested.Fig. 1 is according to this
The schematic diagram of inventive embodiments on-the-spot test energy-saving heat-insulating material thermal conductivity device.Fig. 2 is adaptive in test device shown in Fig. 1
The structural schematic diagram of type thermal response detector.Fig. 3 is self-adaptation type thermal response detector on-the-spot test liquid or powder shown in Fig. 1
The operation diagram of energy-saving heat-insulating material.Fig. 4 is self-adaptation type thermal response detector shown in Fig. 2, Fig. 3 along the sectional view in the faces A-A.The dress
Set including：Self-adaptation type thermal response detector, electrical signal collection module and data processing module.Individually below to various pieces into
Row is described in detail.
Self-adaptation type thermal response detector
Self-adaptation type thermal response detector includes：Substrate 11, thermal response temperature measuring unit 12, abrasion-proof insulating protective film 13,
One current feed part 1a, the second current feed part 1d, first voltage lead part 1b and second voltage lead part 1c.
Thermal response temperature measuring unit 12 is attached to substrate 11 by three kinds of Van der Waals force, diffusion attachment, mechanical snap effects
On top surface.Thermal response temperature measuring unit 12 is " metal faciola side connects a four pads " shape.Lead part 1a~1d is welded in thermal response
On four pads of 12 end of temperature measuring unit.Abrasion-proof insulating protective film 13 is covered in the other side of thermal response temperature measuring unit 12, plays
It protects the thermal response temperature measuring unit 12 of hundred nanometer thickness and makes effect of its metal to external insulation.Preferably, substrate 11 is BK7
Optical glass or PMMA acrylic boards, to meet 10 angstroms of surface roughness, 5 rads of the depth of parallelism may be regarded as the polished processing of substrate
Smooth surface.The thickness of matrix 11 is within the scope of 1~3mm.Thermal response temperature measuring unit 12 is chromium/platinum, chrome gold or chromium/nickel
(10nm/200nm) composite layer, chromium can reinforce the combination of other metals and substrate 11 as fitting metal.Lead part 1a~1d is
Enamel covered wire.Metal faciola partial-length is within the scope of 8~40mm in thermal response temperature measuring unit 12, and width is in 8~100 μ ms
It is interior.Abrasion-proof insulating protective film 13 is silicon nitride, has good heat conduction, insulation and antiwear characteristic, can be with heat-barrier material to be measured
Good fit and reuse.
It should be noted that the manufacturing process of self-adaptation type thermal response detector also belongs to protection scope of the present invention.It is main
The method and step is wanted to include：(1) substrate 11 was placed in deionized water, through ultrasonic cleaning about 15 minutes；(2) substrate 11 is placed in gluing
AZ6130 photoresists, 2000 revs/min of glue spreader rotating speed are applied on machine, rubberization thickness is 2.4 μm, and type used is positive photoresist；(3)
It is dried 10 minutes under 95 DEG C of environment after 11 gluing of substrate, the solvent in the photoresist film applied is promoted to volatilize to increase glued membrane and glass
The adhesiveness of glass substrate surface；(4) using uv-exposure tetramethylammonium hydroxide is used after 15 seconds：Water=1:4 developing liquid developings are shown
Four pad structure patterns of spill thermal response temperature measuring unit 12 are shown；(5) it is 10 in vacuum degree if BK7 substrate of glass- 7Torr, Ar flow are 8sccm, and pressure is priority magnetron sputtering 10nm chromium laminating layer and 200nm metal layers under the conditions of 2mTorr,
If PMMA substrates, using chemical vapor deposition 10nm chromium laminating layer and 200nm metal layers；(6) it if BK7 substrate of glass, uses
Acetone soak mode is removed photoresist stripping, due to the good stickiness of chromium, thermal response temperature measuring unit 12 " metal faciola side connects four welderings
Disk " shape has been retained in well in BK7 substrate of glass, and after being cleaned by ultrasonic, drying, the shape is high-visible；If
PMMA is removed photoresist since acetones organic solvent can dissolve PMMA using dilute alkaline soln as substrate；(7) high-temperature insulation glue is used
Band covers four pad positions of thermal response temperature measuring unit 12, and protection is provided for next plated film；(8) it is formed sediment by chemical gaseous phase
Product method deposits Si3N4Protective layer, main technologic parameters：Environment temperature is 100 DEG C, pressure 900mT.SiH4With NH3Gas
Flow is respectively 300sccm and 200sccm, to prevent PMMA thermal deformations (105 DEG C of thermal denaturation temperature), often plates 50nm (10 minutes
Left and right) shut down postcooling 5 minutes, it is recycled by 6 times, forms the Si of 300nm thickness3N4Film, quality is good, can be clearly visible thin
Film reflects and blue light caused by reflection；(9) substrate 11 of thermal response temperature measuring unit 12 and abrasion-proof insulating protective film 13 will be attached with
It polishes by cutting, if BK7 substrates, then welding lead part 1a~1d on four pads of thermal response temperature measuring unit 12, if
For PMMA substrates, connecting lead wire part 1a~1d by the way of elargol bonding, this completes self-adaptation type thermal response detectors
Making.
First current feed part 1a is electrically connected with the first current feed end 2a of electrical signal collection module.Second current feed
Part 1d is electrically connected with the second current feed end 2d of electrical signal collection module.First voltage lead part 1b and electrical signal collection module
First voltage lead end 2b electrical connection.The second voltage lead end 2c electricity of second voltage lead part 1c and electrical signal collection module
Connection.Two current feed end 2a, 2d periods applied weak periodical sinusoidal current to thermal response temperature measuring unit 12, passed to electricity and generated coke
It has burning ears and asymmetricly heats substrate 11 and heat-barrier material to be measured along both sides, two voltage lead end 2b, 2c constitute voltage circuit access
Electrical signal collection module.
Electrical signal collection module
Electrical signal collection module is set to control host, measures and records default for heat wave detection-response theory under frequency domain
The third harmonic voltage at 12 both ends of thermal response temperature measuring unit and natural logrithm frequency in self-adaptation type thermal response detector under frequency
Curve V3ωFundamental voltage average value V under~ln ω, each frequency3ω。
Fig. 1 provides the circuit diagram of electrical signal collection module of the present invention, and electrical signal collection module includes：Signal generator 21,
First high-precision meter amplifier 22, the second high-precision meter amplifier 23, high precision DC power supply 24, lock-in amplifier 25,
Adjustable resistance R1, the first current feed end 2a, the second current feed end 2d, first voltage lead end 2b and second voltage lead end
2c；For ensure instrument amplifier efficient operation, power output end be added it is a series of for high frequency, low frequency spur signal filter
Capacitance specifically contains：First filter capacitor C1, the second filter capacitor C2, third filter capacitor C3, the 4th filter capacitor C4,
Five filter capacitor C5, the 6th filter capacitor C6, the 7th filter capacitor C7, the 8th filter capacitor C8, the 9th filter capacitor C9, the tenth
Filter capacitor C10, the 11st filter capacitor C11, the 12nd filter capacitor C12.In general, the electrical signal collection module packet
It includes heated current and circuit and circuitry for signal measurement is provided.
Wherein, heated current provides circuit, the first current feed end 2a and the second current feed end 2d respectively with it is adaptive
The first current feed part 1a, the second current feed part 1d electrical connections for answering type thermal response detector, for being thermal response thermometric list
Member 12 provides weak periodical sinusoidal signal, including：Signal generator 21 and adjustable resistance R1, wherein self-adaptation type thermal response is visited
The the first current feed part 1a for surveying device is connect with signal generator 21 by the first current feed end 2a, and self-adaptation type thermal response is visited
The the second current feed part 1d and adjustable resistance R1 for surveying device is connected to the ground by the second current feed end 2d.Signal generator 21
Output end exports the ac voltage signal that angular frequency is ω；The ac voltage signal is in circuit through multiple impedance original papers from turn
Become current signal, which drives the thermal response temperature measuring unit 12 and adjustable electric of self-adaptation type thermal response detector successively
Hinder R1.
Circuitry for signal measurement, first voltage lead end 2b and second voltage lead end 2c are also rung with self-adaptation type heat respectively
First voltage lead part 1b, the 1c electrical connections of second voltage lead part for answering detector, for measuring thermal response temperature measuring unit 12
Fundamental voltage V1ωAnd third harmonic voltage V3ω, including：First high-precision meter amplifier 22, the second high-precision meter amplifier
23, filter capacitor C1~C12, high precision DC power supply 24 and lock-in amplifier 25, wherein：
First high-precision meter amplifier 22 contains eight ports, and second port-IN and third port+IN are separately connected
First voltage lead part 1b, second voltage lead part 1c to thermal response temperature measuring unit 12 are used for thermal response temperature measuring unit 12
The voltage signal at both ends is converted to the first differential wave；Its 4th port-Vs, the 7th port+Vs, the 8th port REF connect respectively
It is connected to the cathode port, positive port and grounding ports of high precision DC power supply 24；Its 6th port OUTPUT outputs first are poor
Signal is moved to the first differential wave input terminal A of lock-in amplifier 25；
Second high-precision meter amplifier 23 contains eight ports, and second port-IN and third port+IN are separately connected
To the both ends of adjustable resistance R1, for the voltage signal at the both ends adjustable resistance R1 to be converted to the second differential wave；Its 4th end
Mouthful-Vs, the 7th port+Vs, the 8th port REF be respectively connected to the cathode port of high precision DC power supply 24, positive port and
Grounding ports；Its 6th port OUTPUT exports the second differential wave to the second differential wave input terminal B of lock-in amplifier 25；
Lock-in amplifier 25, the first differential wave input terminal A are connected to the 6th of the first high-precision meter amplifier 22
Port OUTPUT, is used for：Third harmonic voltage is acquired and calculates, which is that the first differential wave and second are differential
The virtual value of the third-harmonic component of the difference of signal；Its second differential wave input terminal B is connected to the second high-precision meter and puts
6th port OUTPUT of big device 23, for acquiring and calculating fundamental voltage, which is the primary of the second differential wave
The virtual value of harmonic wave；
Due to it is actually measured be the faint voltage harmonic signal of thermal response temperature measuring unit 12, to ensure faint electricity
The accuracy and stability of signal measurement must use high-performance component combination capacitance elimination clutter in circuit.The one of the present invention
A aspect is to propose improvement and the optimisation technique scheme of circuit.Specifically, original difference amplifier end AMP03 is replaced with
The higher instrument amplifier AD620 of precision.Selection ± 15V high-precision 4NIC-X30 DC power supplies are put as the first high-precision meter
The power supply of 22 and second high-precision meter amplifier 23 of big device.By this adjustment, line-voltage regulation is less than or equal to
0.5%, ripple peak value is less than 10mV.First filter capacitor C1, the second filter capacitor C2, the 7th filter capacitor C7, the 8th filtering
Capacitance C8 is the filter capacitor of capacitance 10pF types.Third filter capacitor C3, the 4th filter capacitor C4, the 9th filter capacitor
C9, the tenth filter capacitor C10 are the filter capacitor of 1 μ F types of capacitance.5th filter capacitor C5, the 6th filter capacitor C6,
11st filter capacitor C11, the 12nd filter capacitor C12 are the filter capacitor of 100 μ F types of capacitance.In this way so that signal
Measurement fluctuation amount is apparent small very much, and measuring triple-frequency harmonics undulate quantity under predeterminated frequency in measurement whole process is generally less than
0.0004mV (original system is 0.0024mV or less).
In addition increase line and so that adjustable resistance R1 is four-wire method mode, as shown in Figure 1.Hence improve former measuring system
The measurement error that inevitable conductor resistance introduces when due to two line measurement of adjustable resistance.Table 1 lists before and after the improvement
Measure the variation of resistance.It can be seen that the measurement accuracy of resistance has obtained very big improvement, control errors are within 1 ‰.
The distribution of table 1 resistivity measurements and actual value
Wherein, in the present embodiment, precision is used to replace program-controlled resistor by the metal wound wire adjustable resistance R1 of 0.001 Ω.
In addition, the third input terminal of lock-in amplifier 25 is connected to the first output end of signal generator 21, for passing through
Differential Input Monitor Connector so that 25 measurement frequency of lock-in amplifier is consistent with 21 output voltage frequency of signal generator.
The abrasion-proof insulating protective film 13 of adaptive thermal response detector is in direct contact heat-insulated sample to be measured, signal generator
The ac voltage signal that 21 output angular frequencies are ω is automatically converted to current signal through entire circuit components, which uses
The thermal response temperature measuring unit 12 encapsulated in adjustable resistance R1 and self-adaptation type thermal response detector is driven in simultaneously, since joule is imitated
Answer, thermal response temperature measuring unit 12 generate two frequencys multiplication heat wave signal, thermal penetration depth of the heat wave in heat-barrier material to be measured with
Frequency at subtraction function relationship, put through the first high-precision meter respectively by the voltage signal of adjustable resistance R1 and thermal response temperature measuring unit 12
Big 22 and second high-precision meter amplifier 23 of device is changed into differential wave and amplification, inputs lock-in amplifier 25.Pass through locking phase
Amplifier 25 acquires the fundamental wave V of 12 feedback of thermal response temperature measuring unit1ωAnd harmonic signal V3ω, and then can get to be measured heat-insulated
The thermal conductivity of sample.Under normal circumstances, the third harmonic voltage component V that lock-in amplifier 25 detects3ωIt is its fundamental voltage V1ω
1/5000~1/1000 or so, limited by the limited dynamic memory of lock-in amplifier 25 itself, in order to accurately measure three times
Harmonic component V3ω, it is necessary to take difference channel to eliminate response temperature measuring unit 12 and the fundamental voltage signal V on adjustable resistance R11ω。
Data processing module
Data processing unit is equally set to control host, using following formula by known self-adaptation type thermal response detector
The thermal conductivity of middle substrate 11, the size of thermal response temperature measuring unit 12 calculate to be measured respectively in connection with fundamental voltage, third harmonic voltage
The thermal conductivity of heat-barrier material：
In formula, kyThermal conductivity (the Wm of-heat-barrier material to be measured-1·K-1)；
ksThermal conductivity (the Wm of-substrate 11-1·K-1)；
Temperature-coefficient of electrical resistance (the K of β-thermal response detector 12-1)；
L -12 metal faciola length (m) of thermal response detector；
V1ω- fundamental voltage (V)；
R012 leveling resistance (Ω) of-thermal response detector；
λ"—V3ωThe inverse of~ln ω slopes, the above parameter are parameter when testing heat-barrier material to be measured.
Based on the device that above-mentioned energy-saving heat-insulating material thermal conductivity scene is accurately tested, the present invention also provides it is a kind of it is energy saving every
The method that hot material thermal conductivity scene is accurately tested is related to a kind of based on self-adaptation type thermal response detector, improved signal
The technical solution of acquisition and processing circuit is realized to the accurate test in the scene of heat-barrier material thermal conductivity.At one of the present invention
In embodiment, this method includes：
Step A carries out in-site measurement using above-mentioned apparatus to heat-barrier material to be measured, obtains the fundamental wave electricity of heat-barrier material to be measured
Press (V1ω)yWith third harmonic voltage (V3ω)y；
The step can specifically include：
Sub-step A1, if detected materials are solid-state, by 13 side of abrasion-proof insulating protective film of self-adaptation type thermal response detector
Directly it is affixed on detected materials surface；If detected materials are liquid or powder, sample is directly dripped with suction pipe and is protected in abrasion-proof insulating
On film 13, sample covers subject to full thermal response temperature measuring unit 12, starts next step；
Sub-step A2 adopts first, second current feed part 1a, 1d of adaptive thermal response detector with electric signal respectively
Two current feed end 2a, 2d electrical connections of collection module, first, second voltage lead part 1b, 1c and electrical signal collection module
Two voltage lead end 2b, 2c electrical connections；Two current feed end 2a, 2d of electrical signal collection module is added with weak periodical sinusoidal current
Hot thermal response temperature measuring unit 12；
Sub-step A3 adjusts the knob of adjustable resistance R1 manually, until the differential wave of lock-in amplifier 25 exists
0.0004mV or less is considered as stabilization, and the resistance value recorded at this time is 12 leveling resistance R of thermal response detector0；
Sub-step A4 increases signal generator output power, is recorded by lock-in amplifier 25 adaptive under predeterminated frequency
Fundamental voltage (V between two voltage lead part (1b, 1c) of thermal response detector1ω)y, third harmonic voltage (V3ω)y。
Step B, using (V achieved above1ω)y、(V3ω)yAnd the resistance that thermal response detector 12 has been demarcated before
The thermal conductivity k of temperature coefficient β, core strip length l, substrate 11s, the thermal conductivity of sample is calculated using formula (1).
So far, the accurate measurement energy-saving heat-insulating material thermal conductivity introduction in the present embodiment scene finishes.
Using the present embodiment method, the energy-saving heat-insulating tested as the self-adaptation type thermal response detector of substrate using BK7 glass
Material thermal conductivity range is in 0.2~4Wm-1·K-1Between, measurement error is estimated as 6% or less.Using PMMA acrylic boards as base
The energy-saving heat-insulating material thermal conductivity range of the self-adaptation type thermal response detector test at bottom is in 0.04Wm-1·K-1Under, it measures
Estimation error is 5% or less.Table 2 and table 3 show representative energy-saving heat-insulating testing of materials result.
The thermal conductivity measurement result of 2 adaptive thermal response detector (BK7 substrate of glass) of table
The thermal conductivity measurement result of 3 adaptive thermal response detector of table (PMMA acrylic boards substrate of glass)
It should be noted that the above-mentioned definition to each element is not limited in the various concrete structures mentioned in embodiment
Or shape, those skilled in the art can replace with simply being known to it.Although also, above-mentioned with energy-saving heat-insulating
Sample illustrates, but it will be apparent to those skilled in the art that it is equally applicable in the thermal characteristic measurement of other samples, this
Place is not described in detail.
The above is the preferred embodiment of the present invention, it is noted that for those skilled in the art
For, without departing from the principles of the present invention, several improvements and modifications can also be made, these improvements and modifications
It should be regarded as protection scope of the present invention.
Claims (5)
1. the device that a kind of energy-saving heat-insulating material thermal conductivity scene is accurately tested, it is characterised in that：Including self-adaptation type thermal response
Detector, electrical signal collection module and data processing module,
Wherein, self-adaptation type thermal response detector includes substrate (11), thermal response temperature measuring unit (12), abrasion-proof insulating protective film
(13), the first current feed part (1a), the second current feed part (1d), first voltage lead part (1b) and second voltage lead part
(1c), thermal response temperature measuring unit (12) are attached to substrate (11) by three kinds of Van der Waals force, diffusion attachment, mechanical snap effects
On top surface, the first current feed part (1a), the second current feed part (1d), first voltage lead part (1b) and second voltage lead
Part (1c) is welded on four pads of thermal response temperature measuring unit (12) end, and abrasion-proof insulating protective film (13) is covered in thermal response survey
The other side of warm unit (12)；
Electrical signal collection module includes signal generator (21), the first high-precision meter amplifier (22), the second high-precision meter
Amplifier (23), high precision DC power supply (24), lock-in amplifier (25), adjustable resistance (R1), the first current feed end (2a),
Second current feed end (2d), first voltage lead end (2b) and second voltage lead end (2c), the first current feed part (1a)
It is connect by the first current feed end (2a) with signal generator (21), the second current feed part (1d) is logical with adjustable resistance (R1)
The second current feed end (2d) to be crossed to be connected to the ground, first voltage lead part (1b) is electrically connected with first voltage lead end (2b), the
Two voltage lead parts (1c) are electrically connected with second voltage lead end (2c), and the first high-precision meter amplifier (22) is containing eight ends
Mouthful, wherein second port-IN and third port+IN are respectively connected to first voltage lead part (1b) and second voltage lead part
(1c), the 4th port-Vs, the 7th port+Vs, the 8th port REF are respectively connected to the negative pole end of high precision DC power supply (24)
Mouth, positive port and grounding ports；It is first poor to lock-in amplifier (25) that 6th port OUTPUT exports the first differential wave
Dynamic signal input part A；Second high-precision meter amplifier (23) contains eight ports, wherein second port-IN and third port+IN
The both ends of adjustable resistance (R1) are respectively connected to, the 4th port-Vs, the 7th port+Vs, the 8th port REF are separately connected supreme
The cathode port of precision DC power supply (24), positive port and grounding ports；6th port OUTPUT exports the second differential wave
To the second differential wave input terminal B of lock-in amplifier (25)；The third input terminal of lock-in amplifier (25) is connected to signal hair
First output end of raw device (21)；
The self-adaptation type thermal response detector is made by following methods：First, substrate (11) is placed in deionized water, through super
Sound wave cleans 15 minutes；Then, substrate (11) is placed on gluing machine and applies AZ6130 photoresists, 2000 turns of glue spreader rotating speed/
Minute, rubberization thickness is 2.4 μm, and type used is positive photoresist；It is dried 10 minutes under 95 DEG C of environment after substrate (11) gluing；It reapplies
Uv-exposure uses tetramethylammonium hydroxide after 15 seconds：Water=1:4 developing liquid developings show spill thermal response temperature measuring unit (12)
Four pad structure patterns；Wherein, it is 10 in vacuum degree if BK7 substrate of glass-7Torr, Ar flow are 8sccm, and pressure is
Priority magnetron sputtering 10nm chromium laminating layer and 200nm metal layers under the conditions of 2mTorr, if PMMA substrates, using chemical vapor deposition
Product 10nm chromium laminating layer and 200nm metal layers；In next step, it if BK7 substrate of glass, is removed photoresist stripping with acetone soak mode, warp
It crosses after being cleaned by ultrasonic, drying, it is high-visible that metal faciola side connects four bond pad shapes；If PMMA substrates, are gone using dilute alkaline soln
Glue；In next step, four pad positions of thermal response temperature measuring unit (12) are covered with high-temperature insulation adhesive tape, is formed sediment by chemical gaseous phase
Product method deposits Si3N4Protective layer, main technologic parameters：Environment temperature is 100 DEG C, pressure 900mT, SiH4With NH3Gas
Flow is respectively 300sccm and 200sccm, often plates 50nm and shuts down postcooling 5 minutes, recycled by 6 times, forms 300nm thickness
Si3N4Film；The substrate (11) that thermal response temperature measuring unit (12) and abrasion-proof insulating protective film (13) will be attached with is beaten by cutting
Mill, if BK7 substrates, then welds the first current feed part (1a), second on four pads of thermal response temperature measuring unit (12)
Current feed part (1d), first voltage lead part (1b) and second voltage lead part (1c), it is viscous using elargol if PMMA substrates
The mode connect connects the first current feed part (1a), the second current feed part (1d), first voltage lead part (1b) and the second electricity
Voltage lead wires part (1c)；
The first filter capacitor (C1), the second filter capacitor (C2), third is arranged in power output end in the electrical signal collection module
Filter capacitor (C3), the 4th filter capacitor (C4), the 5th filter capacitor (C5), the 6th filter capacitor (C6), the 7th filter capacitor
(C7), the 8th filter capacitor (C8), the 9th filter capacitor (C9), the tenth filter capacitor (C10), the 11st filter capacitor (C11)
With the 12nd filter capacitor (C12), wherein the first filter capacitor (C1), the second filter capacitor (C2), the 7th filter capacitor
(C7), the 8th filter capacitor (C8) is the filter capacitor of capacitance 10pF types, third filter capacitor (C3), the 4th filtered electrical
Appearance (C4), the 9th filter capacitor (C9), the tenth filter capacitor (C10) are the filter capacitor of 1 μ F types of capacitance, the 5th filtering
Capacitance (C5), the 6th filter capacitor (C6), the 11st filter capacitor (C11), the 12nd filter capacitor (C12) are capacitance
The filter capacitor of 100 μ F types.
2. the device that energy-saving heat-insulating material thermal conductivity according to claim 1 scene is accurately tested, it is characterised in that：It is described
Thermal response temperature measuring unit (12) be metal faciola side connect four bond pad shapes, wherein metal faciola length within the scope of 8~40mm,
For width in 8~100 μ ms, thermal response temperature measuring unit (12) is chromium/platinum, chrome gold or chromium/nickel clad, composite bed thickness
For 10nm/200nm.
3. the device that energy-saving heat-insulating material thermal conductivity according to claim 1 scene is accurately tested, it is characterised in that：It is described
Substrate (11) is BK7 optical glass or PMMA acrylic boards, and the polished processing of substrate (11) meets 10 angstroms of surface roughness, parallel
5 rads of degree, the thickness of matrix (11) is within the scope of 1~3mm.
4. the device that energy-saving heat-insulating material thermal conductivity according to claim 1 scene is accurately tested, it is characterised in that：It is described
First current feed part (1a), the second current feed part (1d), first voltage lead part (1b) and second voltage lead part (1c)
For enamel covered wire, abrasion-proof insulating protective film (13) is silicon nitride.
5. the device that energy-saving heat-insulating material thermal conductivity according to claim 1 scene is accurately tested carries out test heat-barrier material
The method of thermal conductivity, it is characterised in that：It is as follows：
Step A carries out in-site measurement to heat-barrier material to be measured using above-mentioned apparatus, obtains the fundamental voltage of heat-barrier material to be measured
(V1ω)yWith third harmonic voltage (V3ω)y；
Wherein, if detected materials are solid-state, abrasion-proof insulating protective film (13) side of self-adaptation type thermal response detector is directly pasted
In detected materials surface；If detected materials are liquid or powder, sample is directly dripped in abrasion-proof insulating protective film (13) with suction pipe
On, sample covers subject to full thermal response temperature measuring unit (12), starts next step；
By the first current feed part (1a) of adaptive thermal response detector, the second current feed part (1d) respectively with the first electric current
Lead end (2a), the electrical connection of the second current feed end (2d), first voltage lead part (1b), second voltage lead part (1c) and the
One voltage lead end (2b), second voltage lead end (2c) electrical connection；First current feed end (2a), the second current feed end
(2d) heats thermal response temperature measuring unit (12)；
Manually adjust adjustable resistance (R1) knob, until lock-in amplifier (25) differential wave in 0.0004mV hereinafter, note
The resistance value of record at this time is thermal response detector (12) leveling resistance R0；
Increase signal generator output power, adaptive thermal response detector under predeterminated frequency is recorded by lock-in amplifier (25)
First voltage lead part (1b) and second voltage lead part (1c) between fundamental voltage (V1ω)y, third harmonic voltage (V3ω)y；
Step B, using (V achieved above1ω)y、(V3ω)yAnd the resistance temperature that thermal response detector (12) has been demarcated before
The thermal conductivity k of degree factor beta, core strip length l, substrate (11)s, the thermal conductivity of sample is calculated using formula (1)；
In formula, kyThermal conductivity (the Wm of-heat-barrier material to be measured-1·K-1)；
ksThermal conductivity (the Wm of-substrate-1·K-1)；
Temperature-coefficient of electrical resistance (the K of β-thermal response detector-1)；
L-thermal response metal detector faciola length (m)；
V1ω- fundamental voltage (V)；
R0- thermal response detector leveling resistance (Ω)；
λ"—V3ωThe inverse of~ln ω slopes.
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| CN101266220A (en) * | 2007-03-14 | 2008-09-17 | 中国科学院工程热物理研究所 | Method and device for measuring liquid thermal conductivity factor and thermal diffusivity by harmonic detection technology |
| CN104034752A (en) * | 2014-06-16 | 2014-09-10 | 上海大学 | Device and method for measuring longitudinal thermal conductivity of film |
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| CN104034752A (en) * | 2014-06-16 | 2014-09-10 | 上海大学 | Device and method for measuring longitudinal thermal conductivity of film |
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