Summary of the invention
The present invention seeks to solve the existing 3 ω measuring techniques of surveying based on harmonic wave need repeat to prepare micro metal band and insulation difficulty etc. when testing technological deficiency, for this reason, the invention provides a kind of independent probe and can reuse, guarantee the insulation of metal tape and testing sample, can be used for harmonic wave method thermal physical property of solid material method of testing and device that independent probe was tested, had to a plurality of thermal physical property parameters such as the coefficient of heat conductivity of conduction such as metal, pottery and non-conductive solid and film and thermal diffusivity simultaneously.
For reaching described purpose, a first aspect of the present invention, a kind of harmonic wave method thermal physical property of solid material method of testing with independent probe is provided, utilizes the harmonic wave method thermal physical property of solid material proving installation with independent probe to realize this method, the technical scheme of this method is:
Step 1: independent probe is clipped between the identical standard sample of two known thermal physical property parameters and constitutes test structure, and be placed on sample fixed station base above, moving slider and screw rod, when the top of screw rod touches the end face of standard model, stop moving slider and in the side by the bolt slide block;
Step 2: screw rod reverses in portion with torque measurement, on a torsion point, suspend and write down the torque value of correspondence, begin to measure the fundamental voltage and the third harmonic voltage at the micro metal band two ends in the independent probe then, according to the thermal conductivity value of harmonic wave method test philosophy match standard model with the harmonic wave method;
Step 3: be rotated further torque measurement portion torque value is increased, repeating step 2 then, obtain the measured value of standard model coefficient of heat conductivity under a plurality of torque values;
Step 4: the measured value that utilizes a plurality of coefficient of heat conductivity of standard model that obtain, find out and the immediate measured value of the actual value of standard model coefficient of heat conductivity, if the torque value of this measured value correspondence is not influence true independent probe and the pairing torque value of measuring of the thermal contact resistance between standard model of coefficient of heat conductivity, this torque value is best torque value;
Step 5: take off test structure from boss, independent probe is clipped in the new test structure of formation between two identical testing samples, will it be placed on the boss, execution in step 1 fixes new test structure;
Step 6: screw rod reverses in portion with torque measurement, stops to reverse screw rod a plurality of under less than best torque value successively, record torque value and with the coefficient of heat conductivity and the thermal diffusivity value of harmonic wave method test testing sample;
Step 7: the torsional torque measurement section with the coefficient of heat conductivity and the thermal diffusivity of harmonic wave method test testing sample, is promptly finished the test to the testing sample thermal physical property parameter again until best torque value;
Step 8: write down a plurality of sizes less than thermal conductivity measurement value under the best torque value and the thermal conductivity measurement value under the best torque value, will be less than the difference of thermal conductivity measurement value under the best torque value and the thermal conductivity measurement value under the best torque value as having thermal contact resistance between testing sample and independent probe, the size of the thermal contact resistance between described testing sample and independent probe is by an empirical formula decision of the big or small experimental result match of torque value, and do not influence in the thermal contact resistance that exists between testing sample and independent probe under the best torque value that coefficient of heat conductivity is true to be measured and can be left in the basket, by calculating a plurality of differences less than thermal conductivity measurement value under thermal conductivity measurement value under the best torque value and the best torque value, use the relational expression of thermal contact resistance and thermal conductivity difference again, obtain the thermal contact resistance between testing sample and independent probe under a plurality of torque values.
For reaching described purpose, a second aspect of the present invention, a kind of harmonic wave method thermal physical property of solid material proving installation with independent probe is provided, the technical scheme of this device is: contain: independent probe, first testing sample, second testing sample, pressure adjustment part, sample fixed station, torque measurement portion, harmonic measurement unit, wherein: independent probe constitutes sandwiched type structure between two first identical testing samples, second testing sample, sandwiched type structure is positioned over the sample fixed station, and sandwiched type structure and the parallel placement of sample fixed station; The pressure adjustment part is positioned on the upper surface of first testing sample, and the pressure adjustment part compresses first testing sample, sandwiched type structure be positioned over the sample fixed station above; Torque measurement portion is socketed on an end of pressure adjustment part, and torque measurement portion regulates the displacement of pressure adjustment part, and torque measurement portion can show the torque value that acts on sandwiched type structure in real time in regulating pressure adjustment part process; Harmonic measurement unit is electrically connected with independent probe, measure the fundamental voltage and the third harmonic voltage at independent probe two ends under a plurality of torque values with the harmonic wave method, calculate the relation that contacts thermal resistance between match torque value and independent probe and first testing sample, second testing sample according to harmonic wave method measuring principle.
A third aspect of the present invention provides a kind of thermal physical property of solid material measurement mechanism, is used to measure the coefficient of heat conductivity and the thermal diffusivity parameter of conduction such as metal, pottery and non-conductive solid and film.
Beneficial effect of the present invention: the present invention can solve at present the 3 ω measuring techniques of surveying based on harmonic wave need repeat to prepare micro metal band and insulation difficulty on single sample when the specimen thermal physical property parameter problem to a great extent, can directly independent probe be clipped in two sample rooms tests, flexible substrate and flexible coverlay serve as insulation course simultaneously, guarantee the Non-Destructive Testing of non-conductive/conductive solid and film.
Based on the micro metal tape thickness of flexible substrate in 100~1000nm scope, width is in 100~500 mu m ranges, can consider the influence of metal film self thermal capacitance, the thickness of flexible substrate and flexible coverlay can guarantee the insulation between micro metal film and conducting sample and have certain mechanical strength to guarantee that probe is not fragile in use in 8~25 mu m ranges.
Flexible substrate and flexible coverlay have elasticity, can reduce the thermal contact resistance at interface greatly when clamping with sample.
In 2~20mm scope, can effectively eliminate the influence of micro metal strap end portion heat radiation based on two lead end 14b and 14c spacing in the middle of the micro metal band of flexible substrate.
Compare with the 3 ω measuring techniques based on the harmonic wave detection of preparation micro metal band on sample, the present invention no longer needs additionally preparing the micro metal band on the testing sample and the thick dielectric film of preparation hundred nano-scale on conducting sample; The Non-Destructive Testing of the non-conductive/conductive solid that utilizes this method to guarantee.Since between thermal contact resistance and independent probe and testing sample to compress degree relevant, and be scalable degree that compresses between the two and demonstration torque value in real time, so utilize this experimental system also can measure the relation of thermal contact resistance and pressure with a torque measurement portion.
Description of drawings
Fig. 1 is an independent probe synoptic diagram of the present invention;
Fig. 2 is an independent probe sectional view of the present invention;
Fig. 3 is the harmonic wave method thermal physical property of solid material proving installation sample fixed station synoptic diagram with independent probe of the present invention;
Fig. 3 a illustrates the partial enlarged drawing in the dotted line among Fig. 3;
Fig. 4 is the structural representation of harmonic measurement unit 7 of the present invention.
The main element explanation:
Independent probe 1 comprises:
Micro metal band 11, flexible coverlay 12, flexible substrate 13, four 141 to 144 and four lead end 14a to 14d of lead-in wire part;
First testing sample, 2, the second testing samples 3;
The pressure adjustment part comprises: a column 40, slide block 41 and screw rod 42;
The sample fixed station comprises: base 51, boss 52, deck 53 and deck lid 54;
Torque measurement portion 6;
Harmonic measurement unit 7 comprises: first operational amplifier 71, second operational amplifier 72, the 3rd operational amplifier 73, prime amplifier 74, signal generator 75, lock-in amplifier 76, system controlled by computer and data acquisition system (DAS) 77, first low temperature floats resistance R 1, second low temperature floats resistance R 2, the 3rd low temperature floats resistance R 3, the 4th low temperature floats resistance R 4, the 5th low temperature floats resistance R 5, the 6th low temperature floats resistance R 6, the 7th low temperature floats resistance R 7, the 8th low temperature floats resistance R 8, adjustable resistance R9, the first current feed end 7a, the second current feed end 7d, the first detecting voltage lead end 7b, the second detecting voltage lead end 7c.
Embodiment
Describe each related detailed problem in the technical solution of the present invention in detail below in conjunction with accompanying drawing.Be to be noted that described embodiment only is intended to be convenient to the understanding of the present invention, and it is not played any qualification effect.
A kind of harmonic wave method thermal physical property of solid material method of testing of the present invention with independent probe, relate to and be clipped in two structures between identical testing sample with a miniature independent probe and replace to pop one's head in and directly be deposited on technical scheme on the sample surfaces, realized non-destructive testing the testing sample thermal physical property parameter.To calibrate best torque value with standard red copper sample before the test.Utilization has the harmonic wave method thermal physical property of solid material proving installation of independent probe and realizes that the step of this method is as follows: 1. independent probe 1 is clipped between the identical standard sample of two known thermal physical property parameters and constitutes test structure, and be placed on the sample fixed station above, moving slider 41 and screw rod 42, when the top of screw rod 42 touches the end face of standard model, stop moving slider 41 and in the side by bolt slide block 41; 2. reverse screw rod 42 with torque measurement portion 6, on a torsion point, suspend and write down the torque value of correspondence, begin to measure the fundamental voltage and the third harmonic voltage at micro metal band 11 two ends in the independent probe 1 then, according to the thermal conductivity value of harmonic wave method test philosophy match standard model with the harmonic wave method; 3. be rotated further torque measurement portion 6 torque value is increased, 2. repeating step obtains the measured value of standard model coefficient of heat conductivity under a plurality of torque values then; 4. utilize the measured value of a plurality of coefficient of heat conductivity of standard model that obtain, find out and the immediate measured value of the actual value of standard model coefficient of heat conductivity, if the torque value of this measured value correspondence is not influence true independent probe and the pairing torque value of measuring of the thermal contact resistance between standard model of coefficient of heat conductivity, this torque value is best torque value; 5. take off test structure from boss 52, independent probe 1 is clipped in the new test structure of formation between two identical testing samples 2,3, will it be placed on the boss 52, execution in step 1 fixes new test structure; 6. reverse screw rod 42 with torque measurement portion 6, stop to reverse screw rod 42 a plurality of under less than best torque value successively, record torque value and with the coefficient of heat conductivity and the thermal diffusivity value of harmonic wave method test testing sample 2,3; 7. torsional torque measurement section 6 with the coefficient of heat conductivity and the thermal diffusivity of harmonic wave method test testing sample 2,3, is promptly finished the test to testing sample 2,3 thermal physical property parameters again until best torque value; 8. write down a plurality of sizes less than thermal conductivity measurement value under the best torque value and the thermal conductivity measurement value under the best torque value, will be less than the difference of thermal conductivity measurement value under the best torque value and the thermal conductivity measurement value under the best torque value as testing sample 2,3 and 1 of independent probe have thermal contact resistance, described testing sample 2,3 and the size of the thermal contact resistance of 1 of independent probe by an empirical formula decision of the big or small experimental result match of torque value, and testing sample 2 under best torque value, 3 and the thermal contact resistance of 1 existence of independent probe do not influence that coefficient of heat conductivity is true to be measured and can be left in the basket, by calculating a plurality of differences less than thermal conductivity measurement value under thermal conductivity measurement value under the best torque value and the best torque value, use the relational expression of thermal contact resistance and thermal conductivity difference again, obtain testing sample 2 under a plurality of torque values, 3 and the thermal contact resistance of 1 of independent probe.It is the cycle weak current heating of ω that micro metal band 11 in the described independent probe 1 adopts angular frequency.During test, adjust the fundamental voltage of described micro metal band 11, make third harmonic voltage between two lead end 14b, the 14c in the middle of the micro metal band near 1/500~1/1000 fundamental voltage.
Please refer to the thermal physical property of solid material proving installation shown in Fig. 1, Fig. 2, Fig. 3 and Fig. 4, Fig. 3 illustrates this device, contain: independent probe 1, first testing sample 2, second testing sample 3, pressure adjustment part, sample fixed station, torque measurement portion 6, harmonic measurement unit 7 (not making marks among pressure adjustment part, the sample fixed station figure), wherein:
Please refer to Fig. 3 a and independent probe 1 is shown constitutes sandwiched type structure between two first identical testing samples 2, second testing sample 3, sandwiched type structure is positioned over the sample fixed station, and sandwiched type structure and the parallel placement of sample fixed station; The pressure adjustment part is positioned on the upper surface of first testing sample 2, and the pressure adjustment part compresses first testing sample 2, and sandwiched type structure is positioned on the boss 52 of sample fixed station; Torque measurement portion 6 is socketed on an end of pressure adjustment part, and torque measurement portion 6 regulates the displacement of pressure adjustment part, and torque measurement portion 6 can show the torque value that acts on sandwiched type structure in real time in regulating pressure adjustment part process; Harmonic measurement unit 7 is electrically connected with independent probe 1, measure the fundamental voltage and the third harmonic voltage at independent probe 1 two ends under a plurality of torque values with the harmonic wave method, calculate match torque value and independent probe 1 and first testing sample 2,3 relations that contact thermal resistance of second testing sample according to harmonic wave method measuring principle.
Independent probe 1 shown in Fig. 1 and Fig. 2 comprises: micro metal band 11, flexible coverlay 12, flexible substrate 13 and four lead-in wire parts 141~144, micro metal band 11 is connected with an end of four lead-in wire parts 141~144 respectively, and the other end of four lead-in wire parts 141~144 has four lead end 14a~14d; Micro metal band 11 and four lead-in wire parts 141~144 are between flexible coverlay 12 and flexible substrate 13; Lead end 14b, 14c are connected by lead with harmonic wave detecting voltage lead end 7b, the 7c of harmonic measurement unit 7 respectively, and current feed end 7a, the 7d of harmonic measurement unit 7 inserts lead end 14a, 14d cycle to 11 electrical heating of micro metal band by lead.
Described micro metal band 11 and four lead-in wire parts 141~144 are attached to by photoetching or gas-phase deposition by conducting metal and form four thick bond pad shapes structures of hundred nano-scale on the flexible substrate 13; With flexible substrate 13 be same material band glue flexible cover film 12 by heat pressing process with form sandwiched type structures based on the micro metal band 3 of flexible substrate 13 and four lead-in wire parts 141~144, flexible substrate 13 and flexible coverlay 12 form micro metal band 11 with a mechanical strength and the insulating protective layer of four lead-in wire parts 141~144 at the bottom surface of micro metal band 11 and four lead-in wire parts 141~144 and end face.
Described conducting metal is paper tinsel or nickel; Described flexible substrate is polyimide or mica.
In 100~1000nm scope, width is in 100~500 mu m ranges based on micro metal band 11 thickness on the flexible substrate 13, and total length is in 10~50mm scope, and per two lead end spacings of four lead-in wire parts 141~144 are in 2~20mm scope; The thickness of flexible substrate 13 and flexible coverlay 12 is in 8~25 mu m ranges.
Described sample fixed station comprises: a base 51, a boss 52, a deck 53 and deck lid 54, wherein: base 51 is fixedlyed connected with boss 52 or base 51 is structure as a whole with boss 52.Be provided with two threaded holes in base 51 symmetria bilateralis, become 90 ° position to be provided with a square hole with two threaded holes on the base 51; Boss 52 is positioned at the center of base 51; Deck 53 is fixedlyed connected with base 51 by square hole; Deck covers 54 symmetria bilateralis and is provided with two threaded holes, fixedlys connected with deck 53 by two bolts; Four leads of drawing from lead member 141 to 144 lead end 14a to 14d pass the groove of deck 53 and fixing by deck lid 54; The lower surface of second testing sample contacts with boss 52.
Please refer to Fig. 3 a and illustrate, described pressure adjustment part comprises: a column 40, a slide block 41, a screw rod 42; Column 40 is fixedlyed connected with the threaded hole on the base 51; Be arranged with a slide block 41 on two columns 40, the central authorities of slide block 41 are threaded with screw rod 42, the pressure connection terminal crimping of the upper surface of first testing sample 2 and screw rod 42; Slide block 41 and screw rod 42 is the displacement of common decision screw rod 42 pressure connection terminals that are slidingly connected, and is used to realize compressing of 1 of two testing samples 2,3 and independent probe; Two testing samples 2,3 contact the size of thermal resistance and regulate by the degree that compresses that changes 2 of the screw rod 42 and first testing samples with 1 of independent probe; Screw rod 42 tops are that smooth hemisphere or ellipsoid structure are convenient to regulate testing sample 2,3 and independent probe 1 is stressed even.Described torque measurement portion 6 adopts digital display type dial torque wrench or digital torductors.
Described thermal physical property of solid material measurement mechanism is used to measure the coefficient of heat conductivity and the thermal diffusivity parameter of conduction such as metal, pottery and non-conductive solid and film.
Fig. 1, Fig. 2, Fig. 3 and Fig. 4 form the harmonic wave method thermal physical property of solid material proving installation with independent probe; Wherein the independent probe structure for amplifying among Fig. 3 and Fig. 4 is seen Fig. 1 and Fig. 2; The particular location of independent probe 1 is seen Fig. 3 during test; Four lead end 14b, 14c of the independent probe 1 among Fig. 3 and 14a, 14d be harmonic wave detecting voltage lead end 7b, 7c and current feed end 7a, the 7d of the harmonic measurement unit 7 by lead map interlinking 4 respectively.
Independent probe 1 is clipped between two identical first testing samples 2 and second testing sample 3, and to feed angular frequencies to micro metal band 11 be the cycle weak current of ω, the heat that produces because of Joule effect will be with the frequency of 2 ω to micro metal band 11, metal tape outside flexible substrate 13, the flexible coverlay 12 and first testing sample 2 and 3 heating of second testing sample, produce the different temperature wave of frequency, the resistance that causes micro metal band 11 increases, and the resistance that micro metal band 11 increases is the different voltage harmonic of periodic current acting in conjunction generation frequency of ω with angular frequency.Can determine a plurality of thermal parameters such as the coefficient of heat conductivity of solid material and thermal diffusivity according to the relation of voltage harmonic and vibration frequency.Utilize theoretical model that the present invention proposes and data processing method a plurality of thermal physical property parameters such as conduction such as nondestructive measurement metal, pottery and non-conductive solid and film coefficient of heat transfer, thermal diffusivity simultaneously.
It is the micro metal band 11 of the cycle weak current heating of ω based on flexible substrate that the present invention adopts angular frequency, because of the effective value of micro metal band 11 internal currents very little, the heating power that produces has only several milliwatts, adding thermal flexibility coverlay 12, flexible substrate 13, in the process of first testing sample 2 and second testing sample 3, the temperature rise of micro metal band 11 must be less than 1~2K, the frequency range of the periodic current of Cai Yonging is bigger simultaneously, change to several KHz from several Hz, the temperature rise of solid and the heat effect degree of depth are very little under these conditions, lock-in amplifier adopts smaller time constant simultaneously, can so that solid sample than the assumed condition that is easier to satisfy the big border of semiinfinite, and then can be very little so that measure required sample volume.Because the flexible coverlay 12 and the flexible substrate 13 on micro metal band 11 surfaces have certain thickness, and not little (the about 0.8Wm of coefficient of heat conductivity
-1K
-1), so the influence of the temperature change of insulation course can not ignore, but can from experimental data, deduct the influence of insulation course.As long as guarantee that heat wave has penetrated flexible coverlay 12 and flexible substrate 13 in measured frequency range, just can obtain the thermal physical property parameter information of solid sample.The coefficient of heat conductivity scope of the solid of the present invention's test is than broad, and the solid conductive heat coefficient is at 0.1~50Wm
-1K
-1Between, the uncertainty of measurement of coefficient of heat conductivity is less than ± 3.5%, and the solid conductive heat coefficient is at 50~500Wm
-1K
-1Between, the uncertainty of measurement of coefficient of heat conductivity is less than ± 2%, and the uncertainty of measurement of thermal diffusion coefficient is less than ± 6%.
Before the test beginning, to calibrate best torque value, concrete steps are as follows: independent probe 1 is clipped between two standard models the structure that constitutes similar sandwich and places it on the boss 52 of sample fixed station, moving slider 41 and screw rod 42, when the top of screw rod 42 touches the end face of standard model, stop moving slider 41 and in the side by bolt slide block 41; Reverse screw rod 42 with the digital display type dial torque wrench, on a torsion point, suspend and write down the torque value of correspondence, begin to measure the fundamental voltage and the third harmonic voltage at the micro metal band two ends in the independent probe then, according to the thermal conductivity value of harmonic wave method test philosophy match standard model with the harmonic wave method; Be rotated further torque measurement portion torque value is increased, repeat top step then, obtain the measured value of standard model coefficient of heat conductivity under a plurality of torque values; The measured value of a plurality of coefficient of heat conductivity of standard model that utilization obtains, find out and the immediate measured value of the actual value of standard model coefficient of heat conductivity, if the torque value of this measured value correspondence is not influence true independent probe and the pairing torque value of measuring of the thermal contact resistance between standard model of coefficient of heat conductivity, this torque value is best torque value; Promptly finish calibration operation.During official testing, the similar sandwich structure that independent probe 1 and first testing sample 2 and second testing sample 3 is constituted with same method is pressed on the boss 52 by the top of screw rod 42, directly reverse screw rod 42 to best torque value with the digital display type dial torque wrench again, think that first testing sample 2 this moment, second testing sample 3 fully contact with independent probe 1.Regulate the maximum resistance that the adjustable resistance R9 that connects is approaching or may reach greater than micro metal band 11 in the measuring process slightly.In order to prevent that micro metal band 11 from having apparent in view temperature rise, the output voltage of conditioning signal generator, make the voltage at adjustable resistance R9 two ends near 10mV, the fine setting adjustable resistance, differential Input Monitor Connector by lock-in amplifier, make bridge balance, the resistance of adjustable resistance just equals the cold-state resistance of micro metal band.Begin test then, select a series of frequency values, measure the fundamental voltage and the third harmonic voltage at micro metal band 11 two ends under the respective frequencies value.During the third harmonic at measurement micro metal band 11 two ends under a certain frequency, should select rational fundamental voltage, make the third harmonic at micro metal band 11 two ends near 1/500~1/1000 of first-harmonic.In addition, reach in the process of best torque value also and can a plurality ofly stop (mean this moment that independent probe and sample room thermal contact resistance can not ignore) on less than best torque value at digital display type torsional torque spanner, measure the fundamental voltage and the third harmonic voltage at micro metal band 11 two ends then with said method, again according to the thermal conductivity value of harmonic wave method test philosophy match testing sample; By calculating a plurality of differences less than thermal conductivity measurement value under thermal conductivity measurement value under the best torque value and the best torque value, use the relational expression of thermal contact resistance and thermal conductivity difference again, obtain the thermal contact resistance between the testing sample and independent probe under a plurality of torque values.
See also the structure that Fig. 4 illustrates harmonic measurement unit 7 of the present invention, harmonic measurement unit 7 comprises: first operational amplifier 71, second operational amplifier 72, the 3rd operational amplifier 73, prime amplifier 74, signal generator 75, lock-in amplifier 76, system controlled by computer and data acquisition system (DAS) 77, first low temperature floats resistance R 1, second low temperature floats resistance R 2, the 3rd low temperature floats resistance R 3, the 4th low temperature floats resistance R 4, the 5th low temperature floats resistance R 5, the 6th low temperature floats resistance R 6, the 7th low temperature floats resistance R 7, the 8th low temperature floats resistance R 8, adjustable resistance R9, the first current feed end 7a, the second current feed end 7d, the first detecting voltage lead end 7b, the second detecting voltage lead end 7c.
Signal generator 75 output angle frequencies are that the ac voltage signal of ω is converted to current signal through first operational amplifier 71, this current signal is used for driving simultaneously the micro metal band 11 of adjustable resistance R9 and independent probe 1, and the voltage signal of adjustable resistance R9 and independent probe 1 becomes differential wave input lock-in amplifier 76 after prime amplifier 74 amplifies again through second operational amplifier 72 and the 3rd operational amplifier 73 respectively.System controlled by computer and data acquisition system (DAS) 77 control-signals generator 75 lock-in amplifier 76 and adjustable resistances.The first current feed end 7a and the second current feed end 7d are electrically connected with the lead end 14a and the 14d of independent probe 1 respectively, and the first detecting voltage lead end 7b and the second detecting voltage lead end 7c are electrically connected with the lead end 14b and the 14c of independent probe 1 respectively.
The above; only be the embodiment among the present invention; but protection scope of the present invention is not limited thereto; anyly be familiar with the people of this technology in the disclosed technical scope of the present invention; can understand conversion or the replacement expected; all should be encompassed in of the present invention comprising within the scope, therefore, protection scope of the present invention should be as the criterion with the protection domain of claims.