CN101825592A - Method and device for testing thermal physical property of single conductive filamentary material by using harmonic method - Google Patents
Method and device for testing thermal physical property of single conductive filamentary material by using harmonic method Download PDFInfo
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- CN101825592A CN101825592A CN201010141035A CN201010141035A CN101825592A CN 101825592 A CN101825592 A CN 101825592A CN 201010141035 A CN201010141035 A CN 201010141035A CN 201010141035 A CN201010141035 A CN 201010141035A CN 101825592 A CN101825592 A CN 101825592A
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Abstract
The invention discloses a method and a device for testing thermal physical property of a single conductive filamentary material by using a harmonic method. The device comprises that: a single filamentary sample is fixed on a filamentary sample fixer, and the filamentary sample fixer is placed in parallel at the cavity bottom of a thermostatic vacuum cavity; one end of a thermocouple of a temperature adjusting system is inserted in the cavity, the other end of the thermocouple of the temperature adjusting system is electrically connected with a temperature controller, a TEC heater/cooler is arranged in an insulating layer in a mode of jointing the cavity, and the start and shutdown of the TEC heater/cooler is controlled by the temperature controller; a vacuum pumping system is externally connected with the cavity; and a harmonic measurement unit is electrically connected with the single filamentary sample, fundamental voltages, third harmonic voltages and phase angles at two ends of the single filamentary sample under multiple frequencies are measured by using the harmonic method, and heat conduction coefficient, heat capacity and thermal diffusivity parameters of the single filamentary sample are fitted according to the harmonic test principle.
Description
Technical field
The invention relates to method and device that a kind of utilization exchanges heating and harmonic wave method measurement filamentary material thermal physical property parameter (as coefficient of heat conductivity, thermal diffusivity and thermal capacitance etc.), particularly be applied to the method and the device of conduction filamentary material thermal physical property parameters tests such as single piece of metal filament, carbon fiber, carbon nano-tube.
Background technology
Carbon fiber and carbon nano-tube are obtaining using widely aspect the thermal behavior that improves dual-use new materials such as solid propellant rocket nozzle thermofin, aircraft construction material as the enhancing base of multiple compound substance, therefore, the accurate measurement of the thermal parameter of this class filamentary material of carbon fiber and carbon nano-tube self has important effect for the thermal design and the heat control of above-mentioned compound substance.But the diameter of carbon fiber is generally less than 10 μ m, and the diameter of carbon nano-tube is littler, generally is in the magnitude of nm, measure its thermal physical property parameter exactly and become very difficult.Feasible measuring method mainly contains two classes at present: a class is based on the measuring method of body material, concrete useful flicker method is measured the thermal diffusivity of unidirectional and two-way C/C compound substance or is measured the coefficient of heat conductivity of carbon fiber bundle with the Angstrom method, analyzing the characteristics of this class measuring method is not difficult to find, because the influence of factors such as the thermal contact resistance that exists between the fiber, fiber orientation and fiber filled coefficient, these class methods are difficult to characterize exactly the thermal physical property parameter of single filamentary material; Another kind of method is the T type method at single filamentary material that just occurs in recent years, this method of alternating current heating of utilizing has insensitive characteristics to the radiation heat loss, therefore measure aspect the filamentary material very valuable, but do not have other method to contrast the test result of T type method.At above-mentioned these problems, we have invented another kind and have heated based on alternating current, simultaneously, can measure coefficient of heat conductivity, thermal capacitance and the thermal diffusivity parameter of microscales conduction filamentary materials such as single piece of metal filament, carbon fiber and carbon nano-tube simultaneously in conjunction with the apparatus and method of the hot rerum natura of conduction filamentary material that are suitable for measuring little, nano-scale of harmonic wave Detection Techniques.
Summary of the invention
The present invention seeks to solve to have now and can't accurately measure the technological deficiency of single microscale filamentary material thermal physical property parameter, and be independent of the T type method that can be used for the hot physical property measurement of single filamentary material based on body material thermophysical property measurement method.For this reason, the invention provides a kind of thermal physical property of single conductive filamentary material by using harmonic method method of testing and device, this device, has the thread sample fixture that is exclusively used in the filamentary material test, thread sample is detector, and a plurality of thermal physical property parameters such as coefficient of heat conductivity, thermal capacitance and thermal diffusivity that can be used for microscale conduction filamentary materials such as single piece of metal filament, carbon fiber and carbon nano-tube are tested simultaneously.
For reaching described purpose, technical solution of the present invention is:
A kind of thermal physical property of single conductive filamentary material by using harmonic method method of testing, it comprises that step is as follows:
Step 1: single thread sample is separately fixed on four parallel lead wire spares of thread sample fixture, utilizes the lead-in wire part to have certain thickness and make thread sample keep unsettled;
Step 2: thread sample fixture is positioned in the constant temperature vacuum chamber, and the start-up temperature regulating system makes in the constant temperature vacuum chamber and meets the requirements of temperature;
Step 3: open pumped vacuum systems, treat to close pumped vacuum systems after the interior vacuum tightness of constant temperature vacuum chamber reaches requirement;
Step 4: four lead ends on the thread sample fixture are connected harmonic measurement unit, the simple sinusoidal alternating current of feeding a series of amplitudes for thread sample, measure under the same frequency in the middle of the fundamental voltage amplitude and the third harmonic voltage amplitude of thread sample between two point of fixity;
Step 5: the logarithmic relationship curve of record and analysis third harmonic voltage amplitude and fundamental voltage amplitude, if slope, illustrates that the test structure of existing thread sample and four lead-in wire parts compositions is qualified near 3, execution in step 6, otherwise should make test structure again, get back to step 1 and restart;
Step 6: four lead ends on the thread sample fixture are connected harmonic measurement unit, the electric current of feeding certain amplitude size for thread sample, fundamental voltage amplitude, third harmonic voltage amplitude and the phasing degree of the thread sample between down middle two point of fixity of test different frequency;
Step 7: the start-up temperature regulating system makes and arrives another temperature in the constant temperature vacuum chamber, write down under this temperature on the thread sample fixture in the middle of the resistance value of thread sample between two point of fixity;
Step 8: repeating step 7 reaches at least ten groups until resistance value of noting and corresponding temperature value, calculates the temperature-coefficient of electrical resistance of thread sample;
Step 9: according to coefficient of heat conductivity, thermal capacitance and the thermal diffusivity parameter of the single thread sample of harmonic wave method test philosophy match.
Described thermal physical property of single conductive filamentary material by using harmonic method method of testing, in its described step 4, single thread sample adopts faint cycle sinusoidal current heating, during test, adjust the fundamental voltage of described thread sample, the third harmonic voltage in the middle of making between two of two point of fixity lead-in wire part end points is near tens to hundreds of μ V; The frequency values of same frequency is very low, is 4Hz.
Described thermal physical property of single conductive filamentary material by using harmonic method method of testing, its described faint cycle sinusoidal current, its amplitude size is that the filament of micron dimension is tens milliamperes for measuring diameter, for measuring diameter is that the carbon fiber of micron dimension is the hundreds of microampere, is that the carbon nano-tube of nanometer scale is several microamperes for measuring diameter.
Described thermal physical property of single conductive filamentary material by using harmonic method method of testing, its described humidity control system comprises: a thermopair, a TEC heating/cooling device and a temperature controller; Thermoelectricity is on a rare occasion held and is inserted in the inner chamber, and the other end is electrically connected temperature controller; The TEC heating/cooling device is close to inner chamber and is placed heat-insulation layer, and is controlled start and stop by temperature controller; The reading of thermopair is delivered to temperature controller by set algorithm decision hot/cold amount, thereby realizes temperature automatically controlled to inner chamber by the action of the output order control TEC heating/cooling device of temperature controller again.
Described thermal physical property of single conductive filamentary material by using harmonic method method of testing, it is used to measure coefficient of heat conductivity, thermal capacitance and the thermal diffusivity parameter of microscale conduction filamentary materials such as single piece of metal filament, carbon fiber or carbon nano-tube.
The thermal physical property of single conductive filamentary material by using harmonic method proving installation that a kind of described method is used comprises: constant temperature vacuum chamber, humidity control system, pumped vacuum systems, harmonic measurement unit; It also comprises: thread sample fixture; Thread sample fixture is placed horizontally at the bottom of the constant temperature vacuum chamber inner chamber, is electrically connected with harmonic measurement unit; The thermoelectricity of humidity control system is on a rare occasion held and is inserted in the inner chamber, and the other end is electrically connected temperature controller; The TEC heating/cooling device is close to internal chamber wall, places heat-insulation layer; Constant temperature vacuum chamber inner chamber and pumped vacuum systems interlink;
Thread sample fixture comprises base, a plurality of lead-in wire spare; Base upper surface is covered with insulation course, even parallel four the lead-in wire parts that set firmly of insulation course upper surface, and strip lead-in wire part horizontally set, the one end is a lead end; Insulation course is silicon dioxide or silicon nitride layer, and the lead-in wire part is that copper product is made;
During test, single thread sample is fixed on four parallel lead wire spares, and the axially length direction with four lead-in wire parts of thread sample is vertical, utilizes the thickness of lead-in wire part to make thread sample keep unsettled, and harmonic measurement unit is electrically connected with single thread sample through lead end.
Described thermal physical property of single conductive filamentary material by using harmonic method proving installation, its described harmonic measurement unit is electrically connected with single thread sample through lead end, two lead ends are connected by lead with the harmonic wave detecting voltage lead end of harmonic wave probe unit respectively in the middle of being, the current feed end of harmonic measurement unit inserts two lead end cycles of both sides to single thread sample electrical heating by lead.
Described thermal physical property of single conductive filamentary material by using harmonic method proving installation, even parallel four the lead-in wire parts that set firmly of its described base upper surface, the one, when measuring carbon fiber that diameter is a micron dimension or filament, the lead-in wire part by conducting metal by electroplate and etch process attached to forming four thick bond pad shapes structures of tens micron dimensions on the printed wiring board base, diameter be micron dimension thread sample by gold wire bonder pressure welding or the bonding technology of elargol be separately fixed at four the lead-in wire parts an end, form four point of fixity;
The 2nd, when the measurement diameter is the carbon nano-tube of nanometer scale, at thickness the thick insulation course of deposition tens nanometer scale on the silicon chip base of hundreds of micron earlier by high-temperature oxidation, prepare single-root carbon nano-tube then, adopt the nickel coated carbon nanotube of focusing of ion beam process deposits one layer thickness 2～3nm again, be several millimeters carbon nano-tube pipe range direction then along length, with several microns is the spacing about 1 μ m of deposition width thereon, the about 200nm of thickness, length is about four gold solder dishes of 1mm as the lead-in wire part, and the space of elimination pad and carbon nano-tube contact position, reduce thermal contact resistance.
Described thermal physical property of single conductive filamentary material by using harmonic method proving installation, its described preparation single-root carbon nano-tube is the technology preparation that proposes by Yu C.
Described thermal physical property of single conductive filamentary material by using harmonic method proving installation, the thickness of the base of its described thread sample fixture are 0.5～2mm, and width or length are 0.2～20mm; Thickness of insulating layer is 20～200nm; Lead-in wire part width is 1～1000 μ m, and length is 1～10mm, and thickness is 200～25000nm; Adjacent two single thread sample point of fixity spacings are between 0.5～500 μ m.
Beneficial effect of the present invention: the present invention can solve the problem that present body material thermophysical property measurement method can't accurately characterize the thermal physical property parameter of individual carbon fibers and carbon nano-tube to a great extent, can directly the thread sample of conduction little, nano-scale be used as the harmonic wave law detector, measure coefficient of heat conductivity, thermal capacitance and the thermal diffusivity of the thread sample of single conduction simultaneously.
The thickness of thread sample fixture base is in 0.5～2mm scope, and width and length are in 0.2～20mm scope; Thickness of insulating layer is at 20～200nm; Four lead-in wire part width are in 1～1000 mu m range, and length is in 1～10mm scope, and thickness can guarantee that thread sample keeps unsettled in 200～25000nm scope.
Two point of fixity 14b and 14c spacing can effectively be eliminated the influence of micro metal strap end portion heat radiation in the middle of the thread sample in 0.5～1000 mu m range, owing to adopt the mode of connection of four-wire system, the influence of contact resistance and thermal contact resistance can be ignored during measurement simultaneously.
With compare based on the measuring method of body material, the present invention directly with the thread sample of conduction little, nano-scale as the harmonic wave law detector, do not need additionally to introduce miniature harmonic wave law detector; Utilize this method can obtain coefficient of heat conductivity, thermal capacitance and the thermal diffusivity of the thread sample of single conduction simultaneously.Because the spacing of the lead-in wire spare on the thread sample fixture can adjust when design, makes effective measurement length of filamentary material to adjust, and is applicable to the conduction filamentary material of measuring different-diameter and different resistivity.
Description of drawings
Fig. 1 is a thread sample fixture synoptic diagram of the present invention;
Fig. 2 is a thread sample fixture sectional view of the present invention;
Fig. 3 is thread sample fixture of the present invention, constant temperature vacuum chamber, humidity control system and pumped vacuum systems connection diagram;
Fig. 4 is the structural representation of harmonic measurement unit of the present invention.
The main element explanation:
Thread sample fixture 1 comprises:
Constant temperature vacuum chamber 3 comprises: metal shell 31, heat-insulation layer 32 and inner chamber 33;
Humidity control system 4 comprises: thermopair 41, TEC heating/cooling device 42 and temperature controller 43;
Pumped vacuum systems 5;
Harmonic measurement unit 6 comprises: first operational amplifier 61, second operational amplifier 62, the 3rd operational amplifier 63, prime amplifier 64, signal generator 65, lock-in amplifier 66, system controlled by computer and data acquisition system (DAS) 67, 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 6a, the second current feed end 6d, the first detecting voltage lead end 6b, the second detecting voltage lead end 6c.
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 the present invention is not played any qualification effect.
A kind of thermal physical property of single conductive filamentary material by using harmonic method method of testing of the present invention, relate to alternating current and heat the technical scheme of single thread sample, measure when realizing coefficient of heat conductivity, thermal capacitance to microscales such as single piece of metal filament, carbon fiber and carbon nano-tube conduction filamentary material and thermal diffusivity parameter in conjunction with the harmonic wave Detection Techniques.Want the calibration testing structure whether qualified before the test.Utilize the thermal physical property of single conductive filamentary material by using harmonic method proving installation to realize that the step of this method is as follows: 1. single thread sample 2 to be separately fixed at by gold wire bonder pressure welding or the bonding technology of elargol on four parallel lead wire spares 131 to 134 of thread sample fixture 1, to utilize lead-in wire part 131～134 to have certain thickness and make thread sample 2 keep unsettled; 2. thread sample fixture 1 is positioned in the constant temperature vacuum chamber 3, start-up temperature regulating system 4 makes in the constant temperature vacuum chamber 3 and meets the requirements of temperature; 3. open pumped vacuum systems 5, treat to close pumped vacuum systems 5 after constant temperature vacuum chamber 3 interior vacuum tightnesss reach requirement; 4. four lead ends on the thread sample fixture 1 131 to 134 are connected harmonic measurement unit 6, feed the simple sinusoidal alternating current of a series of amplitudes for thread sample 2, measure the fundamental voltage amplitude and the third harmonic voltage amplitude of the thread sample between two point of fixity 14b and 14c in the middle of (generally selecting a very low frequency values) under the same frequency as 4Hz; 5. write down and analyze the logarithmic relationship curve of third harmonic voltage amplitude and fundamental voltage amplitude, if slope, illustrates that the test structure of existing thread sample 2 and four lead-in wire parts, 131～134 compositions is qualified near 3, but execution in step 6, otherwise should make test structure again, get back to step 1 and restart; 6. four lead ends on the thread sample fixture 1 131 to 134 are connected harmonic measurement unit 6, feed the electric current of certain amplitude size for thread sample 2, fundamental voltage amplitude, third harmonic voltage amplitude and the phasing degree of the thread sample between down middle two point of fixity 14b of test different frequency and 14c; 7. start-up temperature regulating system 4 makes constant temperature vacuum chamber 3 arrive another temperature, write down under this temperature on the thread sample fixture 1 in the middle of the resistance value of the thread sample of 14b and 14c between two point of fixity; 8. repeating step 7 until resistance value of noting and corresponding temperature value reach ten groups or more than, calculate the temperature-coefficient of electrical resistance of thread sample 2; 9. according to coefficient of heat conductivity, thermal capacitance and the thermal diffusivity parameter of the single thread sample 2 of harmonic wave method test philosophy match.It is the cycle weak current heating of ω that described single thread sample 2 adopts angular frequency, its amplitude size is that the filament of micron dimension is tens milliamperes for measuring diameter, for measuring diameter is that the carbon fiber of micron dimension is the hundreds of microampere, is that the carbon nano-tube of nanometer scale is several microamperes for measuring diameter.During test, adjust the fundamental voltage of the single thread sample between described centre two point of fixity 14b and 14c, make the third harmonic voltage of the single thread sample between two point of fixity 14b and 14c under low frequency (as 3Hz), be in the scope of 10～150 μ V; Third harmonic voltage can not be too big or too little under the low frequency, third harmonic voltage means that too greatly input current is bigger, radiation loss is also bigger, the too little then extraneous as easy as rolling off a log stability that influences measuring-signal of noise of third harmonic voltage, the reliability of the data that the both collects influence.
Please refer to the thermal physical property of single conductive filamentary material by using harmonic method proving installation shown in Fig. 1, Fig. 2, Fig. 3 and Fig. 4, Fig. 3 illustrates this device, contain: thread sample fixture 1, single thread sample 2, constant temperature vacuum chamber 3, humidity control system 4, pumped vacuum systems 5, harmonic measurement unit 6 (not making marks among the harmonic measurement unit figure), wherein:
Please refer to Fig. 3 the end that single thread sample 2 is fixed in four parallel lead wire spares 131 to 134 of thread sample fixture 1 is shown, utilize lead-in wire part 131～134 to have certain thickness and make thread sample 2 keep unsettled, and the axially length direction with lead-in wire part 131 to 134 of thread sample 2 is vertical; Thread sample fixture 1 is placed in parallel in 33 ends of constant temperature vacuum chamber 3 inner chambers; Thermopair 41 1 ends of humidity control system 4 insert in the inner chamber 33, and the other end is electrically connected temperature controller 43, and TEC heating/cooling device 42 is close to inner chamber 33 and is placed heat-insulation layer 32; The external inner chamber 33 of pumped vacuum systems; Harmonic measurement unit 6 is electrically connected with single thread sample 2, measure fundamental voltage and the third harmonic voltage and the phasing degree at individual thread shape sample 2 two ends under a plurality of frequencies with the harmonic wave method, according to coefficient of heat conductivity, thermal capacitance and the thermal diffusivity parameter of the single thread sample 2 of harmonic wave method test philosophy match.
Thread sample fixture 1 shown in Fig. 1 and Fig. 2 comprises: base 11, insulation course 12, four lead-in wire parts 131～134, four lead end 13a～13d and four point of fixity 14a to 14d, the thread sample 2 of single conduction respectively with four the lead-in wire parts 131～134 an end be connected to form four point of fixity 14a to 14d, four the lead-in wire parts 131～134 the other end four lead end 13a～13d are arranged; Four lead-in wire parts 131～134 are positioned on the insulation course 12 and are parallel to insulation course 12; Insulation course 12 is positioned on the base 11 and is parallel to base 11; Lead end 13b, 13c are connected by lead with harmonic wave detecting voltage lead end 6b, the 6c of harmonic wave probe unit 6 respectively, and current feed end 6a, the 6d of harmonic measurement unit 6 inserts lead end 13a, 13d cycle to thread sample 2 electrical heating by lead.
When measuring diameter and be the carbon fiber of micron dimension or filament, described four lead-in wire parts 131～134 by conducting metal (being generally copper) by electroplate and etch process attached to forming four thick bond pad shapes structures of tens micron dimensions on the printed wiring board base 11, the thread sample of micron dimension by gold wire bonder pressure welding or the bonding technology of elargol be separately fixed at four the lead-in wire parts 131～134 an end, form four point of fixity 14a～14d; When the measurement diameter is the carbon nano-tube of nanometer scale, at thickness the thick insulation course (being generally silicon dioxide or silicon nitride) 12 of deposition tens nanometer scale on the silicon chip base 11 of hundreds of micron earlier by high-temperature oxidation, technology by propositions such as Yu C prepares single-root carbon nano-tube then, may in 3 ω harmonic signals, introduce spurious signal because the thermal contact resistance at electrode place is excessive or contact condition is bad, therefore adopt the nickel coated carbon nanotube of focusing of ion beam process deposits one layer thickness 2～3nm again, be several millimeters carbon nano-tube pipe range direction then along length, with several microns is the spacing about 1 μ m of deposition width thereon, the about 200nm of thickness, length is about four lead-in wire parts 131～134 of 1mm, to eliminate the space of lead-in wire part and carbon nano-tube contact position as far as possible, reduce thermal contact resistance.
The thickness of the base 11 of thread sample fixture 1 is in 0.5～2mm scope, and width and length are in 0.2～20mm scope; Insulation course 12 thickness are at 20～200nm; Four lead-in wire part 131～134 width are in 1～1000 mu m range, and length is in 1～10mm scope, and thickness is in 200～25000nm scope; Adjacent two point of fixity (14a and 14b, 14b and 14c, 14c and 14b) spacing is in 0.5～500 mu m range.
Please refer to Fig. 3 illustrates, described constant temperature vacuum chamber comprises: a metal shell 31, a heat-insulation layer 32 and an inner chamber 33, wherein: the outside of heat-insulation layer 32 is close in the inboard of metal shell 31, and the inboard of heat-insulation layer 32 surrounds the outside of inner chamber 33, the approximate formation of three concentric cylinder body structure; Thread sample fixture 1 parallel being placed at 33 ends of inner chamber; The side perforate of inner chamber 33 is connected with pumped vacuum systems 5.
Described humidity control system comprises: a thermopair 41, a TEC heating/cooling device 42 and a temperature controller 43; Thermopair 41 1 ends insert in the inner chamber 33, and the other end is electrically connected temperature controller 43; TEC heating/cooling device 42 is close to inner chamber 33 and is placed heat-insulation layer 32, and is controlled start and stop by temperature controller 43.The reading of thermopair 41 is delivered to temperature controller 43 by set algorithm decision hot/cold amount, thereby realizes temperature automatically controlled to inner chamber 33 by the action of the output order control TEC heating/cooling device 42 of temperature controller 43 again.
Described thermal physical property of single conductive filamentary material by using harmonic method proving installation is used to measure coefficient of heat conductivity, thermal capacitance and the thermal diffusivity parameter of microscales conduction filamentary materials such as single piece of metal filament, carbon fiber and carbon nano-tube.
Fig. 1, Fig. 2, Fig. 3 and Fig. 4 form the thermal physical property of single conductive filamentary material by using harmonic method proving installation; Wherein the thread sample fixture structure for amplifying among Fig. 3 and Fig. 4 is seen Fig. 1 and Fig. 2; The particular location of thread sample fixture 1 is seen Fig. 3 during test; Four lead end 13b, 13c of the thread sample fixture 1 among Fig. 3 and 13a, 13d be harmonic wave detecting voltage lead end 6b, 6c and current feed end 6a, the 6d of the harmonic measurement unit 6 by lead map interlinking 4 respectively.
It is that the cycle weak current of ω heats single thread sample 2 that the present invention adopts angular frequency, and because of the effective value of internal current is very little, heating power is very little, and in heating process, the harmonic signal that thread sample 2 is caused by temperature rise has only the magnitude of μ V.In order to reduce the influence of issuable stray inductance of test macro and sample structure itself and electric capacity as far as possible, be necessary to adopt alap test frequency simultaneously, also the assumed condition of satisfied temperature fluctuation progression model.During the low frequency test, lock-in amplifier adopts bigger time constant, guarantees that the harmonic value that shows is stable.The coefficient of heat conductivity scope of the single thread sample of the present invention's test is than broad, and single thread sample coefficient of heat conductivity is at 50～5000Wm
-1K
-1Between, the uncertainty of measurement of coefficient of heat conductivity is less than ± 2.5%, and the uncertainty of measurement of thermal diffusion coefficient is less than ± 8%, and the uncertainty of measurement of thermal capacitance is less than ± 6%.
Before the test beginning, to verify experimental system, concrete steps are as follows: single platinum filament sample (purity is 99.99%, and diameter is 16.8 μ m) is separately fixed at by gold wire bonder pressure welding or the bonding technology of elargol on four parallel lead wire spares 131～134 of thread sample fixture 1; Thread sample fixture 1 is positioned in the constant temperature vacuum chamber 3, and start-up temperature regulating system 4 makes in the constant temperature vacuum chamber 3 and meets the requirements of temperature; Open pumped vacuum systems 5, treat to close pumped vacuum systems 5 after constant temperature vacuum chamber 3 interior vacuum tightnesss reach requirement; Feeding angular frequency for the platinum filament sample is the sinusoidal period weak current of ω, according to coefficient of heat conductivity, thermal capacitance and the thermal diffusivity parameter of harmonic wave method test philosophy match platinum filament sample; If the analysis to measure result is platinum filament sample coefficient of heat conductivity and thermal diffusivity measured value and actual value (the about 66.7Wm of platinum filament coefficient of heat conductivity
-1K
-1, the about 0.262MJm of thermal capacitance
-3K
-1, thermal diffusivity about 2.54 * 10
-4m
2/ s) meet, promptly finish calibration operation.During official testing, single thread sample 2 is fixed on four parallel lead wire spares 131～134 of thread sample fixture 1 with same method; Thread sample fixture 1 is positioned in the constant temperature vacuum chamber 3, and start-up temperature regulating system 4 makes in the constant temperature vacuum chamber 3 and meets the requirements of temperature; Open pumped vacuum systems 5, treat to close pumped vacuum systems 5 after constant temperature vacuum chamber 3 interior vacuum tightnesss reach requirement; Regulate the maximum resistance that the adjustable resistance R9 that connects is approaching or may reach greater than single thread sample 2 in the measuring process slightly; Feed the simple sinusoidal alternating current of a series of amplitudes for thread sample 2, measure the fundamental voltage amplitude and the third harmonic voltage amplitude of the thread sample between two point of fixity 14b and 14c in the middle of (generally selecting a very low frequency values) under the same frequency as 4Hz; The logarithmic relationship curve of record and analysis third harmonic voltage amplitude and fundamental voltage amplitude, if slope is near 3, the test structure that existing thread sample 2 and four lead-in wire part 131～134 compositions are described is qualified, can carry out subsequent experimental, otherwise should make test structure again; Four lead ends on the thread sample fixture 1 131 to 134 are connected harmonic measurement unit 6, (size of current amplitude should guarantee that third harmonic voltage amplitude size is about 10-150 μ V under the low frequency to give the electric current that thread sample 2 feeds certain amplitude size, and the third harmonic amplitude is more stable when measuring), fundamental voltage amplitude, third harmonic voltage amplitude and the phasing degree of the thread sample between down middle two point of fixity 14b of test different frequency and 14c; Start-up temperature regulating system 4 makes constant temperature vacuum chamber 3 arrive another temperature, write down under this temperature on the thread sample fixture 4 in the middle of the resistance value of the thread sample of 14b and 14c between two point of fixity; Repeat above-mentioned steps until resistance value of noting and corresponding temperature value reach ten groups or more than, calculate the temperature-coefficient of electrical resistance of thread sample 2; Coefficient of heat conductivity, thermal capacitance and thermal diffusivity parameter according to the single thread sample 2 of harmonic wave method test philosophy match.
See also the structure that Fig. 4 illustrates harmonic measurement unit 6 of the present invention, harmonic measurement unit 6 comprises: first operational amplifier 61, second operational amplifier 62, the 3rd operational amplifier 63, prime amplifier 64, signal generator 65, lock-in amplifier 66, system controlled by computer and data acquisition system (DAS) 67, 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 6a, the second current feed end 6d, the first detecting voltage lead end 6b, the second detecting voltage lead end 6c.
Signal generator 65 output angle frequencies are that the ac voltage signal of ω is converted to current signal through first operational amplifier 61, this current signal is used for driving simultaneously adjustable resistance R9 and single thread sample 2, and the voltage signal of adjustable resistance R9 and single thread sample 2 becomes differential wave input lock-in amplifier 66 after prime amplifier 64 amplifies again through second operational amplifier 62 and the 3rd operational amplifier 63 respectively.System controlled by computer and data acquisition system (DAS) 67 control-signals generator 65, lock-in amplifier 66 and adjustable resistance R9.The first current feed end 6a and the second current feed end 6d are electrically connected with the lead end 13a and the 13d of thread sample fixture 1 respectively, and the first detecting voltage lead end 6b and the second detecting voltage lead end 6c are electrically connected with the lead end 13b and the 13c of thread sample fixture 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.
Claims (10)
1. a thermal physical property of single conductive filamentary material by using harmonic method method of testing is characterized in that, comprises that step is as follows:
Step 1: single thread sample is separately fixed on four parallel lead wire spares of thread sample fixture, utilizes the lead-in wire part to have certain thickness and make thread sample keep unsettled;
Step 2: thread sample fixture is positioned in the constant temperature vacuum chamber, and the start-up temperature regulating system makes in the constant temperature vacuum chamber and meets the requirements of temperature;
Step 3: open pumped vacuum systems, treat to close pumped vacuum systems after the interior vacuum tightness of constant temperature vacuum chamber reaches requirement;
Step 4: four lead ends on the thread sample fixture are connected harmonic measurement unit, the simple sinusoidal alternating current of feeding a series of amplitudes for thread sample, measure under the same frequency in the middle of the fundamental voltage amplitude and the third harmonic voltage amplitude of thread sample between two point of fixity;
Step 5: the logarithmic relationship curve of record and analysis third harmonic voltage amplitude and fundamental voltage amplitude, if slope, illustrates that the test structure of existing thread sample and four lead-in wire parts compositions is qualified near 3, execution in step 6, otherwise should make test structure again, get back to step 1 and restart;
Step 6: four lead ends on the thread sample fixture are connected harmonic measurement unit, the electric current of feeding certain amplitude size for thread sample, fundamental voltage amplitude, third harmonic voltage amplitude and the phasing degree of the thread sample between down middle two point of fixity of test different frequency;
Step 7: the start-up temperature regulating system makes and arrives another temperature in the constant temperature vacuum chamber, write down under this temperature on the thread sample fixture in the middle of the resistance value of thread sample between two point of fixity;
Step 8: repeating step 7 reaches at least ten groups until resistance value of noting and corresponding temperature value, calculates the temperature-coefficient of electrical resistance of thread sample;
Step 9: according to coefficient of heat conductivity, thermal capacitance and the thermal diffusivity parameter of the single thread sample of harmonic wave method test philosophy match.
2. thermal physical property of single conductive filamentary material by using harmonic method method of testing as claimed in claim 1, it is characterized in that, in the described step 4, single thread sample adopts faint cycle sinusoidal current heating, during test, adjust the fundamental voltage of described thread sample, the third harmonic voltage in the middle of making between two of two point of fixity lead-in wire part end points is near tens to hundreds of μ V; The frequency values of same frequency is very low, is 4Hz.
3. thermal physical property of single conductive filamentary material by using harmonic method method of testing as claimed in claim 1, it is characterized in that, described faint cycle sinusoidal current, its amplitude size is that the filament of micron dimension is tens milliamperes for measuring diameter, for measuring diameter is that the carbon fiber of micron dimension is the hundreds of microampere, is that the carbon nano-tube of nanometer scale is several microamperes for measuring diameter.
4. thermal physical property of single conductive filamentary material by using harmonic method method of testing as claimed in claim 1 is characterized in that, described humidity control system comprises: a thermopair, a TEC heating/cooling device and a temperature controller; Thermoelectricity is on a rare occasion held and is inserted in the inner chamber, and the other end is electrically connected temperature controller; The TEC heating/cooling device is close to inner chamber and is placed heat-insulation layer, and is controlled start and stop by temperature controller; The reading of thermopair is delivered to temperature controller by set algorithm decision hot/cold amount, thereby realizes temperature automatically controlled to inner chamber by the action of the output order control TEC heating/cooling device of temperature controller again.
5. thermal physical property of single conductive filamentary material by using harmonic method method of testing as claimed in claim 1 is characterized in that, is used to measure coefficient of heat conductivity, thermal capacitance and the thermal diffusivity parameter of microscale conduction filamentary materials such as single piece of metal filament, carbon fiber or carbon nano-tube.
6. the thermal physical property of single conductive filamentary material by using harmonic method proving installation that the method for claim 1 is used comprises: constant temperature vacuum chamber, humidity control system, pumped vacuum systems, harmonic measurement unit; It is characterized in that, also comprise: thread sample fixture; Thread sample fixture is placed horizontally at the bottom of the constant temperature vacuum chamber inner chamber, is electrically connected with harmonic measurement unit; The thermoelectricity of humidity control system is on a rare occasion held and is inserted in the inner chamber, and the other end is electrically connected temperature controller; The TEC heating/cooling device is close to internal chamber wall, places heat-insulation layer; Constant temperature vacuum chamber inner chamber and pumped vacuum systems interlink;
Thread sample fixture comprises base, a plurality of lead-in wire spare; Base upper surface is covered with insulation course, even parallel four the lead-in wire parts that set firmly of insulation course upper surface, and strip lead-in wire part horizontally set, the one end is a lead end; Insulation course is silicon dioxide or silicon nitride layer, and the lead-in wire part is that copper product is made;
During test, single thread sample is fixed on four parallel lead wire spares, and the axially length direction with four lead-in wire parts of thread sample is vertical, utilizes the thickness of lead-in wire part to make thread sample keep unsettled, and harmonic measurement unit is electrically connected with single thread sample through lead end.
7. thermal physical property of single conductive filamentary material by using harmonic method proving installation as claimed in claim 6, it is characterized in that, described harmonic measurement unit is electrically connected with single thread sample through lead end, two lead ends are connected by lead with the harmonic wave detecting voltage lead end of harmonic wave probe unit respectively in the middle of being, the current feed end of harmonic measurement unit inserts two lead end cycles of both sides to single thread sample electrical heating by lead.
8. thermal physical property of single conductive filamentary material by using harmonic method proving installation as claimed in claim 6, it is characterized in that, even parallel four the lead-in wire parts that set firmly of described base upper surface, the one, when measuring carbon fiber that diameter is a micron dimension or filament, the lead-in wire part by conducting metal by electroplate and etch process attached to forming four thick bond pad shapes structures of tens micron dimensions on the printed wiring board base, diameter be micron dimension thread sample by gold wire bonder pressure welding or the bonding technology of elargol be separately fixed at four the lead-in wire parts an end, form four point of fixity;
The 2nd, when the measurement diameter is the carbon nano-tube of nanometer scale, at thickness the thick insulation course of deposition tens nanometer scale on the silicon chip base of hundreds of micron earlier by high-temperature oxidation, prepare single-root carbon nano-tube then, adopt the nickel coated carbon nanotube of focusing of ion beam process deposits one layer thickness 2～3nm again, be several millimeters carbon nano-tube pipe range direction then along length, with several microns is the spacing about 1 μ m of deposition width thereon, the about 200nm of thickness, length is about four gold solder dishes of 1mm as the lead-in wire part, and the space of elimination pad and carbon nano-tube contact position, reduce thermal contact resistance.
9. thermal physical property of single conductive filamentary material by using harmonic method proving installation as claimed in claim 8 is characterized in that, described preparation single-root carbon nano-tube is the technology preparation that proposes by Yu C.
10. thermal physical property of single conductive filamentary material by using harmonic method proving installation as claimed in claim 8 is characterized in that, the thickness of the base of described thread sample fixture is 0.5～2mm, and width or length are 0.2～20mm; Thickness of insulating layer is 20～200nm; Lead-in wire part width is 1～1000 μ m, and length is 1～10mm, and thickness is 200～25000nm; Adjacent two single thread sample point of fixity spacings are between 0.5～500 μ m.
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