CN104535611B - Solid specific heat capacity measurement standard device and measurement method - Google Patents
Solid specific heat capacity measurement standard device and measurement method Download PDFInfo
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- CN104535611B CN104535611B CN201510024191.XA CN201510024191A CN104535611B CN 104535611 B CN104535611 B CN 104535611B CN 201510024191 A CN201510024191 A CN 201510024191A CN 104535611 B CN104535611 B CN 104535611B
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Abstract
The invention belongs to the field of measurement science and relates to a solid specific heat capacity measurement standard device for solid specific heat capacity measurement and a measurement method. The solid specific heat capacity measurement standard device (100) comprises a sample container (10), an adiabatic following device (20), an air inflating and deflating system (30) and a measurement control system (40), wherein the measurement control system (40) comprises a sample heating system (42), a sample heating energy re-measurement system (41), a temperature measurement system (43), an adiabatic following control system (44) and a computer (45). According to the solid specific heat capacity measurement standard device, highly automatic control during measurement can be realized, and excessive guarders are not needed; and the temperature of the whole sample container can be easily uniform, so that the high adiabaticity of the sample container can be ensured, and solid specific heat capacity can be measured accurately.
Description
Technical field
The invention belongs to field of metrology science, is related to a kind of specific heat of solid and heat measurement criteria for specific heat of solid and heat measurement
Shuttle and adiabatic tracks of device that device and the device include, and adopt the specific heat of solid and heat metrological standard unit
Measuring method.
Background technology
Specific heat capacity (abbreviation thermal capacitance) is one of hot physical property of material, by the measurement of thermal capacitance, on the one hand can obtain enthalpy,
The Basic thermodynamics data such as entropy, Gibbs free energies, on the other hand can also obtain the aspects such as structure about material, phase transformation
Important information.The assay method of thermal capacitance is divided into absolute method and relative method, relative method mainly including DSC, DTA etc., its precision and standard
Exactness is well below absolute method.It is (as shown in Figure 1) it can be seen that the thermodynamics number of relative method from China's thermal capacity value traceability system
Need by one-level α-Al according to measurement2O3Molar heat capacity standard substance is calibrated, and could ensure value accurately and reliably.Wherein
It is to realize effectively measuring basic assurance that is i.e. accurate, comparable, can tracing to the source, country's measurement as the standard substance of magnitude tracing carrier
Disjunction mark standard is the source of standard substance magnitude tracing, is the key problem for ensureing magnitude tracing.The national measurement institute of various countries in order to
Trade development, standard market order, Promote Technology, improve constantly the measurement level of national disjunction mark standard apparatus, develop
Superiority of the related standard substance to be maintained in the market competition of fierceness.Current China one-level α-Al2O3Molar heat capacity mark
Quasi- material and one-level heat analysis standard substance lack metrological standard unit definite value, and original primary standard amount of material is limited, make
For national highest level metrological service, it is standard substance definite value to set up specific heat of solid and heat metrological standard unit, complete so as to be lifted
The measurement level of state's thermodynamics measurement data, it is ensured that China's measurement of correlation analytical tool measurement data it is accurate, while also to open
The standard substance for opening up more wide temperature range lays a good foundation, therefore, set up the work of specific heat of solid and heat metrological standard unit
It is extremely urgent.
Specific heat of solid and heat measurement apparatus are divided into two types by mode of heating difference：A kind of is to be interrupted hot type, Yi Zhongwei
Laser heating type.For mesophilic range, the general mode of heating using discontinuous.Heating is continuously or discontinuously as needed
To adjust what is realized by controller.In whole temperature range, 5 degree or 10 degree are raised often, stop heating, into balance period,
After reaching equilibrium condition, continue heating, here it is alleged discontinuous heating.
To develop the thermal capacitance measurement apparatus of high precision high accuracy, need to develop a set of adiabatic calorimeter device, and fill
Put design, tracking screen and insulated design that most crucial part is shuttle.Wherein, shuttle has and holds sample, pacifies
Put heater and keeping temperature field uniformly acts on.Three then scattered and disappeared around suppression, isolation heat with insulated design are shielded in tracking
The approach of kind.Heat scatters and disappears three kinds of approach, convection current, conduction and radiation, and tracking screen and insulated design are needed around these three approach
Launch.
Zhang Jintao etc. proposes a kind of High Precision Automatic Adiabatic Calorimeter to standard substance α-Al2O3Specific heat measurement is carried out
(" High Precision Automatic Adiabatic Calorimeter " measures journal, Vol.26, No.4, in October, 2005,320-325), this article is introduced
This specification, as reference.The Automatic Adiabatic calorimeter structure of its report is as follows：Shuttle holds for the cylindrical enclosure of thin-walled
Device, volume about 60ml, outer surface are gold-plated to reduce radiation heat transfer, and shuttle mouth is sealed with soldering, extract internal empty after sealing out
Gas, is filled with helium, and the helium being filled with is sealed in shuttle, to strengthen the friendship of the convection of heat between sample and sample heating device
Change；There is the system that the heat radiation screen that can track sample temperature, shuttle and heat radiation screen are constituted to be placed in one outside shuttle
In vacuum interlayer, vacuum interlayer is soaked in liquid nitrogen, therefore, heat radiation screen is placed in the environment of shuttle and liquid nitrogen temperature
Between；Heat radiation screen outer surface is equably disposed between heater strip, with shuttle has thermoelectricity to push away, end of probe and ginseng that thermoelectricity is pushed away
Examine end to be connected on the inwall of shuttle outer wall and heat radiation screen, its potential difference signal is admitted to controller, controller
Feedback adjustment signal control heat radiation screen heater power source so that potential difference signal is gone to zero all the time.Therefore, by such
Temperature control regulating system, the temperature of heat radiation screen are controlled all the time so as to track the wall surface temperature of shuttle.This thermal insulation
The defect that calorimeter is present is mainly：(1) shuttle mouth is sealed with soldering every time, and it is empty that do so directly influences shuttle
The measurement of equivalent, this process itself do not have a very strong repeatability, the uncertainty of introducing than larger, meanwhile, repeat stannum
Weldering also easily causes the damage of unrepairable to device；(2) use of such design in shuttle, is very uneconomical
, because welding quality has higher requirements in processing technique, it is desirable to which weld seam is resistant to vacuum, if vacuum is bad,
Then there is leakage in the noble gases in shuttle in the case of being heated, so as to affect the accuracy of measurement result；(3) Zhang Jintao
Deng within the temperature range of 80～275K using the adiabatic calorimeter to α-Al2O3Calorimetric experiment is carried out.
Chinese patent 200810010885.8 discloses a kind of Calorimetry system, and this patent documentation introduces this specification, makees
It is reference.Wherein, disclosed adiabatic calorimeter keeps adiabatic environment using three layers of heat screen temperature control, shuttle by upper lid and
Main body is constituted, and the lateral margin of the upper end outer wall of main body is provided with sealing margin, and upper cover buckle is bonded together in blend compounds on sealing margin
Be tightly connected, on upper lid, be connected with capillary tube and link, heater strip is wound on the outer wall of main body, be provided with main body fin,
Thermometer and show differential thermal galvanic couple, shuttle is hung in interior heat screen by link, and capillary tube fills helium for shuttle.
This Calorimetry system there is also above-mentioned similar problem, be essentially all to leave for solving the problems, such as heat exchange from a point.But
From for a device, it should can be what is be reused, and every time using produce error be within the specific limits,
It is a determination state.So, the reuse of device will be taken into full account in design, simultaneously for shuttle and dress
The space amount put all can be accurate measurement, thus can reduce the error of device to greatest extent.
Above-mentioned adiabatic calorimeter employs one layer of heat radiation screen or three layers of heat screen on adiabatic tracks of device is designed, but
Avoid a critically important problem-thermograde, i.e. shuttle internal heater and shuttle and directly there is temperature ladder
Degree, shuttle upper and lower directly there is also thermograde, and this problem is equally there is also on tracking screen, due to temperature
The presence of gradient, tracking temperature occur error, it is also difficult to avoid the heat exchange between shuttle and tracking screen, thus
It is difficult to the strict energy for confirming to inject in shuttle.
The most of measurement warm area of existing adiabatic calorimeter is also confined to below 350K, more than the calorimeter pole of 400K warm areas
It is few.This is primarily due to the rising with temperature, and the heat exchange caused by radiant heat transfer is than heat exchange that convection current and conduction cause
It is much bigger, for adiabatic difficult increase is realized, increase the thermal capacitance measurement error of measured matter, meanwhile, in higher temperature
Under, the Insulation Problems of the sealing, heater strip and lead of sample are highlighted.
Therefore, for adiabatic calorimeter, more scientific reasonable design thermal insulation tracks of device and shuttle are guaranteeing sample
The high thermal insulation of container, scientific design fill emission control to realize easy to operate and automatization automatically, so as to more accurate
Ground measurement specific heat of solid and heat, realizes that specific heat capacity measurement data is traced to the source to international SI units, there are needs in this regard.
The content of the invention
Technical problem
In order to solve the above problems, it is an object of the present invention to provide a kind of fill for specific heat of solid and heat measurement criteria
The shuttle put, by appropriate design, in measurement, whole shuttle temperature is uniform, and need not use soldering for the shuttle
Seal and be glued sealing.
Another object of the present invention is to a kind of adiabatic tracks of device for specific heat of solid and heat metrological standard unit is provided,
The adiabatic tracks of device solves the problems, such as thermograde, it is ensured that the high thermal insulation of shuttle.
The a further object of the present invention is to provide the specific heat of solid and heat meter for including above-mentioned shuttle and adiabatic tracks of device
Amount standard set-up, the specific heat of solid and heat metrological standard unit can realize increasingly automated control without the need for excessive people in measurement
Work is on duty, and accurately measures specific heat of solid and heat.
A further object of the present invention is to provide using above-mentioned specific heat of solid and heat metrological standard unit accurate measurement solid ratio
The method of thermal capacitance.
Technical scheme
According to an aspect of the present invention, provided by the present invention for the shuttle of specific heat of solid and heat metrological standard unit
10 are made up of sample cell body 11, bottom of pond 12 and pond lid 13, and pond body 11 and bottom of pond 12 are with being combined into gap cooperation, pond lid 13 and pond body
11 cooperation also coordinates for gap；At least two auxiliary lamellar ceramic heaters 14 are disposed with the sample cell bottom, at least
Two main leaf shape ceramic heaters 15 are symmetricly set in sample cell, and a standard temperature sensor 17 is arranged in sample cell
The heart, at least two operating temperature sensors 16 are arranged between flaky pottery heater 15 and pool wall.
According to a further aspect of the invention, provided by the present invention for the adiabatic tracking dress of specific heat of solid and heat metrological standard unit
20 are put, includes Dewar flask 21, tracking screen 22, heat screen 23 and housing 24 from inside to outside successively.Wherein, the Dewar flask 21 is by bottle
Body and bottle cap composition, the bottle and bottle cap are made by high-temperature resistant double-layer quartz glass, are true in double-deck inside quartz glass
Empty and have silver coating, vacuum is 10-5～10-6Pa, the bottom of bottle are provided with wire hole, and hole is embedded with ceramic insulating tube；
The tracking screen 22 is arranged on outside Dewar flask 21, is made up of red copper, and the bottle by closure of openings and bottom of bottle group
Into being disposed with least two flaky pottery heaters 221 in bottom of bottle, and be disposed with operating temperature sensor 222, and bottom of bottle sets
Wire hole is equipped with, hole is embedded with ceramic insulating tube；
The heat screen 23 is arranged on outside tracking screen 22, is made of stainless steel, is multiple structure, bottom of bottle, body and bottle
Lid stud is fixed as entirety, and bottom of bottle is provided with wire hole, and hole is embedded with ceramic insulating tube；
The housing 24 is arranged on outside heat screen 23, is made of stainless steel, and is made up of housing and shell bottom, housing and shell bottom
Connected using vacuum sealing flange, shell bottom is provided with vacuum high-density connector, high-precision pressure sensor and fill exhaust port.
Further aspect of the invention, the specific heat of solid and heat metrological standard unit 100 that the present invention is provided include that sample holds
Device 10, adiabatic tracks of device 20, inflating and exhausting system 30 and Measurement and Control System 40, wherein, shuttle 10 be placed in it is adiabatic with
In track device 20；
The inflating and exhausting system 30 is for inflating and aerofluxuss to shuttle 10 and adiabatic tracks of device 20；
The Measurement and Control System 40 includes：For controlling the sample heating system 42 of the heating of shuttle 10；For surveying
The sample heat energy of amount injection sample energy size returns examining system 41；For 10 temperature of shuttle and adiabatic tracks of device 20
Temperature real-time measurement temperature measurement system 43；For the adiabatic tracking control system 44 of the control of adiabatic tracks of device 20；With
And for the computer 45 of data acquisition and processing (DAP).
According to another aspect of the invention, the above-mentioned specific heat of solid and heat metrological standard unit measurement of employing that the present invention is provided is solid
The method of body specific heat capacity, the method include：Shuttle 10 and adiabatic tracks of device 20 under inert gas atmosphere, determine empty sample
The thermal capacitance of product container 10, then determines the thermal capacitance of the shuttle 10 for being loaded with testing sample, calculates the mole hot of sample by following formula
Hold：
In formula：Quality (g) of the m for sample,
Molal weights (g/mol) of the M for sample,
ce、cfRespectively empty shuttle, be loaded with testing sample shuttle mean heat capacity (J/K),
cm(T) mean molal heat capacity (J/molK) for sample.
Beneficial effect
The specific heat of solid and heat metrological standard unit of the present invention, in measurement, adiabatic tracks of device is in identical with shuttle
Inert atmosphere under, without the need for soldering or be glued to shuttle seal, and in shuttle by aid in lamellar pottery
The distribution of porcelain heater 14 and main leaf shape ceramic heater 15, in measurement, whole shuttle temperature is easy to uniform；
Dewar flask 21 is set in adiabatic tracks of device 20 and solves the problems, such as thermograde, it is ensured that the height of shuttle is absolutely
It is hot；
The specific heat of solid and heat metrological standard unit can realize increasingly automated control without the need for excessive artificial in measurement
It is on duty, and accurately measure specific heat of solid and heat.
Description of the drawings
Fig. 1 is China's thermal capacity value traceability system schematic diagram；
Fig. 2 is the structural representation of the shuttle 10 of the present invention, wherein (A) is the sectional view along line A-A, (B) it is sample
The structural representation of product container 10, (C) be 10 bottom of pond 12 of shuttle structural representation；
Fig. 3 is the structural representation of the adiabatic tracks of device 20 of the present invention；
Fig. 4 is the structural representation for filling automatically emission control 30 of the present invention；
Fig. 5 is the structural representation of the specific heat of solid and heat metrological standard unit 100 of the present invention.
Specific embodiment
Below, with reference to the accompanying drawing present invention more particularly described below.
Shuttle of the invention 10 as shown in Fig. 2 which is made up of pond body 11, bottom of pond 12 and pond lid 13, the pond
Body 11, bottom of pond 12 and pond lid 13 are made by fine silver, using fine silver material, mainly consider that the heat conductivity of silver is very good, are steel
Seven times, specific heat capacity is little, so can ensure that the sample in sample cell is heated evenly, and heat absorption is relatively good；The pond body
11 spatial volume constituted with bottom of pond 12 are 70ml～100ml, for example, can be 80ml；The thickness of bottom of pond 12 be 8～14mm, example
Can such as be 12mm；The wall thickness of pond body 11 and Chi Gai is 2～5mm, for example, can be 3mm；The sample cell can for square or
Person's cylinder, and it is preferably cylindrical；Pond body 11 and bottom of pond 12, and pond body 11 is gap cooperation with the cooperation of pond lid 13.
At least two auxiliary lamellar ceramic heaters 14 are disposed with the sample cell bottom, for example, can be at least two
2.7～3 ohm, 3 watts of auxiliary lamellar ceramic heater 14, and preferably three 3 ohm, 3 watts of auxiliary lamellar ceramic heat
Device 14, around the distribution triangular in shape of sample cell bottom centre, this 3 ohm, 3 watts of auxiliary lamellar ceramic heater 14 be circle,
It is auxiliary heater, for heating sample cell bottom of pond, which is used as to compensate the temperature difference between the upper and lower differing heights of sample cell；At least two
Individual main leaf shape ceramic heater 15, for example, can be at least two 250～400 ohm, 200 watts of main leaf shape ceramic heater 15
It is symmetricly set in sample cell, and preferably three 380 ohm, 200 watts of main leaf shape ceramic heater 15, in sample cell
Heart distribution triangular in shape, the main leaf shape ceramic heater 15 are square, are primary heaters, for heating sample and sample cell；It is right
In the auxiliary lamellar ceramic heater 14, sample cell bottom is tightly mounted on by way of welding；For the main leaf shape
Ceramic heater 15, is attached with the fine silver fin that maximum gauge is 4 millimeters, in this way on two surfaces, it is ensured that heating
The sample that the energy efficient of device is passed in sample cell.
One standard temperature sensor 17 is arranged on sample cell center, specially 25 ohm standard temperature sensors, the mark
Quasi- temperature sensor is the working standard grade platinum resistance temperature sensor of Jing measurement unit certifications, is so measured in specific heat of solid and heat
Thermometric precision and accuracy are can ensure that in standard set-up system, the uncertainty of single unit system is reduced；At least two
Operating temperature sensor 16 is arranged between main leaf shape ceramic heater 15 and pool wall, and preferably 3 100 ohm of operating temperatures
Sensor 16, the operating temperature sensor accuracy are slightly below standard temperature sensor, are equally through measurement unit certification, mainly
For monitoring the change in sample temperature field in heating process in sample cell.
The shuttle 10 be used for specific heat of solid and heat metrological standard unit when, the operating temperature sensor 16 and mark
Quasi- temperature sensor 17 passes through wire and vacuum high-density connector is connected with temperature measurement system 43, the auxiliary flaky pottery
Heater 14, main leaf shape ceramic heater 15 pass through wire and vacuum high-density connector is connected with sample heating system 42.Meter
The temperature of the standard temperature sensor that calculation machine 45 is measured from 43 retaking of a year or grade of temperature measurement system by Ethernet and operating temperature sensing
The temperature of device, sets up the models for temperature field of sample in current sample pond, and checks the temperature of which part in sample pool space not
Unanimously, instruction is sent to sample heating system 42 by Ethernet from computer 45 then, controls the heater work of corresponding site
Make, ensure that the uniform temperature fields of sample are consistent.
Adiabatic tracks of device of the invention 20 is as shown in figure 3, include Dewar flask 21, tracking screen from inside to outside successively
22nd, heat screen 23 and housing 24, wherein,
21 volume of the Dewar flask can be 500～600 milliliters, for example, can be 520 milliliters；Which is by bottle and bottle cap group
Made by high-temperature resistant double-layer quartz glass into, the bottle and bottle cap, wall thickness is 2～6 millimeters, for example, can be 3 millimeters；
Double-deck inside quartz glass is vacuum and has silver coating, and vacuum can be 10-5～10-6Pa, for example, can be 10-6Pa；Bottle
The bottom of body is provided with wire hole, for example can be 5 wire holes, for for example by the temperature sensor lead of sample cell and plus
Hot device wire wears out, and wire hole is embedded with ceramic insulating tube.
Dewar flask 21 is set in adiabatic tracks of device 20 and solves the problems, such as said temperature gradient, Dewar flask belongs to one-level
Adiabatic apparatus, condition of high vacuum degree Dewar flask have good insulating characteristicses, convection current and radiation-induced heat scatter and disappear can ignore not
Meter, and for the conduction effect of bottleneck, then need to coordinate adiabatic tracking screen lost to reduce heat.
The tracking screen 22 is arranged on outside Dewar flask 21, is made up of red copper, and volume is 3～4 liters, for example, can be 3.3
Rise, wall thickness is 3～6 millimeters, for example, can be 6 millimeters；Tracking screen 22 is made up of the bottle and bottom of bottle of closure of openings, in bottom of bottle cloth
At least two flaky pottery heaters 221 are equipped with, for example, are disposed with least two 250～400 ohm, 200 watts of flaky pottery
Heater 221, is preferably arranged with three or four 250～400 ohm, 200 watts of flaky pottery heater 221, and in bottle
Base fabric is equipped with temperature sensor 222, and bottom of bottle is provided with wire hole, for example, can arrange 5 wire holes, and hole is embedded with ceramic exhausted
Edge pipe.
By monitor 10 temperature of shuttle and tracking screen temperature, if the temperature difference of the two be more than 0.6 degree, start with
The heater of track screen, to tracking screen heating, and ensures that the temperature for tracking screen is lower than shuttle 10, but the temperature difference is not more than 0.6 degree.
When tracking screen 22 tracks the temperature of shuttle 10, although the insulation effect of Dewar flask is good, but does not accomplish complete thermal insulation, if
The temperature of Dewar flask both sides is consistent, then the heat leak of Dewar flask is with regard to very little.
The heat screen 23 is arranged on outside tracking screen 22, is made of stainless steel, is multiple structure, bottom of bottle, bottle and bottle
Lid stud is fixed as entirety.More specifically, the heat screen 23 is made up of 10 layers of rustless steel cylinder, bottom of bottle, bottle and bottle cap spiral shell
Post is fixed as entirety, and the gap between 10 layers of rustless steel cylinder can be 4.8 millimeters, a diameter of 185 millimeters of innermost layer, outermost
A diameter of 275 millimeters of layer, the thickness of every layer of rustless steel cylinder is 0.2 millimeter, and bottom of bottle has 5 wire holes, and hole is embedded with absolutely
Edge earthenware.Thermal convection current and heat exchange are greatly reduced by the form of multi-layer cylinder.
The housing 24 is arranged on outside heat screen 23, is made of stainless steel, and is made up of housing and shell bottom, housing and shell bottom
Connected using vacuum sealing flange, shell bottom vacuum high-density connector, certainty of measurement are installed for 0.03% pressure transducer and
Fill exhaust port.After housing is connected with shell bottom, the pressure of 1～1.3 atmospheric pressure can be born and do not revealed；Pressure transducer is used
To monitor pressure change of the enclosure interior in exhaust process and sample heating process is filled；Fill exhaust port fills row for device
Gas process.
The specific heat of solid and heat metrological standard unit 100 that the present invention is provided, including shuttle 10, adiabatic tracks of device 20,
Inflating and exhausting system 30 (be for example specifically as follows and fill automatically emission control 30) and Measurement and Control System 40, wherein, measurement control
It is (such as lucky that system processed 40 returns examining system 41 (such as Agilent circuit tester 3458A), sample heating system 42 by sample heat energy
When sharp power supply 2425), temperature measurement system 43 (such as ASL bridge for measuring temperature F650), adiabatic 44 (such as Beijing of tracking control system
The ATCS-2000 Automatic Adiabatic controllers of Run Tian Instrument Ltd. of Air China) and the composition such as computer 45, Fig. 5 shows this
The structural representation of the specific specific heat of solid and heat metrological standard unit of bright one 100.
Inflating and exhausting system 30 for inflating and aerofluxuss to shuttle 10 and adiabatic tracks of device 20, as long as can be used for
Shuttle 10 and adiabatic tracks of device 20 are inflated and aerofluxuss, and which is not restricted, for example can be true using vacuum pumping
Idle discharge gas, can be filled with the noble gases in gas cylinder in shuttle 10 and adiabatic tracks of device 20 by air relief valve.At this
In invention, inflating and exhausting system 30 be preferably it is as shown in Figure 4 fill automatically emission control 30, for shuttle 10 and absolutely
Thermal follow-up unit 20 is inflated and aerofluxuss, and this fills mechanical pump and molecular pump 31, unidirectional of the emission control 30 by integration automatically
Valve 32, gas tank 33, accurate ratio adjusting valve 34, air relief valve 36, electromagnet cut off valve 35, noble gases gas cylinder 37 and automatic controller
38 compositions, wherein, the mechanical pump and molecular pump 31 of integration are connected with check valve 32, and check valve 32 is connected with gas tank 33, gas tank
33 are connected with accurate ratio adjusting valve 34, and noble gases gas cylinder 37 is connected with air relief valve 36, air relief valve 36 and precision proportion adjustment
Valve 34 connects, and accurate ratio adjusting valve 34 is connected with electromagnet cut off valve 35, automatic controller 38 control integration mechanical pump and
Molecular pump 31, check valve 32, accurate ratio adjusting valve 34, air relief valve 36, the startup of electromagnet cut off valve 35, regulation and closing.
Automatically the emission control 30 of filling can be with 20 housing 24 of adiabatic tracks of device by electromagnet cut off valve 35
Fill exhaust port connects, such that it is able to inflate and aerofluxuss to shuttle 10 and adiabatic tracks of device 20.Gas tank 33 need not be controlled
System, noble gases gas cylinder 37 can be opened manually, the mechanical pump and molecular pump 31, list of 38 control integration of automatic controller control
To valve 32, accurate ratio adjusting valve 34, air relief valve 36, the startup of electromagnet cut off valve 35, regulation and closing.Wherein, it is integrated
Mechanical pump and molecular pump 31 are for by 10 evacuation of adiabatic tracks of device 20 and shuttle；Noble gases gas cylinder 37 and decompression
Valve 36 is for being filled with noble gases, such as argon or helium to adiabatic tracks of device 20 and shuttle 10, particularly preferably
Argon；Inflation and exhaust process are controlled by accurate ratio adjusting valve；Electromagnet cut off valve be used for cutting off adiabatic tracks of device 20 with
Extraneous path；The effect of gas tank is to maintain the pressure stability in loop.
Automatic controller 38 under the instruction of the computer 45 of Measurement and Control System 40, with exhausted in adiabatic tracks of device 20
Be reference to pressure, using fuzzy algorithmic approach, control voltage is sent to accurate ratio adjusting valve 34, it is slow according to the first predetermined curve
Reduce the pressure in device, until it reaches the vacuum requirement of adiabatic tracks of device 20, adiabatic tracks of device is controlled by pid algorithm
Vacustat in 20, and kept for a period of time under the vacuum state, gas molecule is fully spread, be beneficial to emptying exhausted
Residual air composition in thermal follow-up unit 20.Subsequent automatic controller 38 is according to the second predetermined curve to accurate ratio adjusting valve 34
Control voltage is sent, under pressure transducer closed loop feedback, requires to be slowly injected into noble gases (such as argon) according to pressure curve,
Until the pressure of noble gases reaches pre-provisioning request in device, and by inert gas pressure in pid control algorithm control device
Stablize, noble gases is fully spread, balance, realize device gas replenishment process.The calculating of Measurement and Control System 40 can be passed through
Machine 45 controls charge, exhaust number of times, it is ensured that air is drained in adiabatic tracks of device 20, improves the indifferent gas in adiabatic tracks of device 20
Body purity, and according to the pressure value of noble gases in the accurate temperature amendment thermal insulation tracks of device 20 in adiabatic tracks of device 20,
Guarantee that the inert gas mass being filled with adiabatic tracks of device 20 every time is constant.
In specific heat of solid and heat metrological standard unit 100, the auxiliary lamellar ceramic heater 14 of shuttle 10 and main leaf
Shape ceramic heater 15 is heated with sample heating system 42 and sample by the vacuum high-density connector on wire and housing 24
Energy returns examining system 41 and connects；The flaky pottery heater 221 of adiabatic tracks of device 20 is by the vacuum on wire and housing 24
High-density connector is connected with adiabatic tracking control system 44；The operating temperature sensor 16 of shuttle 10 and standard temperature are passed
The operating temperature sensor 222 of sensor 17 and adiabatic tracks of device 20 is by the vacuum high density connection on wire and housing 24
Device is connected with temperature measurement system 43；Automatically the automatic controller 38 and computer 45 for filling emission control 30 passes through Ethernet
Line connects；Sample heating system 42, sample heat energy return examining system 41, adiabatic tracking control system 44, temperature measurement system
43 grades are connected by ethernet line with computer 45.
Automatically inflating and exhausting system 30 receives the instruction of computer 45 by Ethernet, is automatically performed 20 He of adiabatic tracks of device
The evacuation of shuttle 10, the process for being filled with noble gases (such as argon), and ensure that original state is filled with noble gases
Slightly below one atmospheric pressure of pressure (because subsequent heat process, the pressure of gas can increase, for the pressure for reducing sealing,
So the pressure for being filled with noble gases in original state is slightly below an atmospheric pressure).
44 (the ATCS-2000 Automatic Adiabatic controls of such as Run Tian Instrument Ltd. of Beijing Air China of adiabatic tracking control system
Device processed) and adaptive control algorithm based on fuzzy logic sluggish using great Lin, the temperature of shuttle 10 and adiabatic tracking dress
The temperature for putting the tracking screen 22 in 20 is gathered by temperature measurement system 43 (such as the bridge for measuring temperature F650 of ASL companies), is passed through
Ethernet, issues adiabatic tracking control unit system 44 by computer 45.The sample for gathering is held by adiabatic tracking control unit system 44
Device temperature and tracking screen temperature relatively and carry out fuzzy reasoning, produce three parameters of PID control, the sluggish weightings of Jing great Lin by
PID automatically adjusts output, heating power is adjusted automatically, controlled with design temperature deviation with real time temperature, real
Existing step-less adjustment, reaches the purpose of the fast automatic Loading Control of temperature.Guarantee that temperature following is good by Adaptive PID Control,
Temperature fluctuation is little, it is ensured that tracking screen 22 is less than 0.6K with the temperature difference of shuttle 10, causes so as to eliminate convection current and radiation
Heat transfer, and reach the insulation effect of adiabatic tracks of device 20.
The auxiliary lamellar ceramic heater 14 and main leaf shape ceramic heater 15 of shuttle 10 and sample heating system 42
(such as Keithley power supply 2425) and sample heat energy return examining system 41 (such as Agilent circuit tester 3458A) connection, computer
45 send heating instructions to sample heating system 42 by Ethernet, and sample heat energy returns examining system 41, and reading is heated back in real time
The magnitude of voltage and current value on road, and computer 45 is sent to by Ethernet, computer is by formulaCan be with accurate measurement
And calculate the energy Q of injection shuttle 10.Meanwhile, temperature measurement system 43 (the bridge for measuring temperature F650 of such as ASL companies)
The temperature value of the operating temperature sensor 16 and standard temperature sensor 17 of collection shuttle 10, and meter is issued by Ethernet
Calculation machine 45, computer 45 can calculate the sample temperature change Delta T after being input into certain energy every time.
The method that specific heat of solid and heat is measured using above-mentioned specific heat of solid and heat metrological standard unit of the invention, the method
Including：Shuttle 10 and adiabatic tracks of device 20 under inert gas atmosphere, determine the thermal capacitance of empty shuttle 10, then survey
Surely the thermal capacitance of the shuttle 10 of testing sample is loaded with, the molar heat capacity of sample is calculated by following formula：
In formula：Quality (g) of the m for sample,
Molal weights (g/mol) of the M for sample,
ce、cfRespectively empty shuttle, be loaded with testing sample shuttle mean heat capacity (J/K),
cm(T) mean molal heat capacity (J/molK) for sample.
The method that specific heat of solid and heat is measured using the specific heat of solid and heat metrological standard unit of the present invention is specifically described below.
1. the basic functional principle of specific heat of solid and heat is measured：
Based on Absolute Measurement principle, carried out using the adiabatic calorimetry of interruption heating.Determination sample container is flat first
Weighing apparatus temperature, the temperature for being input into a certain amount of electric energy, the size for determining this electric energy and the shuttle for causing to shuttle are raised,
The equilibrium temperature of determination sample container again after shuttle temperature reaches balance, repeats this operation until the upper limit temperature of experiment
Degree.The thermal capacitance of shuttle is calculated by following equation：
In formula：V (t), I (t) are the terminal voltage (V) and heated current (A) on heater,
T is heating time period (sec),
Δ T is experiment temperature rise (K).
Within the temperature range of measurement, empty shuttle thermal capacitance (also known as space amount) is determined respectively and testing sample is loaded with
Shuttle (also known as full container) thermal capacitance, you can the molar heat capacity of sample is calculated by following formula：
In formula：Quality (g) of the m for sample,
Molal weights (g/mol) of the M for sample,
ce、cfRespectively space amount, the mean heat capacity (J/K) of full container,
cm(T) mean molal heat capacity (J/molK) for sample.
Under full container state, in shuttle, amount of inert gas is fewer than under space amount state, thus produces noble gases
Thermal capacitance difference can adopt following equation amendment：
In formula：ρaFor the density (kg/m of noble gases under space amount original state3)；
VmFor the volume (m for adding sample under full container state3)；
MaFor the molal weight (g/mol) of noble gases under space amount original state；
cpa(T) specific heat capacity (J/ (molK)) for being noble gases at a temperature of T.
According to formula above, noble gases thermal capacitance can be changed poor according to the temperature change of space measurement process.
Under experimental temperature, sample thermal capacitance experiment value is gone out using least square fitting after the difference amendment of noble gases thermal capacitance
Following multinomial：
In formula：cs(T) it is the sample molar heat capacity under T temperature spots；
Coefficients of the A for polynomial fitting；
T is sample temperature.
Thus the easypro level values of sample molar heat capacity can be calculated.
2. measuring method：
1) Preparatory work of experiment work：
Laboratory temperature is maintained at 20 ± 2 DEG C during testing.Open all measuring apparatus in specific heat of solid and heat device
Carry out 1～2h of preheating.The Measurement and Control System of starter so as to enter working condition.
2) sealing of adiabatic tracks of device and noble gases are filled with：
After the housing 24 of adiabatic tracks of device 20 is sealed, emission control 30 is filled in startup automatically, works as system vacuum
1.33Pa is reached, (such as argon, purity are 99.99%), to slightly above 1 atmospheric pressure, Ran Houguan to be filled with high purity inert gas
Inflation system is closed, starts degassing function evacuation.The above-mentioned pumping of repetition and charge operation 3 times, the pressure for finally keeping system is
80KPa, and the pressure value inside adiabatic tracks of device is issued into computer by Ethernet.
3) measurement of space amount：
10 temperature of shuttle is adjusted to starting experimental temperature.Temperature measurement system is according to adopting per the speed of 10 seconds points
Collection 10 Plays temperature sensor of shuttle and the temperature of operating temperature sensor, through the analysis and calculating in temperature field, obtain
To the mean temperature of shuttle at that time, then, rate of temperature change is calculated per 20 points.When rate of temperature change is less than 5 × 10-4K/
During min, system reaches balance.After shuttle balance period terminates, computer is injected to the setting of sample heating system by Ethernet
Energy value, and heating instructions are sent, constant heated current is exported, the adjustment rate of heat addition is 5K/min, meanwhile, sample heat energy
The terminal voltage and heated current of examining system real-time monitoring heater are returned, the energy size of injection is calculated, temperature measurement system is with every
The continuous record standard temperature sensor of speed of 10 seconds points and the temperature value of operating temperature sensor.Dividing through temperature field
Analysis and calculating, obtain the mean temperature of shuttle at that time, then, calculate rate of temperature changes per 20 points.When sample heats energy
When measuring back examining system and detecting Implantation Energy and reach setting value, the output of heated current is closed, sample heat energy returns examining system
The data such as voltage, electric current and time are issued into computer by Ethernet.Shuttle enters the latter stage data acquisition in this stage.
Temperature measurement system continue collection standard temperature sensor and operating temperature sensor temperature value, through temperature field analysis and
Calculate, obtain the mean temperature of shuttle at that time, then, rate of temperature change is calculated per 20 points.When temperature variability less than 5 ×
10-4During K/min, system reaches balance, and now temperature value is latter stage temperature.The standard temperature of overall process is passed by temperature measurement system
Sensor, operating temperature sensor, the average temperature value of temperature field analysis calculating, rate of temperature change data etc. are issued by Ethernet
Computer.Latter stage temperature data is also the initial stage temperature data of next heating cycle.This process is until shuttle temperature repeatedly
Degree is increased to the upper limit of device experimental temperature, and space measurement process terminates.
4) measurement of full container state thermal capacitance：
Weigh standard substance sample α-Al2O3About 100 grams, it is added in shuttle 10, according to the measuring method of space amount
Determine the thermal capacity of full container.
3. data processing：
1) test the determination of temperature rise each heating cycle：
The temperature data least square fitting of each heating cycle, obtains experiment initial temperature T through heat leak amendmentiWith
Last temperature Tf, the experiment temperature rise Δ T of each heating phase shuttle is by following formula calculating：
Δ T=Tf-Ti
2) it is input into the calculating of electric energy：
Sample heat energy returns examining system with terminal voltage V and heated current I of the speed reading heater of 25 times per second.Often
The calculating of the energy Q that individual heating cycle is input into shuttle adopts following equation：
Wherein V, I, t are respectively voltage, electric current and heat time heating time.
3)α-Al2O3The calculating of molar heat capacity：
1., under each experimental temperature, space amount, the thermal capacitance of full container are calculated with following formula：
2. the space amount measured under each experimental temperature is carried out into fitting of a polynomial, full container experiment is calculated according to fitting formula
In space calorimetric capacitance corresponding at each temperature.
3. the space calorimetric that the thermal capacitance of full container is deducted under relevant temperature under each experimental temperature is held, and in view of material
Amount, obtains α-Al under each experimental temperature2O3Mean molal heat capacity.After carrying out every amendment and fitting of a polynomial, entirety can be calculated
At a temperature of, with 5K or 10K temperature as interval, α-Al2O3True molar heat capacity value.
4) uncertainty of measurement：
With U.S. NIST SRM720 standard substance α-Al2O3Measure under 300 to 550K experimental temperatures, obtain result such as
Under：
| T(K) | Cp(J·mol-1·K-1) | T(K) | Cp(J·mol-1·K-1) |
| 306.60 | 80.84 | 444.04 | 101.01 |
| 326.82 | 84.89 | 455.42 | 102.31 |
| 336.58 | 86.65 | 465.77 | 103.19 |
| 346.26 | 88.29 | 474.81 | 104.05 |
| 357.62 | 89.96 | 483.27 | 104.73 |
| 365.32 | 91.33 | 491.96 | 105.45 |
| 374.71 | 92.72 | 500.63 | 106.13 |
| 384.03 | 94.02 | 509.26 | 106.82 |
| 393.26 | 95.25 | 522.78 | 107.78 |
| 402.46 | 96.43 | 533.04 | 108.51 |
| 407.87 | 97.03 | 542.43 | 109.23 |
| 417.65 | 98.24 | 550.03 | 109.64 |
| 430.63 | 99.69 |
The uncertainty of specific heat of solid and heat measurement result is evaluated finally, it is contemplated that from determination sample specific heat capacity measurement result
The A class uncertainties of repeatability, and the B class uncertainties outside measurement result repeatability.With standard substance α-Al2O3
As a example by, its relative expanded uncertainty is about (0.1%-0.4%) (k=2).
Claims (8)
1. a kind of specific heat of solid and heat metrological standard unit, including shuttle (10), adiabatic tracks of device (20), inflating and exhausting system
(30) and Measurement and Control System (40), wherein, shuttle (10) is placed in adiabatic tracks of device (20), be it is characterized in that,
Shuttle (10) is made up of sample cell body (11), bottom of pond (12) He Chigai (13), and pond body (11) is matched somebody with somebody with bottom of pond (12)
Gap cooperation is combined into, Chi Gai (13) is also coordinated for gap with the cooperation of pond body (11)；It is disposed with least in the sample cell bottom
Two auxiliary lamellar ceramic heater (14), at least two main leaves shape ceramic heater (15) are symmetricly set in sample cell, and one
Individual standard temperature sensor (17) is arranged on sample cell center, and at least two operating temperature sensors (16) are arranged on main leaf shape pottery
Porcelain heater (15) is and pool wall between；
Adiabatic tracks of device (20) includes Dewar flask (21), tracking screen (22), heat screen (23) and housing from inside to outside successively
(24)；
The inflating and exhausting system (30) is for shuttle (10) and adiabatic tracks of device (20) inflation and aerofluxuss；
The Measurement and Control System (40) includes：For controlling the sample heating system (42) that shuttle (10) is heated；For
The sample heat energy of measurement injection sample energy size returns examining system (41)；For shuttle (10) temperature and adiabatic tracking
The temperature measurement system (43) of the temperature real-time measurement of device (20)；For the adiabatic tracking control that adiabatic tracks of device (20) is controlled
System (44) processed；And for the computer (45) of data acquisition and processing (DAP),
Wherein, in adiabatic tracks of device (20), the Dewar flask (21) is made up of bottle and bottle cap, and the bottle and bottle cap are equal
Be made up of high-temperature resistant double-layer quartz glass, double-deck inside quartz glass be vacuum and have silver coating, vacuum is 10-5~
10-6Pa, the bottom of bottle are provided with wire hole, and hole is embedded with ceramic insulating tube；
Tracking screen (22) is arranged on Dewar flask (21) outside, is made up of red copper, and the bottle by closure of openings and bottom of bottle group
Into being disposed with least two 250～400 ohm, 200 watts of flaky pottery heater (221) in bottom of bottle, and be disposed with work
Temperature sensor (222), and bottom of bottle is provided with wire hole, hole is embedded with ceramic insulating tube；
It is outside that the heat screen (23) is arranged on tracking screen (22), is made of stainless steel, and is multiple structure, bottom of bottle, body and bottle
Lid stud is fixed as entirety, and bottom of bottle is provided with wire hole, and hole is embedded with ceramic insulating tube；
It is outside that the housing (24) is arranged on heat screen (23), is made of stainless steel, is made up of housing and shell bottom, housing and shell bottom
Connected using vacuum sealing flange, shell bottom is provided with vacuum high-density connector, high-precision pressure sensor and fill exhaust port.
2. specific heat of solid and heat metrological standard unit according to claim 1, is characterized in that, the pond body (11), bottom of pond
(12) He Chigai (13) is made by fine silver；The pond body (11) is 70ml～100ml with the spatial volume that bottom of pond (12) is constituted；
The thickness of bottom of pond (12) is 8～14mm；The wall thickness of pond body (11) He Chigai (13) is 2～5mm；The sample cell for square or
Cylinder；Three 3 ohm, 3 watts of auxiliary lamellar ceramic heater (14) are disposed with the sample cell bottom, around sample cell
Bottom centre's distribution triangular in shape, and aid in lamellar ceramic heater (14) to be circle；Three 380 ohm, 200 watts of main leaf shape
Ceramic heater (15), around the distribution triangular in shape of sample cell center, and main leaf shape ceramic heater (15) is square；For institute
Auxiliary lamellar ceramic heater (14) is stated, and sample cell bottom is tightly mounted on by way of welding；For the main leaf shape is made pottery
Porcelain heater (15), is attached with the fine silver fin that maximum gauge is 4 millimeters on two surfaces；And standard temperature sensor (17)
For 25 ohm of standard temperature sensors；3 100 ohm of operating temperature sensors (16) are arranged on main leaf shape ceramic heater (15)
And pool wall between.
3. specific heat of solid and heat metrological standard unit according to claim 1 and 2, is characterized in that, the Dewar flask (21) is held
Product is 500～600 milliliters；Dewar flask (21) bottle and bottle cap wall thickness are 2～6 millimeters；
Described tracking screen (22) volume is 3～4 liters, and wall thickness is 3～6 millimeters；Tracking screen (22) is disposed with three or four in bottom of bottle
Individual 250～400 ohm, 200 watts of flaky pottery heater (221).
4. specific heat of solid and heat metrological standard unit according to claim 1 and 2, is characterized in that, the inflating and exhausting system
(30) it is to fill automatically emission control (30), this fills mechanical pump and molecular pump of the emission control (30) by integration automatically
(31), check valve (32), gas tank (33), accurate ratio adjusting valve (34), air relief valve (36), electromagnet cut off valve (35), indifferent gas
Bromhidrosis bottle (37) and automatic controller (38) composition, wherein, the mechanical pump and molecular pump (31) of integration are with check valve (32) even
Connect, check valve (32) is connected with gas tank (33), gas tank (33) is connected with accurate ratio adjusting valve (34), noble gases gas cylinder (37)
It is connected with air relief valve (36), air relief valve (36) is connected with accurate ratio adjusting valve (34), accurate ratio adjusting valve (34) and electromagnetism
Stop valve (35) connects, the mechanical pump and molecular pump (31) of automatic controller (38) control integration, check valve (32), accurate ratio
Example regulating valve (34), air relief valve (36), the startup of electromagnet cut off valve (35), regulation and closing.
5. specific heat of solid and heat metrological standard unit according to claim 1 and 2, is characterized in that, the sample heat energy
Examining system (41) is returned using Agilent circuit tester 3458A；The sample heating system (42) is using Keithley power supply 2425；It is described
Temperature measurement system (43) is using ASL bridge for measuring temperature F650；The adiabatic tracking control system (44) is automatic using ATCS-2000
Adiabatic controller.
6. specific heat of solid and heat metrological standard unit according to claim 4, is characterized in that, the shell of adiabatic tracks of device (20)
The fill exhaust port of body (24) is connected with the electromagnet cut off valve (35) for filling automatically emission control (30)；
Auxiliary lamellar ceramic heater (14) and main leaf shape ceramic heater (15) of shuttle (10) is by wire and housing
(24) vacuum high-density connector returns examining system (41) with sample heating system (42) and sample heat energy and is connected；It is adiabatic with
The flaky pottery heater (221) of track device (20) is by the vacuum high-density connector of wire and housing (24) and adiabatic tracking
Control system (44) connects；The operating temperature sensor (16) and standard temperature sensor (17) of shuttle (10) and thermal insulation
The operating temperature sensor (222) of tracks of device (20) is surveyed with temperature by the vacuum high-density connector of wire and housing (24)
Amount system (43) connects；Automatically the automatic controller (38) and computer (45) of emission control (30) are filled by ethernet line
Connection；Sample heating system (42), sample heat energy return examining system (41), adiabatic tracking control system (44) and temperature survey
System (43) is connected by ethernet line with computer (45).
7. a kind of method of measurement specific heat of solid and heat, is characterized in that, the method is using any one of claim 1 to 6
Specific heat of solid and heat metrological standard unit, the method include：Shuttle (10) and adiabatic tracks of device (20) are in indifferent gas bromhidrosis
The thermal capacitance of empty shuttle (10) under atmosphere, is determined, the thermal capacitance of the shuttle (10) for being loaded with testing sample is then determined, by following formula
Calculate the molar heat capacity of sample：
In formula：Quality (g) of the m for sample,
Molal weights (g/mol) of the M for sample,
ce、cfRespectively empty shuttle, be loaded with testing sample shuttle mean heat capacity (J/K), cm(T) it is sample
Mean molal heat capacity (J/molK).
8. the method for measurement specific heat of solid and heat according to claim 7, is characterized in that, the noble gases are argon.
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| CN107677480A (en) * | 2017-11-14 | 2018-02-09 | 吉林大学 | A kind of temperature can active control constant volume bullet heat-insulation system and its control method |
| CN107884437B (en) * | 2017-12-13 | 2023-10-27 | 中国科学院大连化学物理研究所 | Calorimeter sample cell convenient to replace and good in sealing performance |
| CN109142630B (en) * | 2018-08-08 | 2021-03-23 | 山东中烟工业有限责任公司 | Device and method for setting feed liquid solid proportion and boiling strength |
| CN109540968B (en) * | 2018-11-22 | 2020-12-29 | 重庆大学 | Method for quantitatively detecting three-dimensional defects in equipment |
| CN113820357B (en) * | 2021-11-22 | 2022-08-19 | 国家电投集团氢能科技发展有限公司 | Material thermodynamic parameter measuring equipment and measuring method |
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