CN103713006A - Solid-solid phase transition rate measurement device and method for solid material - Google Patents
Solid-solid phase transition rate measurement device and method for solid material Download PDFInfo
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- CN103713006A CN103713006A CN201310754160.0A CN201310754160A CN103713006A CN 103713006 A CN103713006 A CN 103713006A CN 201310754160 A CN201310754160 A CN 201310754160A CN 103713006 A CN103713006 A CN 103713006A
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- 238000005259 measurement Methods 0.000 title claims abstract description 28
- 230000007704 transition Effects 0.000 title claims abstract description 26
- 238000000034 method Methods 0.000 title claims abstract description 20
- 239000007790 solid phase Substances 0.000 title abstract description 8
- 239000011343 solid material Substances 0.000 title abstract 2
- 238000010438 heat treatment Methods 0.000 claims abstract description 78
- 230000007246 mechanism Effects 0.000 claims abstract description 38
- 238000001931 thermography Methods 0.000 claims abstract description 31
- 239000011521 glass Substances 0.000 claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 48
- 238000012545 processing Methods 0.000 claims description 38
- 230000009466 transformation Effects 0.000 claims description 26
- 230000004304 visual acuity Effects 0.000 claims description 23
- 239000000463 material Substances 0.000 claims description 18
- 239000000758 substrate Substances 0.000 claims description 15
- 239000000498 cooling water Substances 0.000 claims description 14
- 239000007787 solid Substances 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 8
- 238000003908 quality control method Methods 0.000 claims description 4
- 238000003860 storage Methods 0.000 claims description 4
- 238000004364 calculation method Methods 0.000 claims description 3
- 238000005070 sampling Methods 0.000 claims description 3
- 238000000691 measurement method Methods 0.000 claims description 2
- 239000012071 phase Substances 0.000 abstract description 49
- 230000008569 process Effects 0.000 abstract description 8
- 230000008859 change Effects 0.000 abstract description 4
- 238000004458 analytical method Methods 0.000 abstract description 2
- 239000007789 gas Substances 0.000 description 33
- 239000005304 optical glass Substances 0.000 description 4
- 239000012782 phase change material Substances 0.000 description 4
- 238000002791 soaking Methods 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 239000000654 additive Substances 0.000 description 1
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- 238000004146 energy storage Methods 0.000 description 1
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- 230000014759 maintenance of location Effects 0.000 description 1
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- 230000000750 progressive effect Effects 0.000 description 1
- 239000012495 reaction gas Substances 0.000 description 1
- 239000011232 storage material Substances 0.000 description 1
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Abstract
The invention discloses a solid-solid phase transition rate measurement device and method for a solid material, which can measure weak phase transition rate under a small quantity of weak reactions and perform measurement and analysis on fast phase transition rate. The solid-solid phase transition rate measurement device disclosed by the invention comprises a vacuum heating chamber, wherein the vacuum heating chamber is connected with a gas source device, a sample heating table is arranged in the vacuum heating chamber, the sample heating table is connected with a heating temperature control mechanism, a glass window for enabling an infrared thermal imaging instrument to measure is formed at the top of the vacuum heating chamber, and the high-resolution and high-speed infrared thermal imaging instrument is arranged outside the glass window. By using the solid-solid phase transition rate measurement device and method disclosed by the invention, the change in phase transition rate in the whole transition process can be measured, and the real-time observation of the phase transition process can be realized.
Description
Technical field
The present invention relates to the measurement of phase-change material, be specifically related to adopt high resolving power high speed infrared thermal imaging system 122 to measure the method for solid-solid phase-change, transformation rate, realize the real-time monitored of phase transition process.
Background technology
Material is called phase transformation from a kind of process that changes mutually another kind of phase into.In recent years, phase-change material becomes study hotspot in the application in energy storage field, but the measurement of the transformation rate of phase-change material does not also have country and international standard.Transformation rate is the important motivity mathematic(al) parameter of phase-change material, so it measures important in inhibiting, especially to the speed of stored energy and release, has in the situation of requirement even more important.For solid-solid phase transition material, general method of testing has: laser ultrasonic mensuration, gas volume mensuration.
The measurement mechanism that Jap.P. JPA2010223635 provides, adopts laser ultrasonic mensuration, laser ultrasonic mensuration easy damaged sample, make test result produce larger error, device structure is complicated, and it is large that technology realizes difficulty, measurement result is easily affected by environment, is difficult for realizing Measurement accuracy.
Document: the hydrogen storage material transformation rate measurement mechanism described in China YouSe Acta Metallurgica Sinica 2003 (13) 3:695-698, adopt hydrogen volume mensuration, but it is mostly that such device obtains is results under initial and final two states, observation for real-time monitored and intermediate reaction rate variation is difficult for, and can produce larger error for the few sample of sucking/placing hydrogen amount.
Summary of the invention
For above-mentioned defect or Improvement requirement, the present invention proposes a kind of transformation rate measurement mechanism and measuring method of carrying solid-solid phase transition material, not only can measure the faint transformation rate under a small amount of weak reaction, also can carry out Measurement and analysis to the speed of rapid phase transition.
For achieving the above object, the invention provides a kind of solid-solid phase-change speed measurement device of solid-state material, its technical scheme is as follows:
A solid-solid phase-change speed measurement device for solid-state material, comprises vacuum heating chamber, and required vacuum environment is heated in vacuum heating chamber sampling, and the place of sample and gas reaction; Vacuum heating chamber is connected with compressed air source unit, vacuum heating chamber is provided with air admission hole, compressed air source unit connects air admission hole through gas flow control mechanism, vacuum heating chamber is provided with vacuum interface and water power interface, the indoor sample warm table that is provided with of heating in vacuum, is provided with well heater in sample warm table, and the well heater in sample warm table connects heated for controlling temperature mechanism, heated for controlling temperature mechanism is used for the heating-up temperature of Quality control, and the temperature of sample warm table is transferred to computer processing module storage;
Vacuum heating chamber top is provided with the optical glass window for infrared heat image instrument measuring, it is positive that glass window is positioned at sample warm table, glass window outside is provided with high resolving power high speed infrared thermal imaging system, and high resolving power high speed infrared thermal imaging system is taken the infrared thermal imaging figure of sample for continuous high speed;
High resolving power high speed infrared thermal imaging system is perpendicular to sample warm table the place ahead, and high resolving power high speed infrared thermal imaging system connects computer processing module; Computer processing module is for showing the thermal-induced imagery with processing sample, and stores processor result.
Further, in certain embodiments, described vacuum heating chamber is Double water-cooled structure, in the locular wall of vacuum heating chamber, is provided with circulating water pipe, vacuum heating chamber locular wall is provided with recirculated water entrance and circulating water outlet, and circulating water pipe two ends connect respectively recirculated water entrance in circulating water outlet.
Further, in certain embodiments, described sample warm table bottom and side are provided with cooling water pipe, and the cooling water pipe of sample warm table bottom and side connects external cooling water pipe through water power interface.
Further, in certain embodiments, the well heater in described sample warm table connects heated for controlling temperature mechanism through water power interface by thermopair.
Further, in certain embodiments, the well heater in described sample warm table is provided with sample, and sample is comprised of substrate and wedge shape film, substrate surface is provided with the wedge shape film that section is right-angle triangle, and after phase transformation, the surfacing of wedge shape film sample is changed to inversion of phases layer;
Further, in certain embodiments, described computer processing module connects gas flow control mechanism and heated for controlling temperature mechanism, and computer processing module is controlled the duty of gas flow control mechanism and heated for controlling temperature mechanism.
For achieving the above object, provide a kind of solid-solid phase-change speed measurement method of solid-state material, comprised the following steps:
1-1, first vacuum heating chamber is connected with outside vacuum unit by vacuum interface, sample is placed on sample warm table, and closes the chamber door of vacuum heating chamber;
1-2, start to vacuumize, the indoor pressure of heating in vacuum reaches 10
-3during Pa, to the logical cooling circulating water of circulating water pipe in the locular wall of vacuum heating chamber, at computer processing module, set and need the temperature of heating and start heating;
1-3, etc. be heated to setting temperature and stable after (establishing now sample is A phase), open high resolving power high speed infrared thermal imaging system take pictures (interval 1～3s takes pictures); Gu in the situation that simple dependence temperature realizes admittedly-changes, measuring method skips steps 1-4～1-6, forwards step 1-7 to;
1-4, then by computer processing module setting, need pass into the amount of the reacting gas of vacuum heating chamber, and open compressed air source unit and start timing, gas carry gas through gas flow control mechanism to vacuum heating chamber, gas starts to react with sample surfaces, surfacing undergoes phase transition (establish and be converted into B phase), the bright-dark degree of thermograph changes, and machine processing module shows as calculated;
After 1-5, reaction finish, stop timing, close compressed air source unit, stop heating the chilled water to the logical external cooling water pipe of sample warm table, sample is cooling, and the gas in sample is overflowed, B changes A phase mutually into, and the bright-dark degree of thermograph changes, and machine processing module shows as calculated;
After 1-6, variation stop, stopping vacuum unit, take out sample;
1-7, by the A of computer processing module calculation sample, changed mutually into the transformation rate of B phase, and B changes the transformation rate of A phase mutually into, complete measurement.
In general, the above technical scheme of conceiving by the present invention compared with prior art, can obtain following effect: device of the present invention adopts the ingenious combination wedge shape of high resolving power high speed infrared thermal imaging system membrane structure to measure the method for transformation rate, can measure the variation of the transformation rate in whole transition process, and realize the real-time monitored of phase transition process simultaneously.
Accompanying drawing explanation
Fig. 1 is the structural representation of the embodiment of the present invention;
Fig. 2 a is initial t
0the thermal imaging schematic diagram of time;
Fig. 2 b is the thermal imaging schematic diagram in phase transition process.
Reference numeral is as follows:
Embodiment
Below with reference to drawings and Examples, the present invention is described in further detail.
The transformation rate measurement mechanism of solid-solid phase transition material of the present invention is mainly comprised of high resolving power high speed infrared thermal imaging system 122, computer processing module 123, heated for controlling temperature mechanism 124, vacuum heating chamber 100, gas flow control mechanism 102, compressed air source unit 101 etc.
The present invention includes vacuum heating chamber 100, vacuum heating chamber 100 is connected with compressed air source unit 101, vacuum heating chamber 100 is Double water-cooled structure, in the locular wall of vacuum heating chamber 100, be provided with circulating water pipe 108, vacuum heating chamber 100 is provided with recirculated water entrance 103 and circulating water outlet 104, water enters spiral fashion circulating water pipe 108 by recirculated water entrance 103, after circulation, from circulating water outlet 104, discharge, vacuum heating chamber 100 is provided with air admission hole 107, compressed air source unit 101 connects air admission hole 107 through gas flow control mechanism 102, by air admission hole 107, inject the reacting gas (H of 1～5Bar air pressure to vacuum heating chamber 100
2,o
2, N
2deng), vacuum heating chamber 100 is provided with vacuum interface 105 and water power interface 106, vacuum heating chamber 100 vacuumizes by vacuum interface 105, in vacuum heating chamber 100, be provided with sample warm table 120, sample warm table 120 bottoms and side are provided with cooling water pipe, the cooling water pipe of sample warm table 120 bottoms and side connects external cooling water pipe 109 through water power interface 106, in sample warm table 120, be provided with soaking plate, soaking plate in sample warm table 120 connects heated for controlling temperature mechanism 124 through water power interface 106 by thermopair, soaking plate in sample warm table 120 is provided with sample, sample is comprised of substrate 201 and wedge shape film 202, substrate 201 is provided with the wedge shape film 202 that section is right-angle triangle, the surfacing of sample after phase transformation (wedge shape film 202 and substrate 201) is changed to inversion of phases layer 203.
Sample is comprised of wedge shape film 202 and substrate 201, and substrate 201 length are L, and original wedge shape film 202 sections are right-angle triangle, and wedge shape film 202 base length are L, and wedge shape film 202 is highly h, and inversion of phases layer 203 thickness are h
1.
Principle of work: the present invention is limited to the transformation rate of solid-solid phase change material and measures, measures admittedly can realize two kinds of transformation rates in solid-transformation situation.The one, the phase transition rate that passes into the cenotype producing under reacting gas while heating state is measured; The 2nd, the measurement in the phase transformation situation producing by temperature variation merely.In two kinds of situations, all need first vacuum heating chamber 100 to be connected with outside vacuum unit by vacuum interface 105, sample (wedge shape film 202 and substrate 201) is placed on sample warm table 120; First vacuum heating chamber 100 is vacuumized, then 124 pairs of samples of heated for controlling temperature mechanism (wedge shape film 202 and substrate 201) heat, Deng the temperature and stable rear (establishing now sample is A phase) that are heated to setting, opens high resolving power high speed infrared thermal imaging system 122 and take pictures continuously.Principle of work in two kinds of situations of division below:
One, the phase transition rate that passes into the cenotype producing under reacting gas while heating state is measured.In aforementioned common step, complete under condition, vacuum heating chamber 100 passed into the reacting gas of certain air pressure, by gas flow control mechanism 102(, regulate vacuum valve) open and maintain air pressure balance.Reacting gas can react with the surface of sample (wedge shape film 202 and substrate 201) at a certain temperature, because reacting the surfacing of rear sample, undergo phase transition (establish and be converted into B phase), because the infrared characteristic of out of phase material is different, therefore the captured figure sector-meeting of high resolving power high speed infrared thermal imaging system 122 is along with the light and shade that presents of reaction changes, and the thermography of sample changes schematic diagram as shown in accompanying drawing 2a, accompanying drawing 2b.When the picture comparison of light and shade of high resolving power high speed infrared thermal imaging system 122 no longer changes, the phase transition process of interpret sample completes.By the length L having changed during time t after changing
1, the total length L of sample, the thickness h in wedge shape film 202 thickness, by similar triangles property theorem, the A that can calculate sample changes the inversion of phases layer 203(phase interface place of B phase mutually into) thickness h
1 
and then calculate transformation rate v=h
1/ t.
Then stop air feed, the logical cold moving water of sample warm table 120 is carried out cooling, vacuumize simultaneously, the gas in sample is overflowed, and B changes A phase mutually into, in the same way, can calculate the transformation rate that sample B changes A phase mutually into.
Two, the measurement in the phase transformation situation producing by temperature variation merely.In such cases, phase transformation starts to change at phase transition temperature point, utilize the infrared characteristic difference of out of phase material to obtain the infrared figure that a series of light and shades change, and then the utilization processing means the same with afore-mentioned can obtain phase transition rate.
As shown in accompanying drawing 2a, accompanying drawing 2b, thickness of sample h is nm level or μ m level, and from a side to opposite side progressive additive, its method for making can referenced patent ZL201120123187.6.
Main device effect of the present invention:
High resolving power high speed infrared thermal imaging system 122, for the infrared thermal imaging figure of continuous high speed shooting sample;
Heated for controlling temperature mechanism 124, for the heating-up temperature of Quality control, and is transferred to computer processing module 123 storages by the temperature of sample warm table 120;
The top of sample warm table 120 is one can place the soaking plate of sample, and bottom and side are water-cooling structure, and chilled water is connected with external water source with external cooling water pipe 109 by water power interface 106;
Gas flow control mechanism 102 is connected with compressed air source unit 101 and computer processing module 123, controls the speed that gas enters vacuum heating chamber 100, thus Quality control at a certain temperature with the speed of gas reaction;
Compressed air source unit 101, storage reaction gas.
Measuring method of the present invention is as follows:
1-1, first vacuum heating chamber 100 is connected with outside vacuum unit by vacuum interface 105, sample is placed on sample warm table 120, and closes the chamber door of vacuum heating chamber 100;
1-2, start to vacuumize, the interior pressure of vacuum heating chamber 100 reaches 10
-3during Pa, to the logical chilled water of circulating water pipe in the locular wall of vacuum heating chamber 100 108, start cooling circulating water, at computer processing module 123, set and need the temperature of heating and start heating;
1-3, etc. be heated to setting temperature and stable after (establishing now sample is A phase), open high resolving power high speed infrared thermal imaging system 122 take pictures (interval 1～3s takes pictures); Gu in the situation that simple dependence temperature realizes admittedly-changes, measuring method skips steps 1-4～1-6, forwards step 1-7 to;
1-4, then the amount of the reacting gas that need pass into vacuum heating chamber 100 is set by computer processing module 123, and open compressed air source unit 101 and start timing, gas carry gas through gas flow control mechanism 102 to vacuum heating chamber 100, gas starts to react with sample surfaces, surfacing undergoes phase transition (establish and be converted into B phase), the bright-dark degree of thermograph changes, and machine processing module 123 shows as calculated;
After 1-5, reaction finish, stop timing, close compressed air source unit 101, stop heating the chilled water to sample warm table 120 logical external cooling water pipes 109, sample is cooling, and the gas in sample is overflowed, and B changes A phase mutually into, the bright-dark degree of thermograph changes, and machine processing module 123 shows as calculated;
After 1-6, variation stop, stopping vacuum unit, take out sample;
1-7, by the A of computer processing module 123 calculation samples, changed mutually into the transformation rate of B phase, and B changes the transformation rate of A phase mutually into, complete measurement.
The above embodiment has only expressed part embodiment of the present invention, and it describes comparatively concrete and detailed, but can not therefore be interpreted as limitation of the scope of the invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with claims.
Claims (7)
1. a solid-solid phase-change speed measurement device for solid-state material, comprises vacuum heating chamber (100), and required vacuum environment is heated in described vacuum heating chamber (100) sampling, and the place of sample and gas reaction, described vacuum heating chamber (100) is connected with compressed air source unit (101), it is characterized in that, described vacuum heating chamber (100) is provided with air admission hole (107), described compressed air source unit (101) connects air admission hole (107) through gas flow control mechanism (102), described vacuum heating chamber (100) is provided with vacuum interface (105) and water power interface (106), in described vacuum heating chamber (100), be provided with sample warm table (120), in described sample warm table (120), be provided with well heater, well heater in described sample warm table (120) connects heated for controlling temperature mechanism (124), described heated for controlling temperature mechanism (124) is for the heating-up temperature of Quality control, and the temperature of sample warm table (120) is transferred to computer processing module (123) storage,
Described vacuum heating chamber (100) top is provided with the glass window (121) for infrared heat image instrument measuring, described glass window (121) is positioned at sample warm table (120) front, described glass window (121) outside is provided with high resolving power high speed infrared thermal imaging system (122), and described high resolving power high speed infrared thermal imaging system (122) is taken the infrared thermal imaging figure of sample for continuous high speed;
Described high resolving power high speed infrared thermal imaging system (122) is perpendicular to sample warm table (120) the place ahead, and described high resolving power high speed infrared thermal imaging system (122) connects computer processing module (123); Described computer processing module (123) is for showing the thermal-induced imagery with processing sample, and stores processor result.
2. the solid-solid phase-change speed measurement device of a kind of solid-state material according to claim 1, it is characterized in that, described vacuum heating chamber (100) is Double water-cooled structure, in the locular wall of described vacuum heating chamber (100), be provided with circulating water pipe (108), described vacuum heating chamber (100) locular wall is provided with recirculated water entrance (103) and circulating water outlet (104), and described circulating water pipe (108) two ends connect respectively recirculated water entrance (103) in circulating water outlet (104).
3. the solid-solid phase-change speed measurement device of a kind of solid-state material according to claim 1, it is characterized in that, described sample warm table (120) bottom and side are provided with cooling water pipe, and the cooling water pipe of described sample warm table (120) bottom and side connects external cooling water pipe (109) through water power interface (106).
4. the solid-solid phase-change speed measurement device of a kind of solid-state material according to claim 1, is characterized in that, the well heater in described sample warm table (120) connects heated for controlling temperature mechanism (124) through water power interface (106) by thermopair.
5. the solid-solid phase-change speed measurement device of a kind of solid-state material according to claim 1, it is characterized in that, well heater in described sample warm table (120) is provided with sample, described sample is comprised of substrate (201) and wedge shape film (202), described substrate (201) surface is provided with the wedge shape film (202) that section is right-angle triangle, and after phase transformation, the surfacing of wedge shape film (202) sample is changed to inversion of phases layer (203).
6. the solid-solid phase-change speed measurement device of a kind of solid-state material according to claim 1, it is characterized in that, described computer processing module (123) connects gas flow control mechanism (102) and heated for controlling temperature mechanism (124), and described computer processing module (123) is controlled the duty of gas flow control mechanism (102) and heated for controlling temperature mechanism (124).
7. a solid-solid phase-change speed measurement method for solid-state material, is characterized in that, comprises the following steps:
1-1, first vacuum heating chamber is connected with outside vacuum unit by vacuum interface, sample is placed on sample warm table, and closes the chamber door of vacuum heating chamber;
1-2, start to vacuumize, the indoor pressure of heating in vacuum reaches 10
-3during Pa, to the logical cooling circulating water of circulating water pipe in the locular wall of vacuum heating chamber, at computer processing module, set and need the temperature of heating and start heating;
1-3, etc. be heated to setting temperature and stable after, establishing now sample is A phase; Open high resolving power high speed infrared thermal imaging system and take pictures, interval 1～3s takes pictures; Gu in the situation that simple dependence temperature realizes admittedly-changes, measuring method skips steps 1-4～1-6, forwards step 1-7 to;
1-4, then by computer processing module setting, need pass into the amount of the reacting gas of vacuum heating chamber, and open compressed air source unit and start timing, gas carry gas through gas flow control mechanism to vacuum heating chamber, gas starts to react with sample surfaces, surfacing undergoes phase transition, if be converted into B phase, the bright-dark degree of thermograph changes, and machine processing module shows as calculated;
After 1-5, reaction finish, stop timing, close compressed air source unit, stop heating the chilled water to the logical external cooling water pipe of sample warm table, sample is cooling, and the gas in sample is overflowed, B changes A phase mutually into, and the bright-dark degree of thermograph changes, and machine processing module shows as calculated;
After 1-6, variation stop, stopping vacuum unit, take out sample;
1-7, by the A of computer processing module calculation sample, changed mutually into the transformation rate of B phase, and B changes the transformation rate of A phase mutually into, complete measurement.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108195875A (en) * | 2017-12-12 | 2018-06-22 | 中国科学院过程工程研究所 | A kind of rapid automatized system and its assay method for measuring phase-change material cold cycling of width warm area |
| WO2018154294A1 (en) * | 2017-02-21 | 2018-08-30 | The University Of Liverpool | Gas sorption screening |
| CN109298010A (en) * | 2017-07-25 | 2019-02-01 | 中国石油化工股份有限公司 | A kind of system detecting core high-temperature fusion feature |
| CN109738321A (en) * | 2019-01-23 | 2019-05-10 | 重庆理工大学 | The quick thermal fatigue test device and method of mechanical reciprocating |
| CN113552516A (en) * | 2021-06-30 | 2021-10-26 | 广东工业大学 | Test device for researching phase change process |
| CN113552516B (en) * | 2021-06-30 | 2024-04-26 | 广东工业大学 | Test device for researching phase change process |
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| WO2018154294A1 (en) * | 2017-02-21 | 2018-08-30 | The University Of Liverpool | Gas sorption screening |
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| CN109738321A (en) * | 2019-01-23 | 2019-05-10 | 重庆理工大学 | The quick thermal fatigue test device and method of mechanical reciprocating |
| CN113552516A (en) * | 2021-06-30 | 2021-10-26 | 广东工业大学 | Test device for researching phase change process |
| CN113552516B (en) * | 2021-06-30 | 2024-04-26 | 广东工业大学 | Test device for researching phase change process |
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| CN103713006B (en) | 2016-01-20 |
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