CN103713006B - A kind of solid-solid phase-change rate measurement device of solid-state material and method - Google Patents

A kind of solid-solid phase-change rate measurement device of solid-state material and method Download PDF

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CN103713006B
CN103713006B CN201310754160.0A CN201310754160A CN103713006B CN 103713006 B CN103713006 B CN 103713006B CN 201310754160 A CN201310754160 A CN 201310754160A CN 103713006 B CN103713006 B CN 103713006B
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phase
heating chamber
vacuum heating
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CN103713006A (en
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谭卓鹏
周济
沈剑山
邓金雁
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CAMDA NEW ENERGY EQUIPMENT Co Ltd
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Abstract

The invention discloses a kind of solid-solid phase-change rate measurement device and method of solid-state material, the faint transformation rate under a small amount of weak reaction can be measured, also can carry out Measurement and analysis to the speed of rapid phase transition.The present invention includes vacuum heating chamber, vacuum heating chamber is connected with compressed air source unit, heating in vacuum indoor are provided with sample warm table, sample warm table connects heated for controlling temperature mechanism, vacuum heating chamber top is provided with the glass window for infrared heat image instrument measuring, is provided with high resolving power high speed infrared thermal imaging system outside glass window.The present invention can measure the change of the transformation rate in whole transition process, and realizes the real-time monitored of phase in version process.

Description

A kind of solid-solid phase-change rate measurement device of solid-state material and method
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 in version process.
Background technology
The process that material is another kind of phase from a kind of phase in version is called phase transformation.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, and therefore it measures important in inhibiting, even more important when especially having a requirement to the speed of stored energy and release.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 comparatively big error, device structure is complicated, and it is large that technology realizes difficulty, measurement result is easily affected by environment, not easily realizes 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 such device obtain are mostly results under initial and final two states, for real-time monitored and intermediate reaction rate variation observation not easily, and comparatively big error can be produced for the sample that sucking/placing hydrogen amount is few.
Summary of the invention
For above-mentioned defect or Improvement requirement, the present invention proposes a kind of transformation rate measurement mechanism and the 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 rate measurement device of solid-state material, its technical scheme is as follows:
A solid-solid phase-change rate measurement device for solid-state material, comprises vacuum heating chamber, the vacuum environment needed for vacuum heating chamber sampling heating, 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, heating in vacuum indoor are provided with sample warm table, are 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, glass window is positioned at sample warm table front, be provided with high resolving power high speed infrared thermal imaging system outside glass window, high resolving power high speed infrared thermal imaging system is used for the infrared thermal imaging figure of continuous high speed shooting sample;
High resolving power high speed infrared thermal imaging system is perpendicular to sample warm table front, 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, is provided with circulating water pipe in the locular wall of vacuum heating chamber, vacuum heating chamber locular wall is provided with recirculated water entrance and circulating water outlet, and circulating water pipe two ends connect recirculated water entrance respectively in circulating water outlet.
Further, in certain embodiments, bottom described sample warm table and side is provided with cooling water pipe, bottom sample warm table and the cooling water pipe of side connect 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 made up of substrate and tapered film, substrate surface is provided with the tapered film that section is right-angle triangle, and after phase transformation, the surfacing of tapered 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 controls 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, comprise the following steps:
1-1, first vacuum heating chamber to be connected with outside vacuum pump set by vacuum interface, sample to be placed on sample warm table, and to close the room door of vacuum heating chamber;
1-2, start to vacuumize, the indoor pressure of heating in vacuum reaches 10 -3during Pa, the locular wall Inner eycle water pipe to vacuum heating chamber leads to cooling circulating water, sets the temperature that need heat and start heating at computer processing module;
1-3, etc. be heated to the temperature that sets and stable after (set now sample as A phase), open high resolving power high speed infrared thermal imaging system and carry out taking pictures (take pictures interval 1 ~ 3s); Gu when simple dependence temperature realizes admittedly-changes, measuring method skips step 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 is set by computer processing module, and open compressed air source unit and start timing, namely 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 terminate, stop timing, close compressed air source unit, stopping is heated and sample warm table is led to the chilled water of external cooling water pipe, and sample cools, the gas effusion in sample, B phase in version is A phase, and the bright-dark degree of thermograph changes, and machine processing module shows as calculated;
After 1-6, change stop, stopping vacuum pump set, take out sample;
1-7, be the transformation rate of B phase by the A phase in version of computer processing module calculation sample, and B phase in version is the transformation rate of A phase, completes measurement.
In general, the above technical scheme conceived by the present invention compared with prior art, following effect can be obtained: device of the present invention adopts the ingenious method in conjunction with tapered film structure measurement transformation rate of high resolving power high speed infrared thermal imaging system, the change of the transformation rate in whole transition process can be measured simultaneously, and realize the real-time monitored of phase in version process.
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:
Vacuum heating chamber 100, compressed air source unit 101, gas flow control mechanism 102, recirculated water entrance 103, circulating water outlet 104, vacuum interface 105, water power interface 106, air admission hole 107, circulating water pipe 108, external cooling water pipe 109, sample warm table 120, glass window 121, high resolving power high speed infrared thermal imaging system 122, computer processing module 123, heated for controlling temperature mechanism 124, substrate 201, tapered film 202, inversion of phases layer 203.
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 primarily of compositions such as 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 units 101.
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, circulating water pipe 108 is provided with in the locular wall of vacuum heating chamber 100, 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, discharge from circulating water outlet 104 after circulation, 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, inject the reacting gas (H of 1 ~ 5Bar air pressure to vacuum heating chamber 100 by air admission hole 107 2,o 2, N 2deng), vacuum heating chamber 100 is provided with vacuum interface 105 and water power interface 106, vacuum heating chamber 100 is vacuumized by vacuum interface 105, sample warm table 120 is provided with in vacuum heating chamber 100, bottom sample warm table 120 and side is provided with cooling water pipe, bottom sample warm table 120 and the cooling water pipe of side connect external cooling water pipe 109 through water power interface 106, soaking plate is provided with in sample warm table 120, 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 made up of substrate 201 and tapered film 202, substrate 201 is provided with the tapered film 202 that section is right-angle triangle, after phase transformation, the surfacing of sample (tapered film 202 and substrate 201) is changed to inversion of phases layer 203.
Vacuum heating chamber 100 top is provided with glass window 121, and glass window 121 adopts optical glass, is optical glass window.Glass window 121 is positioned at sample warm table 120 front, high resolving power high speed infrared thermal imaging system 122 is provided with outside glass window 121, high resolving power high speed infrared thermal imaging system 122 is perpendicular to sample warm table 120 front, high resolving power high speed infrared thermal imaging system 122 connects computer processing module 123, and the data of high resolving power high speed infrared thermal imaging system 122 are imported computer processing module 123 into and processed.
Computer processing module 123 connects gas flow control mechanism 102 and heated for controlling temperature mechanism 124, and computer processing module 123 controls the duty of gas flow control mechanism 102 and heated for controlling temperature mechanism 124.
Sample is made up of tapered film 202 and substrate 201, and substrate 201 length is L, and original tapered film 202 section is right-angle triangle, and tapered film 202 base length is L, and tapered film 202 is highly h, and inversion of phases layer 203 thickness is h 1.
Principle of work: the transformation rate that the present invention is limited to solid-solid phase change material is measured, admittedly the transformation rate that can realize in two kinds of solid-transformation situations is measured.One is that the phase transition rate passing into the cenotype that reacting gas produces under heating state is simultaneously measured; Two is the measurements in the phase transformation situation produced by temperature variation merely.All need in two kinds of situations first vacuum heating chamber 100 to be connected with outside vacuum pump set by vacuum interface 105, sample (tapered film 202 and substrate 201) is placed on sample warm table 120; First vacuum heating chamber 100 is vacuumized, then heated for controlling temperature mechanism 124 pairs of samples (tapered film 202 and substrate 201) heat, etc. be heated to the temperature that sets and stable after (set now sample as A phase), open high resolving power high speed infrared thermal imaging system 122 and take pictures continuously.Principle of work below in division two kinds of situations:
One, the phase transition rate passing into the cenotype that reacting gas produces under heating state is simultaneously measured.Under aforementioned common step completes condition, vacuum heating chamber 100 is passed into the reacting gas of certain air pressure, regulates vacuum valve by gas flow control mechanism 102() open maintenance air pressure balance.Reacting gas can react with the surface of sample (tapered film 202 and substrate 201) at a certain temperature, because the surfacing reacting rear sample undergoes phase transition (establish and be converted into B phase), because the infrared characteristic of out of phase material is different, therefore the figure sector-meeting captured by high resolving power high speed infrared thermal imaging system 122 changes along with the carrying out reacted presents light and shade, and the thermography change schematic diagram of sample is 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 changed during time t after changing 1, the total length L of sample, the thickness h in tapered film 202 thickness, by similar triangles property theorem, the A phase in version that can calculate sample is the inversion of phases layer 203(phase interface place of B phase) thickness h 1 and then calculate transformation rate v=h 1/ t.
Then stop air feed, lead to cold dynamic water and cool, vacuumize simultaneously sample warm table 120, the gas effusion in sample, B phase in version is A phase, in the same way, can calculate the transformation rate that sample B phase in version is A phase.
Two, the measurement in the phase transformation situation produced by temperature variation merely.In such cases, phase transformation starts to change at phase transition temperature point, utilizes the infrared characteristic of out of phase material difference to obtain the infrared figure of a series of light and shade change, and then utilizes the process means the same with afore-mentioned to obtain phase transition rate.
As shown in accompanying drawing 2a, accompanying drawing 2b, thickness of sample h is nm level or μm level, and from 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;
Computer processing module 123, for showing the thermal-induced imagery with processing sample, and stores processor result;
Heated for controlling temperature mechanism 124, for the heating-up temperature of Quality control, and is transferred to computer processing module 123 by the temperature of sample warm table 120 and stores;
The top of sample warm table 120 is a soaking plate can placing 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;
Vacuum heating chamber 100, the vacuum environment needed for sampling heating, and the place of sample and gas reaction;
Vacuum heating chamber 100 is Double water-cooled structure, and vacuum heating chamber 100 locular wall is provided with recirculated water entrance 103, circulating water outlet 104, can effectively prevent locular wall overheated;
Vacuum heating chamber 100 top is provided with the optical glass window 121 for infrared heat image instrument measuring;
Vacuum heating chamber 100 locular wall is provided with vacuum interface 105, can be connected fast with vacuum pump set;
Gas flow control mechanism 102 is connected with compressed air source unit 101 and computer processing module 123, controls gas and enters the speed of 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.
Substrate 201 length is L, and original tapered film 202 section is right-angle triangle, and tapered film 202 base length is L, and tapered film 202 is highly h, the length L changed during time t after changing 1(inversion of phases layer 203 length), inversion of phases layer 203 thickness is h 1.Shown in accompanying drawing 2b, X is film and the inversion of phases layer separatrix on substrate 201 surface, and X boundary line place is to the length L of end 1for inversion of phases layer 203 length, the length changed when it is time t after changing.
Measuring method of the present invention is as follows:
1-1, first vacuum heating chamber 100 to be connected by the vacuum pump set of vacuum interface 105 with outside, sample to be placed on sample warm table 120, and to close the room door of vacuum heating chamber 100;
1-2, start to vacuumize, in vacuum heating chamber 100, pressure reaches 10 -3during Pa, the locular wall Inner eycle water pipe 108 to vacuum heating chamber 100 leads to chilled water, starts cooling circulating water, sets the temperature that need heat and start heating at computer processing module 123;
1-3, etc. be heated to the temperature that sets and stable after (set now sample as A phase), open high resolving power high speed infrared thermal imaging system 122 and carry out taking pictures (take pictures interval 1 ~ 3s); Gu when simple dependence temperature realizes admittedly-changes, measuring method skips step 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, namely 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 terminate, stop timing, close compressed air source unit 101, stopping is heated and sample warm table 120 is led to the chilled water of external cooling water pipe 109, sample cools, the gas effusion in sample, and B phase in version is A phase, the bright-dark degree of thermograph changes, and machine processing module 123 shows as calculated;
After 1-6, change stop, stopping vacuum pump set, take out sample;
1-7, be the transformation rate of B phase by the A phase in version of computer processing module 123 calculation sample, and B phase in version is the transformation rate of A phase, completes measurement.
The above embodiment only have expressed some embodiments of the present invention, and it describes comparatively concrete and detailed, but therefore can not 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 rate measurement device for solid-state material, comprises vacuum heating chamber (100), the vacuum environment needed for described vacuum heating chamber (100) sampling heating, 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), sample warm table (120) is provided with in described vacuum heating chamber (100), well heater is provided with in described sample warm table (120), 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 for the infrared thermal imaging figure of continuous high speed shooting sample;
Described high resolving power high speed infrared thermal imaging system (122) is perpendicular to sample warm table (120) front, 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 rate 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, circulating water pipe (108) is provided with in the locular wall of described vacuum heating chamber (100), 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 recirculated water entrance (103) and circulating water outlet (104) respectively.
3. the solid-solid phase-change rate 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 rate measurement device of a kind of solid-state material according to claim 1, it 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 rate 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 made up of substrate (201) and tapered film (202), described substrate (201) surface is provided with the tapered film (202) that section is right-angle triangle, and after phase transformation, the surfacing of tapered film (202) sample is changed to inversion of phases layer (203).
6. the solid-solid phase-change rate 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) controls 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, comprise the following steps:
1-1, first vacuum heating chamber to be connected with outside vacuum pump set by vacuum interface, sample to be placed on sample warm table, and to close the room door of vacuum heating chamber;
1-2, start to vacuumize, the indoor pressure of heating in vacuum reaches 10 -3during Pa, the locular wall Inner eycle water pipe to vacuum heating chamber leads to cooling circulating water, sets the temperature that need heat and start heating at computer processing module;
1-3, etc. be heated to setting temperature and stable after, if now sample is A phase; Open high resolving power high speed infrared thermal imaging system to take pictures, take pictures interval 1 ~ 3s; Gu when simple dependence temperature realizes admittedly-changes, measuring method skips step 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 is set by computer processing module, and open compressed air source unit and start timing, namely 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 terminate, stop timing, close compressed air source unit, stopping is heated and sample warm table is led to the chilled water of external cooling water pipe, and sample cools, the gas effusion in sample, B phase in version is A phase, and the bright-dark degree of thermograph changes, and machine processing module shows as calculated;
After 1-6, change stop, stopping vacuum pump set, take out sample;
1-7, be the transformation rate of B phase by the A phase in version of computer processing module calculation sample, and B phase in version is the transformation rate of A phase, completes measurement.
CN201310754160.0A 2013-12-31 2013-12-31 A kind of solid-solid phase-change rate measurement device of solid-state material and method Expired - Fee Related CN103713006B (en)

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