CN105758888A - Determination method for temperature rise in furnace caused by martensite phase transformation of copper-based memory alloy - Google Patents
Determination method for temperature rise in furnace caused by martensite phase transformation of copper-based memory alloy Download PDFInfo
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- CN105758888A CN105758888A CN201610272781.9A CN201610272781A CN105758888A CN 105758888 A CN105758888 A CN 105758888A CN 201610272781 A CN201610272781 A CN 201610272781A CN 105758888 A CN105758888 A CN 105758888A
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/20—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity
Abstract
The invention discloses a determination method for temperature rise in a furnace caused by martensite phase transformation of copper-based memory alloy.The determination method includes the steps that 1, a furnace body of a differential scanning calorimeter is changed into a low-temperature furnace body into which liquid cooling media can be added; 2, rapid heating and rapid cooling are adopted for determining ending temperature Af of a sample when the sample is converted to a parent phase and ending temperature Mf of the same when the sample is converted to martensite; 3, the temperature ranges of rapid heating and ultra-low speed cooling are determined; 4, heating and cooling programs are set according to the temperature ranges determined in the step3, and an experiment is performed; measurement of an experiment result is performed, and the ultra-low cooling rate in the step3 is smaller than or equal to 0.1 DEG C/min.The experiment method is safe and simple, experiment data is reliable, it can be seen that phase transformation heat released by martensite phase transformation obviously increases the environment temperature inside the furnace, and the determination method has important meaning for research of influences on environment temperature by phase transformation latent heat.
Description
Technical field
The present invention relates to the assay method that a kind of copper-based memory alloy martensitic phase transformation causes in-furnace temperature to go up.
Background technology
For copper-based shape memory alloy element, it is heated to uniform temperature during heating and changes to parent phase, can be in stove during phase transformation
Absorb certain heat;It is cooled to uniform temperature during cooling to martensite transfor mation, certain heat during phase transformation, can be discharged again in stove.
The heat of release can use differential scanning calorimeter to carry out quantitative measurement.Owing to the heat effect of copper-based shape memory alloy is smaller,
The change of furnace inner environment temperature is the most small, is difficult to detection with conventional General Experimental Procedures and comes, but, this furnace inner environment temperature
The minor variations of degree, if can detect, is particularly important for studying latent heat of phase change on the impact of ambient temperature.
Summary of the invention
The purpose of the present invention is contemplated to solve the problems referred to above, it is provided that a kind of copper-based memory alloy martensitic phase transformation causes in-furnace temperature
The assay method gone up.
To achieve these goals, the present invention adopts the following technical scheme that
The assay method that a kind of copper-based memory alloy martensitic phase transformation causes in-furnace temperature to go up, step is as follows:
(1) body of heater of differential scanning calorimeter is changed into the low temperature body of heater of energy adding liquid cooling medium;
(2) use the method for quickly heating and quickly cooling to determine end temp Af that sample changes to parent phase and turning to martensite
The end temp Mf become;
(3) quickly heating and the temperature range of Ultra-Low Speed cooling are determined;
(4) temperature range determined by step (3) sets heating cooling program, and tests;
(5) experimental result is measured;
Ultra-Low Speed cooldown rate in described step (3) :≤-0.1 DEG C/min.
Preferably: in described step (3), quick heating-up temperature is interval: room temperature is to end temp Af+10 DEG C changed to parent phase;Super
Low speed chilling temperature is interval: Af+10 DEG C to Mf-10 DEG C.
Preferably: described standard specimen is α-Al2O3。
Preferably: described sample is 70-80 milligram with the quality of standard specimen.
Preferably: described cooling medium is liquid nitrogen.
Preferably: the fast heating rate of described step (2) and (3) is 5 DEG C/min-25 DEG C/min, quick cooldown rate is
-5℃/min--10℃/min。
Preferably: in described step (4) with the firing rate of 5 DEG C/min-25 DEG C/min carry out the end temp that heats equal to
The ultralow rate of cooling of 0.1 DEG C/min carries out the beginning temperature cooled down, and heating end temp is higher 5-10 DEG C than Af, ultralow quickly cooling
But end temp is lower 5-10 DEG C than Mf.
The application that above-mentioned assay method causes in stove in slight temperature rise in detection alloy martensite phase transformation.
Above-mentioned assay method is studying latent heat of phase change to the application in ambient temperature effect.
Beneficial effects of the present invention:
Sample is after prepared by the inventive method, and tests by the heating cooling program of defined, is originally quickly cooling down speed
The lower big exothermic peak presented of degree is just opened.Owing to Ultra-Low Speed cooldown rate is less than or equal to-0.1 DEG C/min, by parent phase to
Ambient temperature in stove will be stepped up by the heat that martensite transfor mation is discharged, and it is also clear that.
Prior art is thought as its in-furnace temperature of alloy change that the change of this martensitic transformation temperature of copper-based memory alloy is the least
Cannot measure, but inventor uses the differential scanning calorimeter of routine, by specific method by in-furnace temperature
Change amplificationization and detect accurately.
Experimental technique of the present invention is safe and simple, experimental data is reliable.The experimental technique of the present invention is it can be seen that martensitic phase transformation is discharged
Phase transformation heat the ambient temperature in stove is significantly improved, this is particularly important for research latent heat of phase change on the impact of ambient temperature
's.
Detailed description of the invention
Below in conjunction with embodiment, the invention will be further described.
Embodiment 1
The assay method that a kind of copper-based memory alloy martensitic phase transformation causes in-furnace temperature to go up, comprises the following steps:
Packaged sample is put on the sample stage on the left of differential scanning calorimetry instrument by the first step;
Second step weighs the standard specimen of equal quality, after encapsulating with the sample cell of same material, puts in the face of differential scanning calorimetry instrument
On the sample stage on right side;
The body of heater of differential scanning calorimeter is changed into the low temperature body of heater of energy adding liquid cooling medium by the 3rd step;
4th step use the method for quickly heating and quickly cooling to determine end temp Af that copper-based memory alloy changes to parent phase and
To the end temp Mf of martensite transfor mation;
5th step determines quickly heating and the temperature range of Ultra-Low Speed cooling;
6th step sets heating cooling program by the temperature range that the 5th step determines, and tests;
7th step experimental result is measured, and ging up of in-furnace temperature just can be directly in the lab diagram of R-123TP type monitor record
Read out;After there is martensitic phase transformation, temperature raises in fluctuation, and in this embodiment, martensitic phase transformation occurs than just in in-furnace temperature
Time temperature exceed 7 DEG C.
The quality of the sample that the described first step is packaged is 70 milligrams.
Standard specimen α-Al described in described second step2O3Quality be 70 milligrams.
Cooling medium in described 3rd step is liquid nitrogen.
Fast heating rate described in described 4th step the 5th step is 5 DEG C/min, and quick cooldown rate is-5 DEG C/min.
Ultra-Low Speed cooldown rate described in described 5th step is-0.1 DEG C/min, if if instrument allows, and also can be lower.
Quick heating-up temperature interval described in described 5th step is: room temperature is Af+5 DEG C to the end temp changed to parent phase;Institute
The Ultra-Low Speed chilling temperature interval stated is: Af+5 DEG C to Mf-5 DEG C.
The end temp carrying out heating with the firing rate of 5 DEG C/min in described 6th step should be equal to the ultralow cooling with-0.1 DEG C/min
Speed carries out the beginning temperature cooled down, and the end temp Af changed to parent phase that heating end temp also should determine than the 4th step
High 5 DEG C. Ultra-Low Speed cooling end temp should be lower 5 DEG C to the end temp Mf of martensite transfor mation than what the 4th step determined.
Embodiment 2
The assay method that a kind of copper-based memory alloy martensitic phase transformation causes in-furnace temperature to go up, comprises the following steps:
Packaged sample is put on the sample stage on the left of differential scanning calorimetry instrument by the first step;
Second step weighs the standard specimen of equal quality, after encapsulating with the sample cell of same material, puts in the face of differential scanning calorimetry instrument
On the sample stage on right side;
The body of heater of differential scanning calorimeter is changed into the low temperature body of heater of energy adding liquid cooling medium by the 3rd step;
4th step use the method for quickly heating and quickly cooling to determine end temp Af that copper-based memory alloy changes to parent phase and
To the end temp Mf of martensite transfor mation;
5th step determines quickly heating and the temperature range of Ultra-Low Speed cooling;
6th step sets heating cooling program by the temperature range that the 5th step determines, and tests;
7th step experimental result is measured, and in this embodiment, in-furnace temperature exceeds 7.5 DEG C than temperature when just there is martensitic phase transformation.
The quality of the sample that the described first step is packaged is 75 milligrams.
Standard specimen α-Al described in described second step2O3Quality be 75 milligrams.
Cooling medium in described 3rd step is liquid nitrogen.
Fast heating rate described in described 4th step the 5th step is 10 DEG C/min, and quick cooldown rate is-7 DEG C/min.
Ultra-Low Speed cooldown rate described in described 5th step is-0.1 DEG C/min, if if instrument allows, and also can be lower.
Quick heating-up temperature interval described in described 5th step is: room temperature is Af+7 DEG C to the end temp changed to parent phase;Institute
The Ultra-Low Speed chilling temperature interval stated is: Af+7 DEG C to Mf-7 DEG C.
Carrying out, with the firing rate of 10 DEG C/min, the end temp that heats in described 6th step should ultralow cold equal to-0.1 DEG C/min
But speed carries out the beginning temperature cooled down, and the end temp Af changed to parent phase that heating end temp also should determine than the 4th step
High 7 DEG C. Ultra-Low Speed cooling end temp should be lower 7 DEG C to the end temp Mf of martensite transfor mation than what the 4th step determined.
Embodiment 3
The assay method that a kind of copper-based memory alloy martensitic phase transformation causes in-furnace temperature to go up, comprises the following steps:
Packaged sample is put on the sample stage on the left of differential scanning calorimetry instrument by the first step;
Second step weighs the standard specimen of equal quality, after encapsulating with the sample cell of same material, puts in the face of differential scanning calorimetry instrument
On the sample stage on right side;
The body of heater of differential scanning calorimeter is changed into the low temperature body of heater of energy adding liquid cooling medium by the 3rd step;
4th step use the method for quickly heating and quickly cooling to determine end temp Af that copper-based memory alloy changes to parent phase and
To the end temp Mf of martensite transfor mation;
5th step determines quickly heating and the temperature range of Ultra-Low Speed cooling;
6th step sets heating cooling program by the temperature range that the 5th step determines, and tests;
7th step experimental result is measured, and in this embodiment, in-furnace temperature exceeds 8 DEG C than temperature when just there is martensitic phase transformation.
The quality of the sample that the described first step is packaged is 80 milligrams.
Standard specimen α-Al described in described second step2O3Quality be 80 milligrams.
Cooling medium in described 3rd step is liquid nitrogen.
Fast heating rate described in described 4th step the 5th step is 15 DEG C/min, and quick cooldown rate is-10 DEG C/min.
Ultra-Low Speed cooldown rate described in described 5th step is-0.1 DEG C/min, if if instrument allows, and also can be lower.
Quick heating-up temperature interval described in described 5th step is: room temperature is Af+10 DEG C to the end temp changed to parent phase;
Described Ultra-Low Speed chilling temperature interval is: Af+10 DEG C to Mf-10 DEG C.
Carrying out, with the firing rate of 15 DEG C/min, the end temp that heats in described 6th step should ultralow cold equal to-0.1 DEG C/min
But speed carries out the beginning temperature cooled down, and the end temp Af changed to parent phase that heating end temp also should determine than the 4th step
High 10 DEG C. Ultra-Low Speed cooling end temp should be lower 10 DEG C to the end temp Mf of martensite transfor mation than what the 4th step determined.
Embodiment 4
The assay method that a kind of copper-based memory alloy martensitic phase transformation causes in-furnace temperature to go up, comprises the following steps:
Packaged sample is put on the sample stage on the left of differential scanning calorimetry instrument by the first step;
Second step weighs the standard specimen of equal quality, after encapsulating with the sample cell of same material, puts in the face of differential scanning calorimetry instrument
On the sample stage on right side;
The body of heater of differential scanning calorimeter is changed into the low temperature body of heater of energy adding liquid cooling medium by the 3rd step;
4th step use the method for quickly heating and quickly cooling to determine end temp Af that copper-based memory alloy changes to parent phase and
To the end temp Mf of martensite transfor mation;
5th step determines quickly heating and the temperature range of Ultra-Low Speed cooling;
6th step sets heating cooling program by the temperature range that the 5th step determines, and tests;
7th step experimental result is measured, and in this embodiment, in-furnace temperature exceeds 7 DEG C than temperature when just there is martensitic phase transformation.
The quality of the sample that the described first step is packaged is 70 milligrams.
Standard specimen α-Al described in described second step2O3Quality be 70 milligrams.
Cooling medium in described 3rd step is liquid nitrogen.
Fast heating rate described in described 4th step the 5th step is 20 DEG C/min, and quick cooldown rate is-10 DEG C/min.
Ultra-Low Speed cooldown rate described in described 5th step is-0.1 DEG C/min, if if instrument allows, and also can be lower.
Quick heating-up temperature interval described in described 5th step is: room temperature is Af+10 DEG C to the end temp changed to parent phase;
Described Ultra-Low Speed chilling temperature interval is: Af+10 DEG C to Mf-5 DEG C.
The end temp carrying out heating with the firing rate of 5 DEG C/min in described 6th step should be equal to the ultralow cooling with-0.1 DEG C/min
Speed carries out the beginning temperature cooled down, and the end temp Af changed to parent phase that heating end temp also should determine than the 4th step
High 10 DEG C. Ultra-Low Speed cooling end temp should be lower 5 DEG C to the end temp Mf of martensite transfor mation than what the 4th step determined.
Although the above-mentioned detailed description of the invention to the present invention is described, but not limiting the scope of the invention, affiliated
Skilled person should be understood that on the basis of technical scheme, and those skilled in the art need not pay creativeness
Various amendments that work can be made or adjust still within protection scope of the present invention.
Claims (10)
1. copper-based memory alloy martensitic phase transformation causes the assay method that in-furnace temperature gos up, and it is characterized in that: step is as follows:
(1) body of heater of differential scanning calorimeter is changed into the low temperature body of heater of energy adding liquid cooling medium;
(2) use the method for quickly heating and quickly cooling to determine end temp Af that sample and standard specimen change to parent phase and to horse
The end temp Mf that family name's body changes;
(3) quickly heating and the temperature range of Ultra-Low Speed cooling are determined;
(4) temperature range determined by step (3) sets heating cooling program, and tests;
(5) experimental result is measured;
Ultra-Low Speed cooldown rate in described step (3): less than or equal to-0.1 DEG C/min;In described step (4) with
The end temp that the firing rate of 5 DEG C/min-25 DEG C/min carries out heating is equal to carrying out cold with the ultralow rate of cooling of-0.1 DEG C/min
But beginning temperature, and heating end temp is higher 5-10 DEG C than Af, Ultra-Low Speed cooling end temp is lower 5-10 DEG C than Mf.
2. assay method as claimed in claim 1, is characterized in that: in step (3), quick heating-up temperature is interval: room temperature extremely to
End temp Af+10 DEG C that parent phase changes.
3. assay method as claimed in claim 1, is characterized in that: in step (3), Ultra-Low Speed chilling temperature is interval: Af+10 DEG C
To Mf-10 DEG C.
4. assay method as claimed in claim 1, is characterized in that: described standard specimen is α-Al2O3。
5. assay method as claimed in claim 1, is characterized in that: described sample is 70-80 milligram with the quality of standard specimen.
6. assay method as claimed in claim 1, is characterized in that: described cooling medium is liquid nitrogen.
7. assay method as claimed in claim 1, is characterized in that: the fast heating rate of described step (2) is
5 DEG C/min-25 DEG C/min, quick cooldown rate is-5 DEG C/min--10 DEG C/min.
8. assay method as claimed in claim 1, is characterized in that: the fast heating rate of described step (3) is
5 DEG C/min-25 DEG C/min, quick cooldown rate is-5 DEG C/min--10 DEG C/min.
9. the arbitrary described assay method of claim 1-8 causes during in stove, slight temperature gos up in detection alloy martensite phase transformation
Application.
10. the arbitrary described assay method of claim 1-8 is studying latent heat of phase change to the application in ambient temperature effect.
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2016
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US20080215131A1 (en) * | 2006-12-04 | 2008-09-04 | Cook Incorporated | Method for loading a medical device into a delivery system |
CN101889200A (en) * | 2007-12-04 | 2010-11-17 | 库克公司 | Method of characterizing phase transformations in shape memory materials |
CN103499599A (en) * | 2013-10-11 | 2014-01-08 | 南京航空航天大学 | Memory alloy phase-change temperature measuring method and measuring system for implementing same |
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