CN105758888B - Copper-based memory alloy martensitic traoformation causes the assay method that in-furnace temperature gos up - Google Patents

Copper-based memory alloy martensitic traoformation causes the assay method that in-furnace temperature gos up Download PDF

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CN105758888B
CN105758888B CN201610272781.9A CN201610272781A CN105758888B CN 105758888 B CN105758888 B CN 105758888B CN 201610272781 A CN201610272781 A CN 201610272781A CN 105758888 B CN105758888 B CN 105758888B
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cooling
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CN105758888A (en
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张爱敏
白玉俊
耿贵立
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Shandong University
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    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N25/00Investigating or analyzing materials by the use of thermal means
    • G01N25/20Investigating 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

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Abstract

The invention discloses copper-based memory alloy martensitic traoformations to cause the assay method that in-furnace temperature gos up, and steps are as follows:(1) furnace body of differential scanning calorimeter is changed into low temperature furnace body that energy adding liquid cools down medium;(2) the end temp Af that sample changes to the parent phase and end temp Mf to martensite transfor mation is determined using the method for quickly heating and being quickly cooled down;(3) temperature range of quickly heating and Ultra-Low Speed cooling is determined;(4) the temperature range setting heating cooling program that step (3) determines is pressed, and is tested;(5) experimental result measures;Ultra-Low Speed cooling rate in the step (3):Less than or equal to 0.1 DEG C/min.Experimental method of the present invention is safe and simple, experimental data is reliable, it can be seen that the phase transformation heat that martensitic traoformation is discharged significantly improves the environment temperature in stove, this is particularly important to studying influence of the latent heat of phase change to environment temperature.

Description

Copper-based memory alloy martensitic traoformation causes the assay method that in-furnace temperature gos up
Technical field
The present invention relates to a kind of copper-based memory alloy martensitic traoformations to cause the assay method that in-furnace temperature gos up.
Background technology
For copper-based shape memory alloy element, when heating, is heated to certain temperature and changes to parent phase, meeting when phase transformation Certain heat is absorbed out of stove;Certain temperature is cooled to when cooling to martensite transfor mation, when phase transformation can discharge one into stove again Fixed heat.The heat of release can use differential scanning calorimeter to carry out quantitative measurment.Due to copper-based shape memory alloy Fuel factor is smaller, and the variation of furnace inner environment temperature is very small, with conventional General Experimental Procedures be difficult detection come, still, The minor change of this furnace inner environment temperature, if can detected, the influence for research latent heat of phase change to environment temperature is pole It is important.
Invention content
The purpose of the present invention is exactly that solve the above-mentioned problems, providing a kind of copper-based memory alloy martensitic traoformation causes stove The assay method of interior temperature recovery.
To achieve the goals above, the present invention adopts the following technical scheme that:
A kind of copper-based memory alloy martensitic traoformation causes the assay method of in-furnace temperature rise, and steps are as follows:
(1) furnace body of differential scanning calorimeter is changed into low temperature furnace body that energy adding liquid cools down medium;
(2) end temp Af that sample changes to parent phase determined using the method that quickly heats and be quickly cooled down and to geneva The end temp Mf of body transformation;
(3) temperature range of quickly heating and Ultra-Low Speed cooling is determined;
(4) the temperature range setting heating cooling program that step (3) determines is pressed, and is tested;
(5) experimental result measures;
Ultra-Low Speed cooling rate in the step (3):≤-0.1℃/min.
It is preferred that:Quick heating temperature section in the step (3):Af+10 DEG C of the end temp that room temperature extremely changes to parent phase; Ultra-Low Speed cooling temperature section:Af+10 DEG C to Mf-10 DEG C.
It is preferred that:The standard specimen is α-Al2O3
It is preferred that:The quality of the sample and standard specimen is 70-80 milligrams.
It is preferred that:The cooling medium is liquid nitrogen.
It is preferred that:The fast heating rate of the step (2) and (3) be 5 DEG C/min-25 DEG C/min, be quickly cooled down rate be- 5℃/min--10℃/min。
It is preferred that:The end temp heated with the heating speed of 5 DEG C/min-25 DEG C/min in the step (4) is equal to Cooling start temperature is carried out with the ultralow cooling velocity of 0.1 DEG C/min, and heats end temp ratio Af high 5-10 DEG C, Ultra-Low Speed Cooling end temp ratio Mf is 5-10 DEG C low.
Above-mentioned assay method causes the application in stove in slight temperature rise in detection alloy martensite phase transformation.
Above-mentioned assay method is in research latent heat of phase change to the application in ambient temperature effect.
Beneficial effects of the present invention:
Sample is tested after prepared by the method for the present invention, and by the heating cooling program of defined, originally quick The one big exothermic peak presented under cooling velocity is just opened.Due to Ultra-Low Speed cooling rate be less than or equal to -0.1 DEG C/ Min, the heat released from parent phase to martensite transfor mation will step up the environment temperature in stove, and be also clear that.
Think to change in very small its stove of alloy as this martensitic transformation temperature of copper-based memory alloy in the prior art Temperature change is unable to measure, but inventor passes through specific method using conventional differential scanning calorimeter In-furnace temperature is changed into amplificationization and is accurately detected.
Experimental method of the present invention is safe and simple, experimental data is reliable.Martensitic traoformation can be seen in the experimental method of the present invention The phase transformation heat discharged significantly improves the environment temperature in stove, this is for studying influence of the latent heat of phase change to environment temperature Particularly important.
Specific implementation mode
With reference to embodiment, the invention will be further described.
Embodiment 1
A kind of copper-based memory alloy martensitic traoformation causes the assay method of in-furnace temperature rise, includes 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 the sample cell encapsulation of same material, is put into face of differential scanning calorimetry On sample stage on the right side of analyzer;
The furnace body of differential scanning calorimeter is changed into the low temperature furnace body that energy adding liquid cools down medium by third step;
4th step determines the end temperature that copper-based memory alloy changes to parent phase using the method for quickly heating and being quickly cooled down Spend the Af and end temp Mf to martensite transfor mation;
5th step determines the temperature range of quickly heating and Ultra-Low Speed cooling;
The temperature range setting heating cooling program that 6th step is determined by the 5th step, and tested;
7th step experimental result measures, the rise of the in-furnace temperature energy in the lab diagram that R-123TP type recorders record Directly read out;After there is martensitic traoformation, temperature increases in fluctuation, and in-furnace temperature than just martensite occurs in the embodiment Temperature when phase transformation is higher by 7 DEG C.
The quality of the packaged sample of the first step is 70 milligrams.
Standard specimen α-Al described in the second step2O3Quality be 70 milligrams.
Cooling medium in the third step is liquid nitrogen.
Fast heating rate described in the 5th step of 4th step is 5 DEG C/min, and it is -5 DEG C/min to be quickly cooled down rate.
Ultra-Low Speed cooling rate described in 5th step is -0.1 DEG C/min, if if instrument allows, it can also be lower.
Quick heating temperature section described in 5th step is:Room temperature to the end temp changed to parent phase is Af+5 ℃;The Ultra-Low Speed cooling temperature section is:Af+5 DEG C to Mf-5 DEG C
The end temp heated with the heating speed of 5 DEG C/min in 6th step should be equal to -0.1 DEG C/min's Ultralow cooling velocity carries out cooling start temperature, and heating end temp should also be than the knot of the 4th step determination changed to parent phase 5 DEG C of Ultra-Low Speeds cooling end temps of Shu Wendu Af high should be lower by 5 than the end temp Mf to martensite transfor mation that the 4th step determines ℃。
Embodiment 2
A kind of copper-based memory alloy martensitic traoformation causes the assay method of in-furnace temperature rise, includes 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 the sample cell encapsulation of same material, is put into face of differential scanning calorimetry On sample stage on the right side of analyzer;
The furnace body of differential scanning calorimeter is changed into the low temperature furnace body that energy adding liquid cools down medium by third step;
4th step determines the end temperature that copper-based memory alloy changes to parent phase using the method for quickly heating and being quickly cooled down Spend the Af and end temp Mf to martensite transfor mation;
5th step determines the temperature range of quickly heating and Ultra-Low Speed cooling;
The temperature range setting heating cooling program that 6th step is determined by the 5th step, and tested;
7th step experimental result measures, and in-furnace temperature is higher by than temperature when just there is martensitic traoformation in the embodiment 7.5℃。
The quality of the packaged sample of the first step is 75 milligrams.
Standard specimen α-Al described in the second step2O3Quality be 75 milligrams.
Cooling medium in the third step is liquid nitrogen.
Fast heating rate described in the 5th step of 4th step is 10 DEG C/min, be quickly cooled down rate be -7 DEG C/ min。
Ultra-Low Speed cooling rate described in 5th step is -0.1 DEG C/min, if if instrument allows, it can also be lower.
Quick heating temperature section described in 5th step is:Room temperature to the end temp changed to parent phase is Af+7 ℃;The Ultra-Low Speed cooling temperature section is:Af+7 DEG C to Mf-7 DEG C
The end temp heated with the heating speed of 10 DEG C/min in 6th step should be equal to -0.1 DEG C/min Ultralow cooling velocity carry out cooling start temperature, and changing to parent phase of heating that end temp should also determine than the 4th step 7 DEG C of Ultra-Low Speeds cooling end temps of end temp Af high should be lower by 7 than the end temp Mf to martensite transfor mation that the 4th step determines ℃.
Embodiment 3
A kind of copper-based memory alloy martensitic traoformation causes the assay method of in-furnace temperature rise, includes 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 the sample cell encapsulation of same material, is put into face of differential scanning calorimetry On sample stage on the right side of analyzer;
The furnace body of differential scanning calorimeter is changed into the low temperature furnace body that energy adding liquid cools down medium by third step;
4th step determines the end temperature that copper-based memory alloy changes to parent phase using the method for quickly heating and being quickly cooled down Spend the Af and end temp Mf to martensite transfor mation;
5th step determines the temperature range of quickly heating and Ultra-Low Speed cooling;
The temperature range setting heating cooling program that 6th step is determined by the 5th step, and tested;
7th step experimental result measures, and in-furnace temperature is higher by 8 than temperature when just there is martensitic traoformation in the embodiment ℃。
The quality of the packaged sample of the first step is 80 milligrams.
Standard specimen α-Al described in the second step2O3Quality be 80 milligrams.
Cooling medium in the third step is liquid nitrogen.
Fast heating rate described in the 5th step of 4th step is 15 DEG C/min, be quickly cooled down rate be -10 DEG C/ min。
Ultra-Low Speed cooling rate described in 5th step is -0.1 DEG C/min, if if instrument allows, it can also be lower.
Quick heating temperature section described in 5th step is:Room temperature to the end temp changed to parent phase is Af+ 10℃;The Ultra-Low Speed cooling temperature section is:Af+10 DEG C to Mf-10 DEG C
The end temp heated with the heating speed of 15 DEG C/min in 6th step should be equal to -0.1 DEG C/min Ultralow cooling velocity carry out cooling start temperature, and changing to parent phase of heating that end temp should also determine than the 4th step 10 DEG C of Ultra-Low Speeds cooling end temps of end temp Af high should be lower than the end temp Mf to martensite transfor mation that the 4th step determines 10℃.
Embodiment 4
A kind of copper-based memory alloy martensitic traoformation causes the assay method of in-furnace temperature rise, includes 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 the sample cell encapsulation of same material, is put into face of differential scanning calorimetry On sample stage on the right side of analyzer;
The furnace body of differential scanning calorimeter is changed into the low temperature furnace body that energy adding liquid cools down medium by third step;
4th step determines the end temperature that copper-based memory alloy changes to parent phase using the method for quickly heating and being quickly cooled down Spend the Af and end temp Mf to martensite transfor mation;
5th step determines the temperature range of quickly heating and Ultra-Low Speed cooling;
The temperature range setting heating cooling program that 6th step is determined by the 5th step, and tested;
7th step experimental result measures, and in-furnace temperature is higher by 7 than temperature when just there is martensitic traoformation in the embodiment ℃。
The quality of the packaged sample of the first step is 70 milligrams.
Standard specimen α-Al described in the second step2O3Quality be 70 milligrams.
Cooling medium in the third step is liquid nitrogen.
Fast heating rate described in the 5th step of 4th step is 20 DEG C/min, be quickly cooled down rate be -10 DEG C/ min。
Ultra-Low Speed cooling rate described in 5th step is -0.1 DEG C/min, if if instrument allows, it can also be lower.
Quick heating temperature section described in 5th step is:Room temperature to the end temp changed to parent phase is Af+ 10℃;The Ultra-Low Speed cooling temperature section is:Af+10 DEG C to Mf-5 DEG C
The end temp heated with the heating speed of 5 DEG C/min in 6th step should be equal to -0.1 DEG C/min's Ultralow cooling velocity carries out cooling start temperature, and heating end temp should also be than the knot of the 4th step determination changed to parent phase 10 DEG C of Ultra-Low Speeds cooling end temps of Shu Wendu Af high should be lower by 5 than the end temp Mf to martensite transfor mation that the 4th step determines ℃.
Although the above-mentioned specific implementation mode to the present invention is described, not to the limit of the scope of the present invention System, those skilled in the art should understand that, based on the technical solutions of the present invention, those skilled in the art need not pay Go out the various modifications or adjust still within protection scope of the present invention that creative work can be made.

Claims (6)

1. a kind of copper-based memory alloy martensitic traoformation causes the assay method that in-furnace temperature gos up, it is characterized in that:Steps are as follows:
(1) furnace body of differential scanning calorimeter is changed into low temperature furnace body that energy adding liquid cools down medium;
(2) end temp Af that sample and standard specimen change to parent phase determined using the method that quickly heats and be quickly cooled down and to horse The end temp Mf of family name's body transformation;
(3) temperature range of quickly heating and Ultra-Low Speed cooling is determined;
(4) the temperature range setting heating cooling program that step (3) determines is pressed, and is tested;
(5) experimental result measures;
The fast heating rate of the step (2) be 5 DEG C/min-25 DEG C/min, be quickly cooled down rate be -5 DEG C/min--10 DEG C/ min;
Ultra-Low Speed cooling rate in the step (3):Less than or equal to -0.1 DEG C/min;
The fast heating rate of the step (3) is 5 DEG C/min-25 DEG C/min;
Quick heating temperature section in the step (3):Af+10 DEG C of the end temp that room temperature extremely changes to parent phase;
The temperature range that Ultra-Low Speed cools down in the step (3):Af+10 DEG C to Mf-10 DEG C;
The end temp heated with the heating speed of 5 DEG C/min-25 DEG C/min in the step (4) is equal to be less than or wait Cooling start temperature is carried out in the Ultra-Low Speed cooling rate of -0.1 DEG C/min, and heats end temp ratio Af high 5-10 DEG C, is surpassed Low speed cooling end temp ratio Mf is 5-10 DEG C low.
2. assay method as described in claim 1, it is characterized in that:The standard specimen is α-Al2O3
3. assay method as described in claim 1, it is characterized in that:The quality of the sample and standard specimen is 70-80 milligrams.
4. assay method as described in claim 1, it is characterized in that:The cooling medium is liquid nitrogen.
5. any assay methods of claim 1-4 cause in stove in detection alloy martensite phase transformation in slight temperature rise Application.
6. any assay methods of claim 1-4 are in research latent heat of phase change to the application in ambient temperature effect.
CN201610272781.9A 2016-04-28 2016-04-28 Copper-based memory alloy martensitic traoformation causes the assay method that in-furnace temperature gos up Expired - Fee Related CN105758888B (en)

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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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