CN105973923A - Experiment method of phase transition temperature of copper-based memory alloy micro-area - Google Patents

Experiment method of phase transition temperature of copper-based memory alloy micro-area Download PDF

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Publication number
CN105973923A
CN105973923A CN201610285354.4A CN201610285354A CN105973923A CN 105973923 A CN105973923 A CN 105973923A CN 201610285354 A CN201610285354 A CN 201610285354A CN 105973923 A CN105973923 A CN 105973923A
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copper
memory alloy
phase transition
based memory
transition temperature
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CN201610285354.4A
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CN105973923B (en
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耿贵立
白玉俊
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Shandong University
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Shandong University
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N25/00Investigating or analyzing materials by the use of thermal means
    • G01N25/02Investigating or analyzing materials by the use of thermal means by investigating changes of state or changes of phase; by investigating sintering
    • G01N25/12Investigating or analyzing materials by the use of thermal means by investigating changes of state or changes of phase; by investigating sintering of critical point; of other phase change

Abstract

The invention discloses an experiment method of the phase transition temperature of a copper-based memory alloy micro-area. The method comprises the following steps: detecting the phase transition temperature As of a copper-based memory alloy transiting to a parent phase and the transition ending temperature Af of the copper-based memory alloy at a certain rapid heating rate by using a differential scanning calorimeter; determining the temperature ranges of rapid heating and ultralow speed heating; and setting a heating program according to the determined temperature ranges of rapid heating and ultralow speed heating, and measuring to obtain an experiment result. The experiment method has the advantages of safe and simple steps, reliable experiment data, and no complex devices; and the experiment method is ingeniously designed, further divides the phase transition temperature range, and finally realizes accurate measurement of the phase transition temperature of different micro-areas of the copper-based memory alloy, and lays a foundation for further reveal of the phase transition mechanism and the application design of the micro-area.

Description

A kind of experimental technique of copper-based memory alloy microcell phase transition temperature
Technical field
The present invention relates to the experimental technique of a kind of phase transition temperature, the experiment side of a kind of copper-based memory alloy microcell phase transition temperature Method.
Background technology
For copper-based shape memory alloy element, the operating temperature of namely this memory alloy element of phase transition temperature during heating. Sometimes for meeting memory material some special requirement to performance, often can be added some again in the raw material of copper-based memory alloy Other element a small amount of.But after with the addition of other element of some denier, it is sometimes difficult to detection with conventional general experimental technique The minor variations of phase transition temperature, the especially minor variations of microcell phase transition temperature.But, the most small this microcell phase transition temperature Slight change, if can detect, for disclose microcell phase-change mechanism and design application, be all extremely important.But, existing Have in technology and find no the method that the change of the slight temperature to copper-based memory alloy microcell phase transition temperature is measured.
Summary of the invention
The purpose of the present invention is contemplated to solve the problems referred to above, it is provided that the experimental technique of a kind of copper-based memory alloy microcell phase transition temperature.
To achieve these goals, the present invention adopts the following technical scheme that
The experimental technique of a kind of copper-based memory alloy microcell phase transition temperature, uses differential scanning calorimetry instrument to measure and is the most quickly adding Under hot speed, copper-based memory alloy starts phase transition temperature As and the transformation end temp Af changed to parent phase;Determine quickly heating and The temperature range of Ultra-Low Speed heating;Heating schedule is set also according to the temperature range that fixed described quick heating and Ultra-Low Speed heat Heating, measures and obtains experimental result.
Concrete, the experimental technique of a kind of copper-based memory alloy microcell phase transition temperature, comprise the following steps:
(1) packaged copper-based memory alloy sample to be measured and standard specimen are individually positioned in two samples of differential scanning calorimetry instrument In sample platform;
(2) the copper-based memory alloy sample to be measured that with the addition of trace element starts transformation to parent phase to use fast heating rate to determine Phase transition temperature As and transformation end temp Af;
(3) quickly heating and the temperature range of Ultra-Low Speed heating are determined;
(4) set heating schedule by the temperature range determined in step (3) and heat, measuring and obtain experimental result.
Preferably, in described step (1), copper-based memory alloy sample to be measured and standard specimen is identical in quality, is 70-80 milligram;
Preferably, the standard specimen in described step (1) is α-Al2O3
Preferably, in described step (2), fast heating rate is 5 DEG C/min-15 DEG C/min;
Preferably, in described step (3), the temperature range scope of quickly heating is that room temperature is to than the phase transformation starting to change to parent phase Temperature As is low 5-10 DEG C;
Preferably, in described step (3), the temperature range scope of Ultra-Low Speed heating is than the phase transition temperature starting to change to parent phase As is low 5-10 DEG C extremely high 5-10 DEG C than changing end temp Af;
Preferably, in described step (4), heating schedule is: with 5 DEG C/min-15 DEG C/min in the range of the temperature range of quickly heating Heating rate, with the heating rate of 0.1 DEG C/min in the range of the temperature range of Ultra-Low Speed heating.
Sample after above-mentioned experimental technique heat run, the big endothermic peak originally presented under fast heating rates just in It is now multiple little endothermic peak, thus realizes the accurate measurement of the phase transition temperature to different microcells.Compared with prior art, this Bright have the advantages that:
(1) experimental technique step of the present invention is safe and simple, experimental data is reliable, it is not necessary to additional complexity equipment;
(2) the experimental technique design of the present invention is ingenious, and phase transition temperature interval carries out Further Division, and by changing heating speed Rate realizes the accurate measurement to copper-based memory alloy difference microcell phase transition temperature first, for disclosing microcell phase-change mechanism further and answering Lay a good foundation with design.
Detailed description of the invention
Below in conjunction with embodiment, the invention will be further described.
Embodiment 1: the experimental technique of a kind of copper-based memory alloy microcell phase transition temperature, comprises the following steps:
(1) packaged copper-based memory alloy sample to be measured and standard specimen are individually positioned in two samples of differential scanning calorimetry instrument In sample platform, described copper-based memory alloy sample to be measured and standard specimen quality are 70 milligrams, and described standard specimen is α-Al2O3
(2) heat with the fast heating rate of 5 DEG C/min, determine that the copper-based memory alloy that with the addition of trace element is to mother Start phase transition temperature As and the transformation end temp Af changed mutually;
(3) determining quickly heating and the temperature range of Ultra-Low Speed heating, i.e. quickly the temperature range of heating is that room temperature is to lower than As 10℃;The temperature range of Ultra-Low Speed heating is As-10 DEG C to Af+10 DEG C;
(4) by the heating rate of 5 DEG C/min in room temperature is extremely than the temperature range of As-10 DEG C, at As-10 DEG C extremely By the heating rate of 0.1 DEG C/min in the temperature range of Af+10 DEG C, experimental result is measured.
Embodiment 2: the experimental technique of a kind of copper-based memory alloy microcell phase transition temperature, comprises the following steps:
(1) packaged copper-based memory alloy sample to be measured and standard specimen are individually positioned in two samples of differential scanning calorimetry instrument In sample platform, described copper-based memory alloy sample to be measured and standard specimen quality are 75 milligrams, and described standard specimen is α-Al2O3
(2) heat with the fast heating rate of 10 DEG C/min, determine that the copper-based memory alloy that with the addition of trace element is to mother Start phase transition temperature As and the transformation end temp Af changed mutually;
(3) determining quickly heating and the temperature range of Ultra-Low Speed heating, i.e. quickly the temperature range of heating is that room temperature is to lower than As 7℃;The temperature range of Ultra-Low Speed heating is As-7 DEG C to Af+7 DEG C;
(4) by the heating rate of 15 DEG C/min in room temperature is extremely than the temperature range of As-7 DEG C, at As-7 DEG C to Af+7 DEG C Temperature range in by the heating rate of 0.1 DEG C/min, experimental result is measured.
Embodiment 3: the experimental technique of a kind of copper-based memory alloy microcell phase transition temperature, comprises the following steps:
(1) packaged copper-based memory alloy sample to be measured and standard specimen are individually positioned in two samples of differential scanning calorimetry instrument In sample platform, described copper-based memory alloy sample to be measured and standard specimen quality are 80 milligrams, and described standard specimen is α-Al2O3
(2) heat with the fast heating rate of 15 DEG C/min, determine that the copper-based memory alloy that with the addition of trace element is to mother Start phase transition temperature As and the transformation end temp Af changed mutually;
(3) determining quickly heating and the temperature range of Ultra-Low Speed heating, i.e. quickly the temperature range of heating is that room temperature is to lower than As 5℃;The temperature range of Ultra-Low Speed heating is As-5 DEG C to Af+5 DEG C;
(4) by the heating rate of 15 DEG C/min in room temperature is extremely than the temperature range of As-5 DEG C, at As-5 DEG C to Af+5 DEG C Temperature range in by the heating rate of 0.1 DEG C/min, experimental result is measured.
Embodiment 4: the experimental technique of a kind of copper-based memory alloy microcell phase transition temperature, comprises the following steps:
(1) packaged copper-based memory alloy sample to be measured and standard specimen are individually positioned in two samples of differential scanning calorimetry instrument In sample platform, described copper-based memory alloy sample to be measured and standard specimen quality are 80 milligrams, and described standard specimen is α-Al2O3
(2) heat with the fast heating rate of 15 DEG C/min, determine that the copper-based memory alloy that with the addition of trace element is to mother Start phase transition temperature As and the transformation end temp Af changed mutually;
(3) determining quickly heating and the temperature range of Ultra-Low Speed heating, i.e. quickly the temperature range of heating is that room temperature is to lower than As 10℃;The temperature range of Ultra-Low Speed heating is As-10 DEG C to Af+10 DEG C;
(4) by the heating rate of 8 DEG C/min in room temperature is extremely than the temperature range of As-10 DEG C, at As-10 DEG C extremely By the heating rate of 0.1 DEG C/min in the temperature range of Af+10 DEG C, experimental result is measured.
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 (8)

1. the experimental technique of a copper-based memory alloy microcell phase transition temperature, it is characterised in that use differential scanning calorimetry instrument Under certain fast heating rate, measure phase transition temperature As and transformation end temp that copper-based memory alloy starts to change to parent phase Af;Determine quickly heating and the temperature range of Ultra-Low Speed heating;The temperature heated according to fixed described quick heating and Ultra-Low Speed Interval setting heating schedule also heats, and measures and obtains experimental result.
The experimental technique of a kind of copper-based memory alloy microcell phase transition temperature the most as claimed in claim 1, it is characterised in that include Following steps:
(1) packaged copper-based memory alloy sample to be measured and standard specimen are individually positioned in two samples of differential scanning calorimetry instrument In sample platform;
(2) the copper-based memory alloy sample to be measured that with the addition of trace element starts transformation to parent phase to use fast heating rate to determine Phase transition temperature As and transformation end temp Af;
(3) quickly heating and the temperature range of Ultra-Low Speed heating are determined;
(4) set heating schedule by the temperature range determined in step (3) and heat, measuring and obtain experimental result.
The experimental technique of a kind of copper-based memory alloy microcell phase transition temperature the most as claimed in claim 2, it is characterised in that described In step (1), copper-based memory alloy sample to be measured and standard specimen is identical in quality, is 70-80 milligram.
The experimental technique of a kind of copper-based memory alloy microcell phase transition temperature the most as claimed in claim 2, it is characterised in that described Standard specimen in step (1) is α-Al2O3
The experimental technique of a kind of copper-based memory alloy microcell phase transition temperature the most as claimed in claim 2, it is characterised in that described In step (2), fast heating rate is 5 DEG C/min-15 DEG C/min.
The experimental technique of a kind of copper-based memory alloy microcell phase transition temperature the most as claimed in claim 2, it is characterised in that described In step (3), the temperature range scope of quickly heating is that room temperature is to lower 5-10 DEG C than phase transition temperature As starting to change to parent phase.
The experimental technique of a kind of copper-based memory alloy microcell phase transition temperature the most as claimed in claim 2, it is characterised in that described In step (3), the temperature range scope of Ultra-Low Speed heating is to turn to ratio than low 5-10 DEG C of phase transition temperature As starting to change to parent phase Become end temp Af height 5-10 DEG C.
The experimental technique of a kind of copper-based memory alloy microcell phase transition temperature the most as claimed in claim 2, it is characterised in that described In step (4), heating schedule is: with the heating rate of 5 DEG C/min-15 DEG C/min in the range of the temperature range of quickly heating; With the heating rate of 0.1 DEG C/min in the range of the temperature range of Ultra-Low Speed heating.
CN201610285354.4A 2016-04-30 2016-04-30 A kind of experimental method of copper-based memory alloy microcell phase transition temperature Expired - Fee Related CN105973923B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110524203A (en) * 2019-09-24 2019-12-03 山东大学 It is a kind of can automatic complex copper alloy intelligence car shell preparation method
CN112506248A (en) * 2020-11-20 2021-03-16 华中科技大学 Memory alloy component capable of deforming and recovering and device using same

Citations (2)

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Publication number Priority date Publication date Assignee Title
US7909505B2 (en) * 2005-04-22 2011-03-22 The Ohio State University Method and device for investigation of phase transformations in metals and alloys
CN102062743A (en) * 2009-11-18 2011-05-18 上海梅山钢铁股份有限公司 Method for testing dynamic phase transition of steel

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7909505B2 (en) * 2005-04-22 2011-03-22 The Ohio State University Method and device for investigation of phase transformations in metals and alloys
CN102062743A (en) * 2009-11-18 2011-05-18 上海梅山钢铁股份有限公司 Method for testing dynamic phase transition of steel

Non-Patent Citations (2)

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Title
白玉俊等: ""Influence of Heating Rates on Double Reversible Transformations in CuZnZlMnNi Shape Memory Alloy"", 《稀有金属材料与工程》 *
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110524203A (en) * 2019-09-24 2019-12-03 山东大学 It is a kind of can automatic complex copper alloy intelligence car shell preparation method
CN112506248A (en) * 2020-11-20 2021-03-16 华中科技大学 Memory alloy component capable of deforming and recovering and device using same
CN112506248B (en) * 2020-11-20 2021-08-03 华中科技大学 Memory alloy component capable of deforming and recovering and device using same

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Inventor after: Zhang Aimin

Inventor after: Bai Yujun

Inventor after: Geng Guili

Inventor before: Geng Guili

Inventor before: Bai Yujun

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Granted publication date: 20190402