CN105738405A - Method for determining pure phase change enthalpy of copper-based memory alloy martensite - Google Patents
Method for determining pure phase change enthalpy of copper-based memory alloy martensite Download PDFInfo
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- G01N25/02—Investigating or analyzing materials by the use of thermal means by investigating changes of state or changes of phase; by investigating sintering
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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
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Abstract
The invention discloses a method for determining pure phase change enthalpy of a copper-based memory alloy martensite. The method includes the following steps that 1, the end temperature Af of transformation towards a parent phase and the end temperature Mf of transformation from the parent phase to the martensite of a copper-based memory alloy sample are firstly detected by utilizing a differential scanning calorimetry analyzer; 2, secondary rapid heating and ultra-low-speed sub-cooling are performed, the end temperature of the transformation towards the parent phase of the copper-based memory alloy sample during rapid heating is Af + 5 DEG C-Af + 10 DEG C, the starting temperature of ultra-low-speed sub-cooling is Af + 5 DEG C-Af + 10 DEG C, the end temperature of ultra-low-speed sub-cooling is Mf +10 DEG C-Mf +15 DEG C, and the sum of the right side small peak areas in peaks scanned in the ultra-low-speed sub-cooling process is the pure phase change enthalpy. According to the method, the mode that the total phase-change enthalpy and a heat capacity change enthalpy are firstly and respectively calculated and then a method for subtracting the heat capacity change enthalpy from total phase-change enthalpy is utilized to calculate the pure phase change enthalpy is not needed, a pure phase change enthalpy value can be directly obtained by creatively determining the temperature range of the ultra-low-speed sub-cooling, and the operating process can be made more simplified, quicker and more convenient.
Description
Technical field
Present invention relates particularly to the assay method of a kind of pure enthalpy of phase change of copper-based memory alloy martensite.
Background technology
For copper-based shape memory alloy, start cooling down from parent phase state, when temperature reaches parent phase to martensite transfor mation
Beginning temperature Ms time, another kind of phase will be converted into from a kind of phase, i.e. be converted into martensitic phase from parent phase, its pure phase transformation
Enthalpy is how many？How about carry out means of differential scanning calorimetry (DSC) experiment, could directly obtain pure enthalpy of phase change？From present case
From the point of view of, there is no the experimental technique of maturation, be therefore experimental technique the most urgently to be resolved hurrily and technical problem.Real with regard to current routine
For testing, being only capable of obtaining total enthalpy of phase change, pure enthalpy of phase change cannot individually obtain.Accordingly, it would be desirable to cuprio can be remembered by research one
The method that the pure enthalpy of phase change of alloy martensite individually detects.
Summary of the invention
It is an object of the invention to as overcoming above the deficiencies in the prior art, it is provided that a kind of pure enthalpy of phase change of copper-based memory alloy martensite
Assay method.
For achieving the above object, technical scheme is as follows:
The assay method of the pure enthalpy of phase change of copper-based memory alloy martensite, comprises the following steps:
1) first with the differential scanning calorimetry instrument detection end temp Af that changes to parent phase of copper-based memory alloy sample and by
Parent phase is to the end temp Mf of martensite transfor mation；
2) carry out secondary rapid heating and time Ultra-Low Speed cooling, quickly add and hanker the knot that copper-based memory alloy sample changes to parent phase
Shu Wendu is Af+5 DEG C-Af+10 DEG C, and the initial temperature of secondary Ultra-Low Speed cooling is Af+5 DEG C-Af+10 DEG C, and end temp is
Mf-10 DEG C-Mf-15 DEG C, in the peak that obtains of secondary Ultra-Low Speed cooling procedure scanning, a series of little peak area on right side and be pure phase
Become enthalpy.
In secondary Ultra-Low Speed cooling procedure, inside scanning figure right side a series of small peak and be pure enthalpy of phase change, of left side
Bigger peak area is that phase transformation thermal capacitance changes enthalpy.
When using differential scanning calorimetry instrument that sample is quickly heated, Af can be made slightly to raise, during post bake, will
Quickly the end temp of heating is set as Af+5 DEG C-Af+10 DEG C, it is ensured that during cooling, the parent phase from 100% starts test；Secondary super
Low speed cooling can make martensite finish temperature Mf reduce more, by secondary Ultra-Low Speed cooling end temp be set as Mf-10 DEG C-
Mf-15 DEG C, can guarantee that terminating in the record range that curve all appears in instrument of pure enthalpy of phase change.When initiateing to knot of pure enthalpy of phase change
When the curve of bundle all appears within instrument record range, with temperature as abscissa, so that it may directly measurement martensitic phase transformation is pure
Enthalpy of phase change, it is not necessary to obtain phase transformation total enthalpy the most respectively and thermal capacitance changes enthalpy, then deduct the method calculating of thermal capacitance change enthalpy with phase transformation total enthalpy
Pure enthalpy of phase change.
Preferably, step 1) in the quality of sample used and standard specimen be 70-80mg, standard specimen is α-Al2O3。
Preferably, step 1) and step 2) in the speed of quickly heating be 5-25 DEG C/min.
Preferably, step 1) in, quickly the speed of cooling is 5-10 DEG C/min.
Preferably, step 2) in, the speed of secondary Ultra-Low Speed cooling is 0.2 DEG C/min.
Preferably, step 1) concretely comprise the following steps:
1) packaged sample and standard specimen are individually placed on the left of differential scanning calorimetry instrument and on the sample stage on right side；
2) body of heater of DSC is replaced with the low temperature body of heater of energy adding liquid cooling medium；
3) use the method for quickly heating to determine the end temp Af that copper-based memory alloy changes to parent phase, use quickly cooling
Method determine copper-based memory alloy by parent phase to the end temp Mf of martensite transfor mation.
It is changed without body of heater and cannot add liquid nitrogen, if natural cooling can only be realized more than room temperature without liquid nitrogen, natural cooling
Speed is change, is not maintained at setting value.It addition, cannot be carried out without liquid nitrogen cooling below room temperature at all.Change
Body of heater, has had a cooling of liquid nitrogen, and rate of temperature fall just can be cooled down by the rate of temperature fall set, and then meets wanting of this experiment
Ask.
Preferably, step 2) in cooling medium be liquid nitrogen.
Said determination method is the application in the pure enthalpy of phase change of martensite measuring memorial alloy, is especially measuring cuprio memory
Application in the pure enthalpy of phase change of martensite of alloy.
The Advantageous Effects of the present invention is:
The method of the present invention, by creatively determining time Ultra-Low Speed chilling temperature scope, can directly try to achieve the value of pure enthalpy of phase change,
Phase transformation total enthalpy need not be obtained the most respectively and thermal capacitance changes enthalpy, then deduct the method pure phase transformation of calculating of thermal capacitance change enthalpy with phase transformation total enthalpy
Enthalpy, makes operating process more simplify, fast.This had both had great theoretical meaning to the physicochemical characteristic of research copper-based memory alloy
Justice, has again extremely important practical significance.Also the pure enthalpy of phase change research for same type of material provides simplifications, accurately, fast
Experimental technique.Therefore, the method for the present invention has extremely important using value for material phase transformation research.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is further described.
Embodiment 1: the assay method of the pure enthalpy of phase change of copper-based memory alloy martensite, comprises the following steps:
The first step, is individually placed on the left of differential scanning calorimetry instrument and the sample on right side by packaged sample and standard specimen
On platform；
Second step, is replaced with the low temperature body of heater of energy adding liquid cooling medium by the body of heater of DSC；
3rd step, uses the method for quickly heating to determine the end temp Af that copper-based memory alloy changes to parent phase, uses quickly
Cooling method determine copper-based memory alloy by parent phase to the end temp Mf of martensite transfor mation；
4th step, determines quickly heating and the temperature range of secondary Ultra-Low Speed cooling；
5th step, the temperature range determined by the 4th step sets quickly heating and secondary Ultra-Low Speed cooling program, and tests；
6th step, experimental result is measured.
Sample and the quality of standard specimen described in the described first step are 70 milligrams, and standard specimen is α-Al2O3。
Cooling medium described in described second step is liquid nitrogen.
Fast heating rate described in described 3rd step is 5 DEG C/min, and quick cooldown rate is-5 DEG C/min.
Secondary Ultra-Low Speed cooldown rate described in described 4th step is-0.2 DEG C/min.
Quick heating-up temperature interval described in described 4th step is: room temperature is to end temp Af+5 DEG C changed to parent phase；Institute
The secondary Ultra-Low Speed chilling temperature interval stated is: Af+5 DEG C to Mf-10 DEG C.
The end temp quickly heated with the firing rate of 5 DEG C/min in described 5th step should equal to-0.2 DEG C/min time
Ultralow rate of cooling carries out the beginning temperature cooled down, and the knot changed to parent phase that heating end temp also should determine than the 3rd step
Shu Wendu Af is high 5 DEG C.The end temp Mf to martensite transfor mation that secondary Ultra-Low Speed cooling end temp should determine than the 3rd step
Low 10 DEG C, the pure enthalpy of phase change recorded is equal to 4.02mJ.
Comparative example 1
Other conditions are the most same as in Example 1, and the quick heating-up temperature interval in the 4th step is that room temperature is to the knot changed to parent phase
Shu Wendu Af, secondary Ultra-Low Speed chilling temperature scope is Af-Mf.Total enthalpy of phase change is 267.92mJ, and phase transformation thermal capacitance changes enthalpy and is
263.49mJ, both differences-pure enthalpy of phase change is 4.43mJ.
Comparative example 2
Other conditions are the most same as in Example 1, and the quick heating-up temperature interval in the 4th step is that room temperature is to the knot changed to parent phase
Shu Wendu Af, secondary Ultra-Low Speed chilling temperature scope is Af-Mf-10 DEG C.Total enthalpy of phase change is 267.92mJ, and phase transformation thermal capacitance changes enthalpy
For 263.89mJ, both differences-pure enthalpy of phase change is 4.03mJ.
Visible, the pure enthalpy of phase change that documents 1 records has bigger deviation, and reason is the meeting when using low speed cooling cooling
The end temp Mf making martensite reduces more, when being reduced to Mf, the most completely converts, and namely peak does not also have
It is fully completed, but owing to this part peak area is less, the most difficult discovery.
Inventor is found that this phenomenon, and is adjusted temperature range in concrete test, has not only saved detection,
Also improve the accuracy of detection.
Embodiment 2: the assay method of the pure enthalpy of phase change of copper-based memory alloy martensite, comprises the following steps:
The first step, is individually placed on the left of differential scanning calorimetry instrument and the sample on right side by packaged sample and standard specimen
On platform；
Second step, is replaced with the low temperature body of heater of energy adding liquid cooling medium by the body of heater of DSC；
3rd step, uses the method for quickly heating to determine the end temp Af that copper-based memory alloy changes to parent phase, uses quickly
Cooling method determine copper-based memory alloy by parent phase to the end temp Mf of martensite transfor mation；
4th step, determines quickly heating and the temperature range of secondary Ultra-Low Speed cooling；
5th step, the temperature range determined by the 4th step sets quickly heating and secondary Ultra-Low Speed cooling program, and tests；
6th step, experimental result is measured.
Sample and the quality of standard specimen described in the described first step are 75 milligrams, and standard specimen is α-Al2O3。
Cooling medium described in described second step is liquid nitrogen.
Fast heating rate described in described 3rd step the 4th step is 10 DEG C/min, and quick cooldown rate is-10 DEG C/min.
Secondary Ultra-Low Speed cooldown rate described in described 4th step is-0.2 DEG C/min.
Quick heating-up temperature interval described in described 4th step is: room temperature is to end temp Af+6 DEG C changed to parent phase；Institute
The secondary Ultra-Low Speed chilling temperature interval stated is: Af+6 DEG C to Mf-11 DEG C.
The end temp quickly heated with the firing rate of 10 DEG C/min in described 5th step should be equal to-0.2 DEG C/min's
Secondary ultralow rate of cooling carries out the beginning temperature cooled down, and heating end temp also should be than changing to parent phase of determining of the 3rd step
End temp Af is high 6 DEG C.The end temp to martensite transfor mation that secondary Ultra-Low Speed cooling end temp should determine than the 3rd step
Mf is low 11 DEG C.
Embodiment 3: the assay method of the pure enthalpy of phase change of copper-based memory alloy martensite, comprises the following steps:
The first step, is individually placed on the left of differential scanning calorimetry instrument and the sample on right side by packaged sample and standard specimen
On platform；
Second step, is replaced with the low temperature body of heater of energy adding liquid cooling medium by the body of heater of DSC；
3rd step, uses the method for quickly heating to determine the end temp Af that copper-based memory alloy changes to parent phase, uses quickly
Cooling method determine copper-based memory alloy by parent phase to the end temp Mf of martensite transfor mation；
4th step, determines quickly heating and the temperature range of secondary Ultra-Low Speed cooling；
5th step, the temperature range determined by the 4th step sets quickly heating and secondary Ultra-Low Speed cooling program, and tests；
6th step, experimental result is measured.
Sample and the quality of standard specimen described in the described first step are 77 milligrams, and standard specimen is α-Al2O3。
Cooling medium described in described second step is liquid nitrogen.
Fast heating rate described in described 3rd step the 4th step is 15 DEG C/min, and quick cooldown rate is-15 DEG C/min.
Secondary Ultra-Low Speed cooldown rate described in described 4th step is-0.2 DEG C/min.
Quick heating-up temperature interval described in described 4th step is: room temperature is to end temp Af+8 DEG C changed to parent phase；Institute
The secondary Ultra-Low Speed chilling temperature interval stated is: Af+8 DEG C to Mf-12 DEG C.
The end temp quickly heated with the firing rate of 15 DEG C/min in described 5th step should be equal to-0.2 DEG C/min's
Secondary ultralow rate of cooling carries out the beginning temperature cooled down, and heating end temp also should be than changing to parent phase of determining of the 3rd step
End temp Af is high 8 DEG C. the end temp Mf to martensite transfor mation that secondary Ultra-Low Speed cooling end temp should determine than the 3rd step
Low 12 DEG C.
Embodiment 4: the assay method of the pure enthalpy of phase change of copper-based memory alloy martensite, comprises the following steps:
The first step, is individually placed on the left of differential scanning calorimetry instrument and the sample on right side by packaged sample and standard specimen
On platform；
Second step, is replaced with the low temperature body of heater of energy adding liquid cooling medium by the body of heater of DSC；
3rd step, uses the method for quickly heating to determine the end temp Af that copper-based memory alloy changes to parent phase, uses quickly
Cooling method determine copper-based memory alloy by parent phase to the end temp Mf of martensite transfor mation；
4th step, determines quickly heating and the temperature range of secondary Ultra-Low Speed cooling；
5th step, the temperature range determined by the 4th step sets quickly heating and secondary Ultra-Low Speed cooling program, and tests；
6th step, experimental result is measured.
Sample and the quality of standard specimen described in the described first step are 80 milligrams, and standard specimen is α-Al2O3。
Cooling medium described in described second step is liquid nitrogen.
Fast heating rate described in described 3rd step the 4th step is 20 DEG C/min, and quick cooldown rate is-20 DEG C/min.
Secondary Ultra-Low Speed cooldown rate described in described 4th step is-0.2 DEG C/min.
Quick heating-up temperature interval described in described 4th step is: room temperature is to end temp Af+10 DEG C changed to parent phase；Institute
The secondary Ultra-Low Speed chilling temperature interval stated is: Af+10 DEG C to Mf-15 DEG C.
The end temp quickly heated with the firing rate of 20 DEG C/min in described 5th step should be equal to-0.2 DEG C/min's
Secondary ultralow rate of cooling carries out the beginning temperature cooled down, and heating end temp also should be than changing to parent phase of determining of the 3rd step
End temp Af is high 10 DEG C.The end temp to martensite transfor mation that secondary Ultra-Low Speed cooling end temp should determine than the 3rd step
Mf is low 15 DEG C.
The detailed description of the invention of the present invention is described although above-mentioned in conjunction with the embodiments, but not to invention protection domain
Limiting, one of ordinary skill in the art should be understood that, on the basis of technical scheme, those skilled in the art are not required to
Various amendments or adjustment that creative work to be paid can be made are the most within the scope of the present invention.
Claims (8)
1. the assay method of the pure enthalpy of phase change of copper-based memory alloy martensite, it is characterised in that: comprise the following steps:
1) first with the differential scanning calorimetry instrument detection end temp Af that changes to parent phase of copper-based memory alloy sample and by
Parent phase is to the end temp Mf of martensite transfor mation；
2) carry out secondary rapid heating and time Ultra-Low Speed cooling, quickly add and hanker the knot that copper-based memory alloy sample changes to parent phase
Shu Wendu is Af+5 DEG C-Af+10 DEG C, and the initial temperature of secondary Ultra-Low Speed cooling is Af+5 DEG C-Af+10 DEG C, and end temp is
Mf-10 DEG C-Mf-15 DEG C, in the peak that obtains of secondary Ultra-Low Speed cooling procedure scanning, the area of a series of small peaks on right side and be pure
Enthalpy of phase change.
Assay method the most according to claim 1, it is characterised in that: step 1) in sample used and the quality of standard specimen
For 70-80mg, standard specimen is α-Al2O3。
Assay method the most according to claim 1, it is characterised in that: step 1) and step 2) in quick heating
Speed is 5-25 DEG C/min.
Assay method the most according to claim 1, it is characterised in that: step 1) in, quickly the speed of cooling is 5-10 DEG C
/min。
Assay method the most according to claim 1, it is characterised in that: step 2) in, the speed of secondary Ultra-Low Speed cooling is
0.2℃/min。
Assay method the most according to claim 1, it is characterised in that: step 1) concretely comprise the following steps:
1) packaged sample and standard specimen are individually placed on the left of differential scanning calorimetry instrument and on the sample stage on right side；
2) body of heater of DSC is replaced with the low temperature body of heater of energy adding liquid cooling medium；
3) use the method for quickly heating to determine the end temp Af that copper-based memory alloy changes to parent phase, use quickly cooling
Method determine copper-based memory alloy by parent phase to the end temp Mf of martensite transfor mation.
Assay method the most according to claim 6, it is characterised in that: step 2) in cooling medium be liquid nitrogen.
8. the arbitrary described assay method of claim 1-7 is the application in the pure enthalpy of phase change of martensite measuring memorial alloy,
The especially application in the pure enthalpy of phase change of martensite measuring copper-based memory alloy.
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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 |
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