CN105738405B - The assay method of the pure enthalpy of phase change of copper-based memory alloy martensite - Google Patents
The assay method of the pure enthalpy of phase change of copper-based memory alloy martensite Download PDFInfo
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- CN105738405B CN105738405B CN201610267880.8A CN201610267880A CN105738405B CN 105738405 B CN105738405 B CN 105738405B CN 201610267880 A CN201610267880 A CN 201610267880A CN 105738405 B CN105738405 B CN 105738405B
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Abstract
The invention discloses the assay methods of the pure enthalpy of phase change of copper-based memory alloy martensite, include the following steps：1) first with the differential scanning calorimetry instrument end temp Af that changes to parent phase of detection copper-based memory alloy sample and from parent phase to the end temp Mf of martensite transfor mation；2) it carries out secondary rapid heating and time Ultra-Low Speed cools down, the end temp that quickly copper-based memory alloy sample changes to parent phase in heating is Af+5 DEG C Af+10 DEG C, the initial temperature of secondary Ultra-Low Speed cooling is Af+5 DEG C Af+10 DEG C, end temp is 10 DEG C of Mf, 15 DEG C of Mf, in the peak that secondary Ultra-Low Speed cooling procedure scans, the small peak area in right side and as pure enthalpy of phase change.The method of the present invention need not first find out phase transformation total enthalpy respectively and thermal capacitance changes enthalpy, again the pure enthalpy of phase change of method calculating that thermal capacitance changes enthalpy is subtracted with phase transformation total enthalpy, by creatively determining time Ultra-Low Speed cooling temperature range, the value of pure enthalpy of phase change can be directly acquired, so that operating process is more simplified, is quick.
Description
Technical field
Present invention relates particularly to a kind of assay methods of the pure enthalpy of phase change of copper-based memory alloy martensite.
Background technology
For copper-based shape memory alloy, the cooling down since parent phase state, when temperature reaches parent phase to geneva
When the start temperature Ms of body transformation, it will be converted into another phase from a kind of phase, i.e., be converted into martensitic phase from parent phase,
Pure enthalpy of phase change is how manyDifferential scanning calorimetry (DSC) experiment how about is carried out, pure enthalpy of phase change can be just directly acquiredFrom current
From the point of view of situation, ripe experimental method is there is no, therefore is experimental method and technical problem urgently to be resolved hurrily at present.With regard to current normal
For rule experiment, it is only capable of obtaining total phase change enthalpy, pure enthalpy of phase change can not be obtained individually.It can will be copper-based therefore, it is necessary to study one kind
The method that the pure enthalpy of phase change of memorial alloy martensite is individually detected.
Invention content
The purpose of the present invention is to overcome the above the deficiencies in the prior art, provide a kind of copper-based memory alloy martensite pure phase
Become the assay method of enthalpy.
To achieve the above object, technical scheme is as follows：
The assay method of the pure enthalpy of phase change of copper-based memory alloy martensite, includes the following steps：
1) end temp changed to parent phase first with differential scanning calorimetry instrument detection copper-based memory alloy sample
Af and from parent phase to the end temp Mf of martensite transfor mation；
2) it carries out secondary rapid heating and time Ultra-Low Speed cools down, quickly copper-based memory alloy sample changes to parent phase in heating
End temp be Af+5 DEG C-Af+10 DEG C, the initial temperature of secondary Ultra-Low Speed cooling is Af+5 DEG C-Af+10 DEG C, and end temp is
It is Mf-10 DEG C-Mf-15 DEG C, a series of small peak areas on right side and as pure in the peak that secondary Ultra-Low Speed cooling procedure scans
Enthalpy of phase change.
In secondary Ultra-Low Speed cooling procedure, inside scanning figure a series of small peak on right side and be pure enthalpy of phase change, left side
A larger peak area be phase transformation thermal capacitance change enthalpy.
When quickly being heated to sample using differential scanning calorimetry instrument, Af can be made slightly to increase, when reheating,
The end temp quickly heated is set as Af+5 DEG C-Af+10 DEG C, it is ensured that tested since 100% parent phase when cooling；It is secondary
Ultra-Low Speed cooling can make martensite finish temperature Mf reduce it is more, by secondary Ultra-Low Speed cooling end temp be set as Mf-10 DEG C-
Mf-15 DEG C, it can guarantee that the end curve of pure enthalpy of phase change all appears in the record range of instrument.When pure enthalpy of phase change starting extremely
When the curve of end is all appeared within instrument record range, using temperature as abscissa, so that it may directly measure martensitic traoformation
Pure enthalpy of phase change, it is not necessary to first find out phase transformation total enthalpy and thermal capacitance respectively and change enthalpy, then the side that thermal capacitance changes enthalpy is subtracted with phase transformation total enthalpy
Method calculates pure enthalpy of phase change.
Preferably, the quality of sample used in step 1) and standard specimen is 70-80mg, and standard specimen is α-Al2O3。
Preferably, the rate quickly heated in step 1) and step 2) is 5-25 DEG C/min.
Preferably, in step 1), the rate being quickly cooled down is 5-10 DEG C/min.
Preferably, in step 2), the rate of secondary Ultra-Low Speed cooling is 0.2 DEG C/min.
Preferably, step 1) the specific steps are：
1) packaged sample and standard specimen are individually placed to the sample in face of differential scanning calorimetry instrument left and right side
On platform；
2) furnace body of DSC is replaced with the low temperature furnace body that energy adding liquid cools down medium；
3) the end temp Af that copper-based memory alloy changes to parent phase is determined using the method quickly heated, using fast quickly cooling
But method determines end temp Mf of the copper-based memory alloy from parent phase to martensite transfor mation.
Liquid nitrogen can not be added by being changed without furnace body, natural if natural cooling can only be realized more than room temperature by not adding liquid nitrogen
Cooling rate is variation, is not maintained at setting value.In addition, do not add liquid nitrogen room temperature cooling below at all can not be into
Row.Furnace body has been changed, has had the cooling of liquid nitrogen, rate of temperature fall can be cooled down by the rate of temperature fall of setting, and then meet the reality
The requirement tested.
Preferably, the cooling medium in step 2) is liquid nitrogen.
Said determination method is the application in the pure enthalpy of phase change of martensite for measuring memorial alloy, especially copper-based in measurement
Application in the pure enthalpy of phase change of martensite of memorial alloy.
The present invention advantageous effects be：
The method of the present invention by creatively determining time Ultra-Low Speed cooling temperature range, can directly acquire pure enthalpy of phase change it
Value, it is not necessary to first find out phase transformation total enthalpy and thermal capacitance respectively and change enthalpy, then with phase transformation total enthalpy subtract thermal capacitance change enthalpy method calculate it is pure
Enthalpy of phase change makes operating process more simplify, is quick.This both has great theory to the physicochemical characteristic for studying copper-based memory alloy
Meaning, and there is extremely important practical significance.Also it is provided for the research of the pure enthalpy of phase change of same type of material and simplifies, is accurate, is quick
Experimental method.Therefore, method of the invention has extremely important application value for material phase transformation research.
Specific implementation mode
With reference to 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, includes the following steps：
Packaged sample and standard specimen are individually placed in face of differential scanning calorimetry instrument left and right side by the first step
On sample stage；
The furnace body of DSC is replaced with the low temperature furnace body that energy adding liquid cools down medium by second step；
Third walks, and the end temp Af that copper-based memory alloy changes to parent phase is determined using the method quickly heated, uses
The method being quickly cooled down determines end temp Mf of the copper-based memory alloy from parent phase to martensite transfor mation；
4th step determines the temperature range of quickly heating and the cooling of secondary Ultra-Low Speed；
5th step, the temperature range setting determined by the 4th step is quickly heated and secondary Ultra-Low Speed cooling program, and carries out reality
It tests；
6th step, experimental result measure.
The quality of sample and standard specimen described in the first step is 70 milligrams, and standard specimen is α-Al2O3。
Cooling medium described in the second step is liquid nitrogen.
Fast heating rate described in the third step is 5 DEG C/min, and it is -5 DEG C/min to be quickly cooled down rate.
Secondary Ultra-Low Speed cooling rate described in 4th step is -0.2 DEG C/min.
Quick heating temperature section described in 4th step is：The end temp Af+5 that room temperature extremely changes to parent phase
℃；The secondary Ultra-Low Speed cooling temperature section is：Af+5 DEG C to Mf-10 DEG C.
The end temp quickly heated with the heating speed of 5 DEG C/min in 5th step should be equal to -0.2 DEG C/
Time ultralow cooling velocity of min carries out cooling start temperature, and heats end temp also and should be walked than third and is determining to parent phase
5 DEG C of the end temp Af high of transformation.Secondary Ultra-Low Speed cooling end temp should walk the determining end to martensite transfor mation than third
The low pure enthalpy of phase change 10 DEG C, measured of temperature Mf is equal to 4.02mJ.
Comparative example 1
Other conditions are same as Example 1, and the quick heating temperature section in the 4th step is that room temperature turns to parent phase
The end temp Af of change, secondary Ultra-Low Speed cooling temperature range are Af-Mf.Total phase change enthalpy is 267.92mJ, and phase transformation thermal capacitance changes enthalpy
The pure enthalpy of phase change of difference-for 263.49mJ, the two is 4.43mJ.
Comparative example 2
Other conditions are same as Example 1, and the quick heating temperature section in the 4th step is that room temperature turns to parent phase
The end temp Af of change, secondary Ultra-Low Speed cooling temperature range are Af-Mf-10 DEG C.Total phase change enthalpy is 267.92mJ, and phase transformation thermal capacitance changes
For change enthalpy into 263.89mJ, the pure enthalpy of phase change of difference-of the two is 4.03mJ.
As it can be seen that there is the pure enthalpy of phase change that documents 1 measure larger deviation, reason to be to be cooled down when using low speed cooling
When that the end temp Mf of martensite can be made to reduce is more, when being reduced to Mf, there are no completely it is transformed come, that is, peak do not have also
It is fully completed, but since the part peak area is smaller, generally more difficult discovery.
Inventor is found that this phenomenon, and is adjusted to temperature range in specific experiment, and inspection has not only been saved
Link is surveyed, the accuracy of detection is also improved.
Embodiment 2：The assay method of the pure enthalpy of phase change of copper-based memory alloy martensite, includes the following steps：
Packaged sample and standard specimen are individually placed in face of differential scanning calorimetry instrument left and right side by the first step
On sample stage；
The furnace body of DSC is replaced with the low temperature furnace body that energy adding liquid cools down medium by second step；
Third walks, and the end temp Af that copper-based memory alloy changes to parent phase is determined using the method quickly heated, uses
The method being quickly cooled down determines end temp Mf of the copper-based memory alloy from parent phase to martensite transfor mation；
4th step determines the temperature range of quickly heating and the cooling of secondary Ultra-Low Speed；
5th step, the temperature range setting determined by the 4th step is quickly heated and secondary Ultra-Low Speed cooling program, and carries out reality
It tests；
6th step, experimental result measure.
The quality of sample and standard specimen described in the first step is 75 milligrams, and standard specimen is α-Al2O3。
Cooling medium described in the second step is liquid nitrogen.
It is 10 DEG C/min that the third, which walks the fast heating rate described in the 4th step, be quickly cooled down rate be -10 DEG C/
min。
Secondary Ultra-Low Speed cooling rate described in 4th step is -0.2 DEG C/min.
Quick heating temperature section described in 4th step is：The end temp Af+6 that room temperature extremely changes to parent phase
℃；The secondary Ultra-Low Speed cooling temperature section is：Af+6 DEG C to Mf-11 DEG C.
The end temp quickly heated with the heating speed of 10 DEG C/min in 5th step should be equal to -0.2 DEG C/
Time ultralow cooling velocity of min carries out cooling start temperature, and heats end temp also and should be walked than third and is determining to parent phase
6 DEG C of the end temp Af high of transformation.Secondary Ultra-Low Speed cooling end temp should walk the determining end to martensite transfor mation than third
Temperature Mf is 11 DEG C low.
Embodiment 3：The assay method of the pure enthalpy of phase change of copper-based memory alloy martensite, includes the following steps：
Packaged sample and standard specimen are individually placed in face of differential scanning calorimetry instrument left and right side by the first step
On sample stage；
The furnace body of DSC is replaced with the low temperature furnace body that energy adding liquid cools down medium by second step；
Third walks, and the end temp Af that copper-based memory alloy changes to parent phase is determined using the method quickly heated, uses
The method being quickly cooled down determines end temp Mf of the copper-based memory alloy from parent phase to martensite transfor mation；
4th step determines the temperature range of quickly heating and the cooling of secondary Ultra-Low Speed；
5th step, the temperature range setting determined by the 4th step is quickly heated and secondary Ultra-Low Speed cooling program, and carries out reality
It tests；
6th step, experimental result measure.
The quality of sample and standard specimen described in the first step is 77 milligrams, and standard specimen is α-Al2O3。
Cooling medium described in the second step is liquid nitrogen.
It is 15 DEG C/min that the third, which walks the fast heating rate described in the 4th step, be quickly cooled down rate be -15 DEG C/
min。
Secondary Ultra-Low Speed cooling rate described in 4th step is -0.2 DEG C/min.
Quick heating temperature section described in 4th step is：The end temp Af+8 that room temperature extremely changes to parent phase
℃；The secondary Ultra-Low Speed cooling temperature section is：Af+8 DEG C to Mf-12 DEG C.
The end temp quickly heated with the heating speed of 15 DEG C/min in 5th step should be equal to -0.2 DEG C/
Time ultralow cooling velocity of min carries out cooling start temperature, and heats end temp also and should be walked than third and is determining to parent phase
8 DEG C of Ultra-Low Speed cooling end temps of end temp Af high of transformation should walk the determining end to martensite transfor mation than third
Temperature Mf is 12 DEG C low.
Embodiment 4：The assay method of the pure enthalpy of phase change of copper-based memory alloy martensite, includes the following steps：
Packaged sample and standard specimen are individually placed in face of differential scanning calorimetry instrument left and right side by the first step
On sample stage；
The furnace body of DSC is replaced with the low temperature furnace body that energy adding liquid cools down medium by second step；
Third walks, and the end temp Af that copper-based memory alloy changes to parent phase is determined using the method quickly heated, uses
The method being quickly cooled down determines end temp Mf of the copper-based memory alloy from parent phase to martensite transfor mation；
4th step determines the temperature range of quickly heating and the cooling of secondary Ultra-Low Speed；
5th step, the temperature range setting determined by the 4th step is quickly heated and secondary Ultra-Low Speed cooling program, and carries out reality
It tests；
6th step, experimental result measure.
The quality of sample and standard specimen described in the first step is 80 milligrams, and standard specimen is α-Al2O3。
Cooling medium described in the second step is liquid nitrogen.
It is 20 DEG C/min that the third, which walks the fast heating rate described in the 4th step, be quickly cooled down rate be -20 DEG C/
min。
Secondary Ultra-Low Speed cooling rate described in 4th step is -0.2 DEG C/min.
Quick heating temperature section described in 4th step is：The end temp Af+10 that room temperature extremely changes to parent phase
℃；The secondary Ultra-Low Speed cooling temperature section is：Af+10 DEG C to Mf-15 DEG C.
The end temp quickly heated with the heating speed of 20 DEG C/min in 5th step should be equal to -0.2 DEG C/
Time ultralow cooling velocity of min carries out cooling start temperature, and heats end temp also and should be walked than third and is determining to parent phase
10 DEG C of the end temp Af high of transformation.Secondary Ultra-Low Speed cooling end temp should walk the determining end to martensite transfor mation than third
Temperature Mf is 15 DEG C low.
Although above-mentioned be described the specific implementation mode of the present invention in conjunction with the embodiments, model not is protected to invention
The limitation enclosed, those skilled in the art should understand that, based on the technical solutions of the present invention, those skilled in the art are not
It needs to make the creative labor the various modifications that can be made or adjustment is still within the scope of the present invention.
Claims (5)
1. the assay method of the pure enthalpy of phase change of copper-based memory alloy martensite, it is characterised in that：Include the following steps：
1) packaged sample and standard specimen are individually placed on the sample stage of differential scanning calorimetry instrument left and right side；
2) furnace body of DSC is replaced with the low temperature furnace body that energy adding liquid cools down medium；
3) the end temp Af that copper-based memory alloy changes to parent phase is determined using the method quickly heated, using what is be quickly cooled down
Method determines end temp Mf of the copper-based memory alloy from parent phase to martensite transfor mation；
4) it carries out secondary rapid heating and time Ultra-Low Speed cools down, the knot that quickly copper-based memory alloy sample changes to parent phase in heating
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, end temp Mf-10
DEG C-Mf-15 DEG C, in the peak that secondary Ultra-Low Speed cooling procedure scans, a series of area of small peaks on right side and as pure phase
Become enthalpy；
Cooling medium described in step 2) is liquid nitrogen；
The rate being quickly cooled down described in step 3) is 5-10 DEG C/min.
2. assay method according to claim 1, it is characterised in that：The quality of sample used in step 1) and standard specimen is
70-80mg, standard specimen are α-Al2O3。
3. assay method according to claim 1, it is characterised in that：Step 3) and 4) in the rate quickly heated be 5-
25℃/min。
4. assay method according to claim 1, it is characterised in that：In step 4), the rate of secondary Ultra-Low Speed cooling is 0.2
℃/min。
5. any assay method answering in the pure enthalpy of phase change of martensite for measuring copper-based memory alloy in claim 1-4
With.
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Citations (2)
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| 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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| ATE499912T1 (en) * | 2006-12-04 | 2011-03-15 | Cook Inc | METHOD FOR INSERTING A MEDICAL DEVICE INTO A RELEASE SYSTEM |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Non-Patent Citations (3)
| Title |
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| CuZnAlMnNi形状记忆合金马氏体相变焓的研究;耿贵立;《功能材料》;19961231;第27卷(第6期);49-50、54，参见摘要、第1-4部分 * |
| 冷速对CuZnAlMnNi记忆合金Ms点的影响;吕伟 等;《山东工业大学学报》;20000630;第30卷(第3期);250-253 * |
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