CN111830074A - Thermal analysis method for testing easily volatile and oxidizable alloy material by reusable nested sealed crucible - Google Patents
Thermal analysis method for testing easily volatile and oxidizable alloy material by reusable nested sealed crucible Download PDFInfo
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- CN111830074A CN111830074A CN202010717163.7A CN202010717163A CN111830074A CN 111830074 A CN111830074 A CN 111830074A CN 202010717163 A CN202010717163 A CN 202010717163A CN 111830074 A CN111830074 A CN 111830074A
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- 238000012360 testing method Methods 0.000 title claims abstract description 41
- 238000002076 thermal analysis method Methods 0.000 title claims abstract description 40
- 239000000956 alloy Substances 0.000 title claims abstract description 16
- 238000007789 sealing Methods 0.000 claims abstract description 91
- 238000000034 method Methods 0.000 claims abstract description 15
- 229910052715 tantalum Inorganic materials 0.000 claims abstract description 11
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 claims abstract description 11
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052802 copper Inorganic materials 0.000 claims abstract description 7
- 239000010949 copper Substances 0.000 claims abstract description 7
- 238000005303 weighing Methods 0.000 claims description 9
- 238000003825 pressing Methods 0.000 claims description 8
- 238000010998 test method Methods 0.000 claims description 7
- 238000012937 correction Methods 0.000 claims description 4
- 238000004064 recycling Methods 0.000 claims description 2
- 229910045601 alloy Inorganic materials 0.000 abstract description 9
- 230000008569 process Effects 0.000 abstract description 9
- 238000005259 measurement Methods 0.000 abstract description 6
- 238000013461 design Methods 0.000 abstract description 5
- 238000007254 oxidation reaction Methods 0.000 abstract description 5
- 230000003647 oxidation Effects 0.000 abstract description 4
- 238000004458 analytical method Methods 0.000 abstract description 2
- 238000002474 experimental method Methods 0.000 abstract 1
- 229910000861 Mg alloy Inorganic materials 0.000 description 12
- 239000007789 gas Substances 0.000 description 9
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 7
- 230000000694 effects Effects 0.000 description 7
- 229910052749 magnesium Inorganic materials 0.000 description 7
- 239000011777 magnesium Substances 0.000 description 7
- 229910000838 Al alloy Inorganic materials 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 230000001681 protective effect Effects 0.000 description 3
- 238000010926 purge Methods 0.000 description 3
- 238000004364 calculation method Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 229910001297 Zn alloy Inorganic materials 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000001938 differential scanning calorimetry curve Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- -1 magnesium-aluminum-zinc Chemical compound 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Materials Using Thermal Means (AREA)
Abstract
The invention belongs to the technical field of analysis and test, and relates to a thermal analysis method for testing a volatile and easily-oxidized alloy material by using a reusable nested sealed crucible. The test sample is placed in a sealed crucible for thermal analysis, the sealed crucible comprises an outer crucible, a cylindrical sealing gasket and an inner crucible, the inner crucible and the outer crucible are made of tantalum with the purity of 99.7, the gasket is made of red copper, and the crucible is sealed through interference fit of the inner crucible and the outer crucible and the gasket. The sealing process is operated in an open space, and the operation requirement is not high. The inner crucible and the outer crucible can be repeatedly used, and the experiment cost is reduced. The sealed crucible is adopted to prevent the sample from contacting with air, so that the influence of sample volatilization and oxidation on thermal analysis measurement is inhibited, and a more accurate test result can be obtained; so that the thermal analysis becomes a conventional experimental means for the alloy design of the easily volatile and oxidizable alloy.
Description
Technical Field
The invention belongs to the technical field of analysis and test, and relates to a thermal analysis method for testing an alloy material containing volatile and easily-oxidizable elements by using a nested sealed crucible.
Background
The information in this background section is only for enhancement of understanding of the general background of the invention and is not necessarily to be construed as an admission or any form of suggestion that this information forms the prior art that is already known to a person of ordinary skill in the art.
In the research and production process of metal materials, the thermophysical parameters of the metal materials, such as phase transition temperature, enthalpy and specific heat, need to be accurately known, and thermal analysis is the most important experimental means for obtaining the parameters.
During the thermal analysis test, the thermal analysis was performed in a protective atmosphere and in an open crucible for materials that did not contain volatile, easily oxidizable elements. For magnesium alloys containing volatile, easily oxidizable elements: on one hand, because elements are easy to oxidize, a sample is easy to have oxidation reaction with impurities such as water and oxygen in protective gas in protective atmosphere, so that the heat effect of the oxidation process interferes the test result; on the other hand, due to the high volatility of magnesium, the vapor pressure of the metal continues to increase as the temperature increases during thermal analysis. In the open crucible, the volatilized metal vapor is continuously discharged to pollute a sensor of the thermal analyzer and reduce the service life of the analyzer; meanwhile, the quality and heat of the sample are taken away by the volatile metal vapor, and the accuracy of the test is reduced. Under the combined action of two factors, the conventional thermal analysis method is rarely used for measuring the thermal physical parameters of the alloys containing volatile and easily-oxidized elements such as magnesium, zinc and the like, so that the thermal physical parameters of the alloys are rare and have poor consistency.
Disclosure of Invention
The invention aims to provide a reusable sealed nested crucible low-cost thermal analysis method aiming at the problems of high measurement result error and pollution test equipment of alloy containing volatile and easily-oxidizable elements
In order to achieve the technical purpose, the invention adopts the following technical scheme:
in a first aspect of the invention, there is provided a reusable nested sealed crucible comprising: inner and outer crucibles and a sealing gasket; the sealing gasket is barrel-shaped, and the inner crucible, the outer crucible and the sealing gasket are in interference fit to form a sealing space.
Inside and outside crucible and seal gasket pass through interference fit and form sealed sample space, and rough calculation learns that the confined space can bear 4 atmospheric pressures, because the expansion rate of tantalum crucible is far less than the copper sealing pad at the intensification in-process, the sealed pressure-bearing of crucible exceeds 4 atmospheric pressures in the test procedure, and the sealed gas only forms 3 atmospheric pressures in the intensification process in the crucible in the test procedure. The sealing also inhibits volatilization, so that the heat loss caused by volatilization in the subsequent heating process can be effectively reduced, and the precision of measuring the thermal physical parameters is improved.
In a second aspect of the invention, there is provided a method of testing the sealing of any one of the above reusable nested sealed crucibles, comprising:
pressing the inner crucible into the sealing gasket, then putting the sample into the inner crucible, and pressing the outer crucible from top to bottom to form a sealed space, thus obtaining the product.
The mass of gas in the sealed space was about 0.065mg, taking a 15mg magnesium alloy sample as an example, the effect of oxidation on the test was within four thousandths of an hour. The error of the whole test is basically consistent with the error of other conventional thermal analysis.
In a third aspect of the present invention, a thermal analysis method for testing a volatile and easily oxidizable alloy material is provided, which includes:
any of the reusable nested sealed crucibles described above is used as a reference crucible;
pressing the inner crucible into the sealing gasket, then putting the sample into the inner crucible, and pressing the outer crucible from top down to form a sealed space; respectively weighing the crucible, the sealing gasket and the sample;
and (3) putting the sealed crucible into DSC equipment, and carrying out thermal analysis by using the temperature and heat correction file of the sealed crucible disclosed by the invention.
By adopting the thermal analysis method, the thermal analysis test for measuring the volatile and easily-oxidized alloy with easy operation, low cost and high precision can be realized, so that the thermal analysis becomes a conventional experimental means for magnesium alloy design. The DSC experimental effect of the magnesium alloy is basically consistent with that of the aluminum alloy.
In a fourth aspect of the invention, there is provided a method of recycling any of the above reusable nested sealed crucibles, wherein FeCl is added after completion of the thermal analysis test3The solution dissolves the sealing gasket and collects the inner crucible and the outer crucible, thus being capable of being repeatedly used.
The invention has the beneficial effects that:
(1) by adopting the thermal analysis method, the thermal analysis test for measuring the volatile and easily-oxidized alloy with easy operation, low cost and high precision can be realized, so that the thermal analysis becomes a conventional experimental means for magnesium alloy design. The DSC experimental effect of the magnesium alloy is basically consistent with that of the aluminum alloy.
(2) The device has the advantages of simple structure, convenient operation, strong practicability and easy popularization.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate exemplary embodiments of the invention and together with the description serve to explain the invention and not to limit the invention.
FIG. 1 is a three-dimensional solid explanatory view of a nested crucible of example 1 of the present invention; wherein, 1, the inner crucible, 2, the sealing gasket and 3, the outer crucible.
FIG. 2 is a DSC curve of pure magnesium in example 1 of the present invention.
Detailed Description
It is to be understood that the following detailed description is exemplary and is intended to provide further explanation of the invention as claimed. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the invention. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof, unless the context clearly indicates otherwise.
The invention designs a set of sealed crucible for testing. In order to make the object and technical solution of the present invention more clear, the present invention provides the following drawings for explanation: FIG. 1 is a three-dimensional solid view of a nested crucible; the size of the outer crucible is consistent with that of a crucible for conventional thermal analysis, the crucible is made of a tantalum sheet with the purity of 99.7, which does not react with elements of a test sample, the sealing gasket is changed into a cylindrical shape from a sheet shape, the sealing area is increased, the friction force between the crucible and the gasket is increased, and the material is red copper; inside and outside crucible and seal gasket pass through interference fit and form sealed sample space, and rough calculation learns that the confined space can bear 4 atmospheric pressures, because the expansion rate of tantalum crucible is far less than the copper sealing pad at the intensification in-process, the sealed pressure-bearing of crucible exceeds 4 atmospheric pressures in the test procedure, and the sealed gas only forms 3 atmospheric pressures in the intensification process in the crucible in the test procedure. The sealing also inhibits volatilization, can effectively reduce heat loss caused by volatilization in the subsequent heating process, and improves the precision of the measurement of the thermophysical parameters, which can be seen from the embodiment 1 (figure 2).
The typical sample sealing method of the invention: to reduce the complexity of the operation, the seal is operated in an open environment. The inner crucible is pressed into the sealing gasket firstly, then the sample is placed into the inner crucible, the outer crucible is pressed down from the top to form a sealing space, then the whole crucible is placed into the measuring support in an inverted mode, and the sealing gasket is not in contact with the bottom in the outer crucible due to the round angle at the bottom of the outer crucible, so that the contact between the sample and the sealing gasket after the sample is melted is avoided. The mass of gas in the sealed space was about 0.065mg, taking a 15mg magnesium alloy sample as an example, the effect of oxidation on the test was within four thousandths of an hour. The error of the whole test is basically consistent with the error of other conventional thermal analysis.
The method can be used for thermal analysis of alloy materials containing volatile easily-oxidizable elements, such as magnesium alloys.
A typical thermal analysis method for magnesium alloys: taking a magnesium alloy sample which is in a sheet shape and has the mass of about 15mg, weighing the crucible and the sample in the sealing process, placing the crucible and the sample into DSC equipment after sealing, and using a temperature and heat correction file (namely, a conventional correction operation parameter electronic file built in thermal analysis equipment) of the sealed crucible. Other test procedures were consistent with conventional thermal analysis operations.
After the test, FeCl is used for sealing the sealing gasket of the crucible3The solution is dissolved, the inner crucible and the outer crucible can be repeatedly used, and the test cost is reduced.
The present invention is described in further detail below with reference to specific examples, which are intended to be illustrative of the invention and not limiting.
Example 1
A reusable nested sealed crucible, comprising: inner and outer crucibles 1 and 3, and a sealing gasket 2; the sealing gasket 2 is in a barrel shape, and the inner crucible 1, the outer crucible 3 and the sealing gasket 2 are in interference fit to form a sealing space.
Pure magnesium DSC, the specific tests include:
firstly, sealing the inner crucible and the outer crucible and a sealing gasket to form a reference crucible, and weighing the mass of the reference crucible; weighing the mass of the inner crucible, the mass of the outer crucible and the sealing gasket and the mass of the pure magnesium sample, and then sealing to form a sample crucible; respectively placing a reference crucible and a sample on a thermal analysis equipment bracket;
then, a test program is set up,
naming a test result file; opening the purge gas and starting the measurement; and opening the test result file and outputting the test result, which is shown in figure 2.
And finally, taking out the experimental crucible for standby after cleaning.
Example 2
The thermal analysis of the magnesium-aluminum-zinc alloy adopts the same crucible as that of the embodiment 1, and the specific test comprises the following steps:
firstly, sealing an inner crucible, an outer crucible and a sealing gasket to form a reference crucible, and weighing the mass of the reference crucible; weighing the mass of the inner crucible, the mass of the outer crucible and the sealing gasket and the mass of the pure magnesium sample, and then sealing to form a sample crucible; respectively placing a reference crucible and a sample on a thermal analysis equipment bracket;
then, a test program is set up,
naming a test result file; opening the purge gas and starting the measurement; and opening the test result file and outputting the test result.
And finally, taking out the experimental crucible for standby after cleaning.
Example 3
The thermal analysis of the AZ31 alloy, using the same crucible as in example 1, specifically tested the following:
firstly, sealing an inner crucible, an outer crucible and a sealing gasket to form a reference crucible, and weighing the mass of the reference crucible; weighing the mass of the inner crucible, the mass of the outer crucible and the sealing gasket and the mass of the pure magnesium sample, and then sealing to form a sample crucible; respectively placing a reference crucible and a sample on a thermal analysis equipment bracket;
then, a test program is set up,
naming a test result file; opening the purge gas and starting the measurement; and opening the test result file and outputting the test result.
And finally, taking out the experimental crucible for standby after cleaning.
Example 4
A reusable nested sealed crucible, comprising: inner and outer crucibles 1 and 3, and a sealing gasket 2; the sealing gasket 2 is in a barrel shape, and the inner crucible 1, the outer crucible 3 and the sealing gasket 2 are in interference fit to form a sealing space.
By adopting the thermal analysis method, the thermal analysis test for measuring the volatile and easily-oxidized alloy with easy operation, low cost and high precision can be realized, so that the thermal analysis becomes a conventional experimental means for magnesium alloy design. The DSC experimental effect of the magnesium alloy is basically consistent with that of the aluminum alloy.
Example 5
A reusable nested sealed crucible, comprising: inner and outer crucibles 1 and 3, and a sealing gasket 2; the sealing gasket 2 is in a barrel shape, and the inner crucible 1, the outer crucible 3 and the sealing gasket 2 are in interference fit to form a sealing space.
The inner crucible 1 is sleeved in the sealing gasket 2 so as to put the sample into the inner crucible for subsequent detection.
Example 6
A reusable nested sealed crucible, comprising: inner and outer crucibles 1 and 3, and a sealing gasket 2; the sealing gasket 2 is in a barrel shape, and the inner crucible 1, the outer crucible 3 and the sealing gasket 2 are in interference fit to form a sealing space.
The outer crucible 3 is sleeved outside the sealing gasket 2. The outer crucible is pressed from the top down to form a sealed space.
Example 7
A reusable nested sealed crucible, comprising: inner and outer crucibles 1 and 3, and a sealing gasket 2; the sealing gasket 2 is in a barrel shape, and the inner crucible 1, the outer crucible 3 and the sealing gasket 2 are in interference fit to form a sealing space.
The bottom of the outer crucible 3 is a round angle. The sealing area is increased, and the friction force between the crucible and the gasket is increased.
Example 8
A reusable nested sealed crucible, comprising: inner and outer crucibles 1 and 3, and a sealing gasket 2; the sealing gasket 2 is in a barrel shape, and the inner crucible 1, the outer crucible 3 and the sealing gasket 2 are in interference fit to form a sealing space.
The inner crucible 1 and the outer crucible 3 are made of tantalum sheets. In the temperature rise process, because the expansion rate of the tantalum crucible is far lower than that of the copper sealing gasket, the sealed pressure bearing of the crucible exceeds 4 atmospheric pressures in the test process, and the sealing gas in the crucible only forms 3 atmospheric pressures in the temperature rise process in the test process.
Example 9
A reusable nested sealed crucible, comprising: inner and outer crucibles 1 and 3, and a sealing gasket 2; the sealing gasket 2 is in a barrel shape, and the inner crucible 1, the outer crucible 3 and the sealing gasket 2 are in interference fit to form a sealing space.
The inner crucible 1 and the outer crucible 3 are made of tantalum sheets. The purity of the tantalum sheet is more than 99.7. So that the crucible and the test sample elements do not react.
Example 10
A reusable nested sealed crucible, comprising: inner and outer crucibles 1 and 3, and a sealing gasket 2; the sealing gasket 2 is in a barrel shape, and the inner crucible 1, the outer crucible 3 and the sealing gasket 2 are in interference fit to form a sealing space.
The sealing gasket 2 is made of red copper. The expansion rate of the sealing gasket is far greater than that of the tantalum crucible, so that the sealing effect is improved, volatilization is inhibited, and the precision of measuring the thermophysical parameters is improved.
It should be noted that the above-mentioned embodiments are only preferred embodiments of the present invention, and the present invention is not limited thereto, and although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications and equivalents can be made in the technical solutions described in the foregoing embodiments, or equivalents thereof. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention. Although the present invention has been described with reference to the specific embodiments, it should be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention.
Claims (10)
1. A reusable nested sealed crucible, comprising: inner and outer crucibles and a sealing gasket; the sealing gasket is barrel-shaped, and the inner crucible, the outer crucible and the sealing gasket are in interference fit to form a sealing space.
2. The reusable nested sealed crucible of claim 1, wherein the inner crucible is nested within the sealing gasket.
3. The reusable nested sealed crucible of claim 1, wherein the outer crucible is nested outside the sealing gasket.
4. The reusable nested sealed crucible of claim 1, wherein the outer crucible bottom is rounded.
5. The reusable nested sealed crucible of claim 1, wherein the inner and outer crucibles are comprised of tantalum sheets.
6. The reusable nested sealed crucible of claim 5, wherein the tantalum pieces have a purity of 99.7 or greater.
7. A reusable nested sealed crucible as claimed in claim 1 wherein the sealing gasket is made of red copper.
8. A method of testing the sealing of a reusable nested sealed crucible as claimed in any one of claims 1 to 7, comprising:
pressing the inner crucible into the sealing gasket, then putting the sample into the inner crucible, and pressing the outer crucible from top to bottom to form a sealed space, thus obtaining the product.
9. A thermal analysis method for testing a volatile and easily-oxidized alloy material is characterized by comprising the following steps:
using the reusable nested sealed crucible of any one of claims 1-7 as a reference crucible;
pressing the inner crucible into the sealing gasket, then putting the sample into the inner crucible, and pressing the outer crucible from top down to form a sealed space; respectively weighing the crucible, the sealing gasket and the sample;
and (3) putting the sealed crucible into DSC equipment, and carrying out thermal analysis by using the temperature and heat correction file of the sealed crucible disclosed by the invention.
10. A method for recycling a reusable nested sealed crucible according to any one of claims 1 to 7, wherein FeCl is added after the thermal analysis test is finished3The solution dissolves the sealing gasket and collects the inner crucible and the outer crucible, thus being capable of being repeatedly used.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116046653A (en) * | 2022-12-08 | 2023-05-02 | 中国兵器装备集团西南技术工程研究所 | Method for predicting response of corrosion performance of microalloyed magnesium alloy to heat treatment |
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