CN110064454A - Magnesium alloy in course of solidification experiment crucible and packaging method under synchrotron radiation state - Google Patents
Magnesium alloy in course of solidification experiment crucible and packaging method under synchrotron radiation state Download PDFInfo
- Publication number
- CN110064454A CN110064454A CN201910438320.8A CN201910438320A CN110064454A CN 110064454 A CN110064454 A CN 110064454A CN 201910438320 A CN201910438320 A CN 201910438320A CN 110064454 A CN110064454 A CN 110064454A
- Authority
- CN
- China
- Prior art keywords
- crucible
- potsherd
- graphite crucible
- magnesium alloy
- sample
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 229910000861 Mg alloy Inorganic materials 0.000 title claims abstract description 35
- 238000007711 solidification Methods 0.000 title claims abstract description 17
- 230000008023 solidification Effects 0.000 title claims abstract description 17
- 238000002474 experimental method Methods 0.000 title claims abstract description 15
- 238000000034 method Methods 0.000 title claims abstract description 15
- 230000005469 synchrotron radiation Effects 0.000 title claims abstract description 13
- 238000004806 packaging method and process Methods 0.000 title abstract description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 58
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 58
- 239000010439 graphite Substances 0.000 claims abstract description 58
- 239000003292 glue Substances 0.000 claims abstract description 39
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000005864 Sulphur Substances 0.000 claims abstract description 12
- 239000000843 powder Substances 0.000 claims abstract description 12
- 238000005538 encapsulation Methods 0.000 claims abstract description 9
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 8
- 238000004026 adhesive bonding Methods 0.000 claims description 4
- 238000005498 polishing Methods 0.000 claims description 3
- 239000004575 stone Substances 0.000 claims description 3
- 229910052571 earthenware Inorganic materials 0.000 claims description 2
- 238000007254 oxidation reaction Methods 0.000 abstract description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 4
- 229910052760 oxygen Inorganic materials 0.000 abstract description 4
- 239000001301 oxygen Substances 0.000 abstract description 4
- 230000008569 process Effects 0.000 description 5
- 238000003384 imaging method Methods 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 2
- 229920001651 Cyanoacrylate Polymers 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 239000004830 Super Glue Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000010429 evolutionary process Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000010921 in-depth analysis Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 238000004382 potting Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000001360 synchronised effect Effects 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
- B01L3/00—Containers or dishes for laboratory use, e.g. laboratory glassware; Droppers
- B01L3/04—Crucibles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
- B01L2300/00—Additional constructional details
- B01L2300/04—Closures and closing means
Landscapes
- Health & Medical Sciences (AREA)
- Clinical Laboratory Science (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Analysing Materials By The Use Of Radiation (AREA)
Abstract
The invention discloses magnesium alloy in course of solidification experiment crucible and packaging methods under a kind of synchrotron radiation state, including potsherd I (1), graphite crucible (2), potsherd II (3), crucible protects glue frame (4) and inorganic fill layer (5), the graphite crucible (2) is equipped with sample cavity (6), sample is placed in sample cavity (6) and places sulphur powder in the gap of sample and sample cavity, graphite crucible (2) is arranged in potsherd I (1) upper surface, and crucible protection glue frame (4) is enclosed on the outside of graphite crucible (2), gap location in potsherd I (1) Yu graphite crucible (2) is equipped with inorganic fill layer (5), potsherd II (3) is covered on potsherd I (1) and is compacted graphite crucible (2).Sulphur powder is placed in graphite crucible and effectively removes residual oxygen, and the vapour pressure of generation inhibits magnesium alloy volatilization, solves magnesium alloy high-temperature oxydation, the difficult technical problem of sample encapsulation.
Description
Technical field
The present invention relates to a kind of crucibles, in particular under synchrotron radiation state magnesium alloy in course of solidification experiment with crucible and its
Packaging method.
Background technique
Using synchrotron radiation imaging technique in-situ observation magnesium alloy solidification Microstructural Evolution process, magnesium alloy can be related to
Fusing and solidification.And magnesium alloy easily aoxidizes, this just brings challenge to the encapsulation of sample.Conventional package is not easy to make with crucible
Standby, encapsulation step and method are relatively complicated, and leakproofness is poor, often result in sample in heating process and aoxidize, seriously affect
Imaging results；Meanwhile the sample damage after imaging is also caused, it is difficult to carry out other Experimental Characterizations again, is later period further investigated
Certain difficulty is caused with the microscopic feature of analysis sample.
Summary of the invention
To overcome the shortcomings of that existing crucible is oxidizable cumbersome with encapsulation for magnesium alloy, the present invention provides a kind of synchronous spoke
Penetrate magnesium alloy in course of solidification experiment crucible and its packaging method under state.Experiment is improved with crucible on the original basis
And optimization, so that crucible preparation process is simply quick, sample potting is good and economic and practical, complete after guaranteeing sample imaging
While whole property, it is more conducive to the observation and in-depth analysis of magnesium alloy microstructures evolutionary process.
In order to solve the above technical problems, the technical solution adopted in the present invention is as follows:
Magnesium alloy in course of solidification experiment crucible under a kind of synchrotron radiation state, including potsherd I, graphite crucible, potsherd II,
Crucible protects glue frame and inorganic fill layer, and the potsherd I and potsherd II are alumina ceramic plate.The crucible protective glue
Frame is the inorganic high-temperature resistant glue frame formed by inorganic high-temperature resistant glue, for protecting graphite crucible；The inorganic fill layer is inorganic
The inorganic fill layer that high-temperature plastic is formed.
The graphite crucible is equipped with sample cavity, and sample is placed in sample cavity and places in the gap of sample and sample cavity
Sulphur powder, the present invention in, magnesium alloy print shape be isometrical T-type, size as the sample cavity of graphite crucible, with a thickness of
0.5mm。
Graphite crucible is arranged in I upper surface of potsherd, and crucible protection glue frame is enclosed on the outside of graphite crucible, is making pottery
The gap location of tile I and graphite crucible is equipped with inorganic fill layer, and potsherd II is covered on potsherd I and by graphite crucible pressure
It is real.The sulphur powder placed in graphite crucible effectively removes residual oxygen, and the vapour pressure of generation inhibits magnesium alloy volatilization, solves magnesium and closes
The technical issues of golden high-temperature oxydation.
The magnesium alloy in course of solidification experiment packaging method of crucible under a kind of synchrotron radiation state, steps are as follows:
Step 1 by graphite crucible with super gluing in the centre of potsherd I, and is placed 2 minutes at room temperature.
Step 2 smears one layer of inorganic high-temperature resistant glue on the outside of graphite crucible and forms a crucible protection glue frame to protect stone
Black crucible is placed 5 minutes at room temperature, and crucible protects the thickness of glue frame less than the thickness of graphite crucible.
The magnesium alloy print of polishing both surfaces is put into the sample cavity of graphite crucible by step 3.
Step 4 is put into sulphur powder in the gap of magnesium alloy print and sample cavity.
The blank space of potsherd I is uniformly smeared inorganic high-temperature resistant glue, and potsherd II is symmetrically covered in ceramics by step 5
Piece I, compacted graphite crucible, and place 4 ~ 8 hours at room temperature and complete encapsulation, and in compacting process, inorganic high-temperature resistant
The stomata that glue generates carries out curing process at room temperature.
The medicine have the advantages that the graphite crucible in the present invention is hollow type, it is placed in the identical oxidation of two chip sizes
Between aluminium potsherd, the hollow type cavity of graphite crucible places sulphur powder, between graphite crucible and two panels alumina ceramic plate
It is filled with inorganic high-temperature resistant glue in gap.Graphite crucible first uses super gluing among a piece of alumina ceramic plate, with graphite frame earthenware
The identical magnesium alloy sample of crucible cavity type size is placed in graphite crucible, smears one layer of inorganic high-temperature resistant glue in graphite crucible surrounding
An inorganic high-temperature resistant glue frame is formed to protect graphite crucible, thickness is slightly less than graphite crucible thickness, aluminium oxide is made pottery after solidification
Remaining place of tile, which uniformly applies, spreads inorganic high-temperature resistant glue, and another piece aluminum oxide potsherd is covered, is compacted.It is put in graphite crucible
It sets sulphur powder and effectively removes residual oxygen, the vapour pressure of generation inhibits magnesium alloy volatilization, solves magnesium alloy high-temperature oxydation, sample envelope
Fill difficult technical problem.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
Some embodiments of invention for those of ordinary skill in the art without creative efforts, can be with
It obtains other drawings based on these drawings.
Fig. 1 is unencapsulated structural schematic diagram of the invention.
Fig. 2 is the side view after present invention encapsulation.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, those of ordinary skill in the art are obtained every other under that premise of not paying creative labor
Embodiment shall fall within the protection scope of the present invention.
Embodiment 1: magnesium alloy in course of solidification experiment crucible under a kind of synchrotron radiation state, as shown in Figs. 1-2, including pottery
Tile I 1, graphite crucible 2, potsherd II 3, crucible protection glue frame 4 and inorganic fill layer 5, the potsherd I 1 and potsherd II 3
It is alumina ceramic plate.The crucible protection glue frame 4 is the inorganic high-temperature resistant glue frame formed by inorganic high-temperature resistant glue, for protecting
Protect graphite crucible；The inorganic fill layer 5 is the inorganic fill layer that inorganic high-temperature resistant glue is formed.
The graphite crucible 2 is equipped with sample cavity 6, and sample is placed in sample cavity 6 and in the gap of sample and sample cavity
Place sulphur powder, the present invention in, magnesium alloy print shape be isometrical T-type, size as the sample cavity of graphite crucible, with a thickness of
0.5mm。
Graphite crucible 2 is arranged in I 1 upper surface of potsherd, and is enclosed with crucible protection glue frame 4 in the outside of graphite crucible 2,
Inorganic fill layer 5 is equipped in the gap location of potsherd I 1 and graphite crucible 2, and potsherd II 3 is covered on potsherd I 1 and by stone
Black crucible 2 is compacted.The sulphur powder placed in graphite crucible effectively removes residual oxygen, and the vapour pressure of generation inhibits magnesium alloy to wave
The technical issues of hair, solution magnesium alloy high-temperature oxydation.
Embodiment 2: the magnesium alloy in course of solidification experiment packaging method of crucible under a kind of synchrotron radiation state, step is such as
Under:
Step 1 by graphite crucible 2 with super gluing in the centre of potsherd I 1, and is placed 2 minutes at room temperature.The present invention makes
Super glue does not react with molten metal.
Step 2 smears one layer of inorganic high-temperature resistant glue on the outside of graphite crucible 2 and forms a crucible protection glue frame 4 to protect
Graphite crucible 2 is placed 5 minutes at room temperature, and crucible protects the thickness of glue frame 4 less than the thickness of graphite crucible.Inorganic high-temperature resistant glue
800 DEG C or more high temperature can be born, does not react with magnesium alloy, seals after solidification.
The magnesium alloy print of polishing both surfaces is put into the sample cavity 6 of graphite crucible 2 by step 3.
Step 4 is put into sulphur powder in the gap of magnesium alloy print and sample cavity 6.
The blank space of potsherd I 1 is uniformly smeared inorganic high-temperature resistant glue by step 5, and by the symmetrical Gai Tao of potsherd II 3
Tile I 1, compacted graphite crucible 2, and place 4 ~ 8 hours at room temperature and complete encapsulation, it is placed 6 hours in the present embodiment, and
In compacting process, the stomata that inorganic high-temperature resistant glue generates carries out curing process at room temperature.
The graphite crucible and inorganic high-temperature resistant glue frame that the present invention uses play fixed and sealing function, sample cavity configuration and are avoided that
Influence of the graphite to X-ray improves the photo contrast that experiment obtains.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
In the technical scope disclosed by the present invention, any changes or substitutions that can be easily thought of by anyone skilled in the art,
It should be covered by the protection scope of the present invention.
Claims (4)
1. magnesium alloy in course of solidification experiment crucible under a kind of synchrotron radiation state, it is characterised in that: including potsherd I (1), stone
Black crucible (2), potsherd II (3), crucible protection glue frame (4) and inorganic fill layer (5), the graphite crucible (2) are equipped with sample
Chamber (6), sample are placed in sample cavity (6) and place in the gap of sample and sample cavity sulphur powder, graphite crucible (2) setting
In potsherd I (1) upper surface, and be enclosed on the outside of graphite crucible (2) crucible protection glue frame (4), potsherd I (1) with
The gap location of graphite crucible (2) is equipped with inorganic fill layer (5), and potsherd II (3) is covered on potsherd I (1) and by graphite earthenware
Crucible (2) compacting.
2. magnesium alloy in course of solidification experiment crucible under synchrotron radiation state according to claim 1, it is characterised in that: institute
Stating potsherd I (1) and potsherd II (3) is alumina ceramic plate.
3. magnesium alloy in course of solidification experiment crucible, feature exist under synchrotron radiation state according to claim 1 or 2
In: crucible protection glue frame (4) is the inorganic high-temperature resistant glue frame formed by inorganic high-temperature resistant glue；The inorganic fill layer (5)
The inorganic fill layer formed for inorganic high-temperature resistant glue.
4. the magnesium alloy in course of solidification experiment encapsulation side of crucible under synchrotron radiation state according to claim 1 or 2 or 3
Method, steps are as follows:
Step 1 by graphite crucible (2) with super gluing in the centre of potsherd I (1), and is placed 2 minutes at room temperature；
Step 2 smears one layer of inorganic high-temperature resistant glue on the outside of graphite crucible (2) and forms crucible protection glue frame (4) to protect
Graphite crucible (2) is placed 5 minutes at room temperature, and crucible protects the thickness of glue frame (4) less than the thickness of graphite crucible；
The magnesium alloy print of polishing both surfaces is put into the sample cavity (6) of graphite crucible (2) by step 3；
Step 4 is put into sulphur powder in the gap of magnesium alloy print Yu sample cavity (6)；
The blank space of potsherd I (1) is uniformly smeared inorganic high-temperature resistant glue by step 5, and by the symmetrical Gai Tao of potsherd II (3)
Tile I (1), compacted graphite crucible (2), and encapsulation is completed after placing 4 ~ 8 hours at room temperature.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910438320.8A CN110064454A (en) | 2019-05-24 | 2019-05-24 | Magnesium alloy in course of solidification experiment crucible and packaging method under synchrotron radiation state |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910438320.8A CN110064454A (en) | 2019-05-24 | 2019-05-24 | Magnesium alloy in course of solidification experiment crucible and packaging method under synchrotron radiation state |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110064454A true CN110064454A (en) | 2019-07-30 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910438320.8A Pending CN110064454A (en) | 2019-05-24 | 2019-05-24 | Magnesium alloy in course of solidification experiment crucible and packaging method under synchrotron radiation state |
Country Status (1)
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| CN (1) | CN110064454A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112717850A (en) * | 2020-12-11 | 2021-04-30 | 郑州轻工业大学 | Pocket-sized multifunctional alloy solidification heating table and use method thereof |
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|---|---|---|---|---|
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| CN103071780A (en) * | 2013-01-15 | 2013-05-01 | 西北工业大学 | Crucible for magnesium alloy directional solidification and preparation method of crucible |
| CN105413774A (en) * | 2015-12-03 | 2016-03-23 | 西北工业大学 | Crucible for magnesium alloy solidification synchrotron radiation real-time imaging study and preparation method of crucible |
| CN105651578A (en) * | 2016-04-01 | 2016-06-08 | 扬州大学 | Method for preparing synchrotron-radiation X-ray absorption fine-structure test sample of hydrogen storage material |
| CN209968441U (en) * | 2019-05-24 | 2020-01-21 | 郑州轻工业学院 | Crucible for magnesium alloy solidification process experiment under synchrotron radiation state |
-
2019
- 2019-05-24 CN CN201910438320.8A patent/CN110064454A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2010140352A1 (en) * | 2009-06-02 | 2010-12-09 | ジャパンスーパークォーツ株式会社 | Lid for fused quartz crucible, fused quartz crucible and method for handling same |
| CN103071780A (en) * | 2013-01-15 | 2013-05-01 | 西北工业大学 | Crucible for magnesium alloy directional solidification and preparation method of crucible |
| CN105413774A (en) * | 2015-12-03 | 2016-03-23 | 西北工业大学 | Crucible for magnesium alloy solidification synchrotron radiation real-time imaging study and preparation method of crucible |
| CN105651578A (en) * | 2016-04-01 | 2016-06-08 | 扬州大学 | Method for preparing synchrotron-radiation X-ray absorption fine-structure test sample of hydrogen storage material |
| CN209968441U (en) * | 2019-05-24 | 2020-01-21 | 郑州轻工业学院 | Crucible for magnesium alloy solidification process experiment under synchrotron radiation state |
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| Title |
|---|
| 朱洪法: "《催化剂手册》", 31 August 2008, 金盾出版社, pages: 104 - 105 * |
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| CN112717850A (en) * | 2020-12-11 | 2021-04-30 | 郑州轻工业大学 | Pocket-sized multifunctional alloy solidification heating table and use method thereof |
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