CN105413774A - Crucible for magnesium alloy solidification synchrotron radiation real-time imaging study and preparation method of crucible - Google Patents

Crucible for magnesium alloy solidification synchrotron radiation real-time imaging study and preparation method of crucible Download PDF

Info

Publication number
CN105413774A
CN105413774A CN201510874462.0A CN201510874462A CN105413774A CN 105413774 A CN105413774 A CN 105413774A CN 201510874462 A CN201510874462 A CN 201510874462A CN 105413774 A CN105413774 A CN 105413774A
Authority
CN
China
Prior art keywords
crucible
ludox
graphite
graphite paper
mixture
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.)
Granted
Application number
CN201510874462.0A
Other languages
Chinese (zh)
Other versions
CN105413774B (en
Inventor
罗时峰
杨光昱
刘少军
肖磊
介万奇
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Northwestern Polytechnical University
Original Assignee
Northwestern Polytechnical University
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Northwestern Polytechnical University filed Critical Northwestern Polytechnical University
Priority to CN201510874462.0A priority Critical patent/CN105413774B/en
Publication of CN105413774A publication Critical patent/CN105413774A/en
Application granted granted Critical
Publication of CN105413774B publication Critical patent/CN105413774B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01LCHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L3/00Containers or dishes for laboratory use, e.g. laboratory glassware; Droppers
    • B01L3/04Crucibles

Landscapes

  • Health & Medical Sciences (AREA)
  • Clinical Laboratory Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Particle Accelerators (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

The invention discloses a crucible for magnesium alloy solidification synchrotron radiation real-time imaging study and a preparation method of the crucible, and is used for solving the technical problem that the crucible for magnesium alloy is likely to oxidize. According to the technical scheme, the crucible comprises a graphite frame, corundum sheets, a piece of graphite paper, a mixture of zircon powder and silicon sol and a high-temperature-resistant inorganic CPS adhesive, wherein the graphite paper is hollow and is arranged between two corundum sheets identical in size, sulfur powder is arranged in a hollow cavity of the graphite paper, and a gap between the graphite paper and each corundum sheet is filled with the mixture of zircon powder and silicon sol; after being assembled, the graphite paper and the two corundum sheets are arranged into the hollow graphite frame with a groove, the periphery of the graphite paper and the groove of the graphite frame is filled with the mixture of zircon powder and silicon sol, and the graphite paper and the graphite frame are coated with the high-temperature-resistant inorganic CPS adhesive after being cured. By adopting the crucible, the magnesium alloy is completely isolated from the air, the sulfur powder can remove residual oxygen in the crucible, and the generated vapor pressure inhibits the volatilization of the magnesium alloy, so that the technical problem that the magnesium alloy is oxidized at a high temperature is solved.

Description

Magnesium alloy in course of solidification synchrotron radiation real time imagery research crucible and preparation method thereof
Technical field
The present invention relates to a kind of crucible, particularly a kind of magnesium alloy in course of solidification synchrotron radiation real time imagery research crucible.Also relate to the preparation method of this crucible.
Background technology
With reference to Fig. 5, document " " metal alloy solidifies the research of dendritic growth synchrotron radiation real time imagery " [D] is permitted lush Dalian University of Technology master thesis 2010.06p19-20 " discloses one and solidifies synchrotron radiation real time imagery crucible for metal alloy, comprise quartz glass plate 6, ptfe sheet 7 and clip 8, the ptfe sheet 7 of hollow belt groove is clipped in two panels quartz glass plate 6, clamps outside quartz glass plate 6 with clip 8.This crucible can not completely cut off the contact of technic metal and oxygen, is only applicable to the metal alloy that high temperature is not oxidizable, as Al alloy, Sn-Pb alloy etc.But Mg-based hydrogen storage character is very active, chemical reaction can be there is with many metals or nonmetal and oxide etc., very easily oxidized under high temperature.Therefore, the alloy that this crucible is oxidizable under can not being applicable to the high temperature such as Mg-based hydrogen storage.
Summary of the invention
In order to overcome the deficiency that existing crucible is easily oxidized for magnesium alloy, the invention provides a kind of magnesium alloy in course of solidification synchrotron radiation real time imagery research crucible.This crucible comprises mixture and the high temperature resistant inorganic CPS glue of graphite frame, corundum sheet, graphite paper, zirconium English powder and Ludox.Described graphite paper is hollow type, is placed between the measure-alike corundum sheet of two panels, and place Cosan in the hollow type cavity of graphite paper, the space between graphite paper and two panels corundum sheet uses the mixture of zirconium English powder and Ludox to fill.Put into the graphite frame of hollow belt groove after graphite paper and two panels corundum sheet assemble, the groove vicinity of graphite paper and graphite frame is filled with the mixture of zirconium English powder and Ludox, is coated with one deck high temperature resistant inorganic CPS glue after solidification again.The present invention adopts BN spray coated corundum sheet and graphite paper, and magnesium alloy can not be reacted with corundum sheet and graphite paper; The mixture of zirconium English powder and Ludox and the double-layer seal of high temperature resistant inorganic CPS glue, make magnesium alloy and air completely isolated; Crucible inside is put into appropriate Cosan and can be consumed residual oxygen; the not oxidated pollution of sulphur dioxide reduction gas shield magnesium alloy produced; at high temperature can also produce certain vapour pressure; suppress the volatilization of magnesium alloy; by multilayer proofing technology, solve the technical problem of magnesium alloy high-temperature oxydation.
The present invention also provides the preparation method of above-mentioned crucible.
The technical solution adopted for the present invention to solve the technical problems is: a kind of magnesium alloy in course of solidification synchrotron radiation real time imagery research crucible, is characterized in: the mixture 4 and the high temperature resistant inorganic CPS glue 5 that comprise graphite frame 1, corundum sheet 2, graphite paper 3, zirconium English powder and Ludox.Described graphite paper 3 is hollow types, is placed between the measure-alike corundum sheet 2 of two panels, and place Cosan in the hollow type cavity of graphite paper 3, the space between graphite paper 3 and two panels corundum sheet 2 uses the mixture 4 of zirconium English powder and Ludox to fill.Put into the graphite frame 1 of hollow belt groove after graphite paper 3 and two panels corundum sheet 2 assemble, graphite paper 3 is filled with the groove vicinity zirconium English powder of graphite frame 1 and the mixture 4 of Ludox, is coated with one deck high temperature resistant inorganic CPS glue 5 after solidification again.
A preparation method for above-mentioned crucible, is characterized in comprising the following steps:
Step one, on corundum sheet 2 with graphite paper 3, spray one deck BN spray, at room temperature place 2 minutes.
Step 2, by zirconium English powder and Ludox mixing and stirring, make the mixture 4 of zirconium English powder and Ludox, modulation ratio is that 4 ~ 5g zirconium English powder joined by 1mL Ludox.
Step 3, the magnesium alloy thin slice of equal for two sides polishing is put into the graphite paper 3 of hollow, clamp with two panels corundum sheet 2.Void area around magnesium alloy thin slice and graphite paper 3 puts into Cosan, fills the mixture 4 of zirconium English powder and Ludox subsequently on corundum sheet 2 four limit.
Step 4, graphite paper 3 put into the graphite frame 1 of hollow belt groove after assembling with two panels corundum sheet 2, graphite paper 3 is filled with the groove vicinity zirconium English powder of graphite frame 1 and the mixture 4 of Ludox, at room temperature makes the mixture 4 of zirconium English powder and Ludox solidify.
Mixture 4 surface of step 5, zirconium English powder after hardening and Ludox is coated with last layer high temperature resistant inorganic CPS glue 5, solidifies the pore produced, be at room temperature cured process for the mixture 4 sealing zirconium English powder and Ludox.
Described magnesium alloy thin chip size is 35*15* (0.15 ~ 0.2) mm.
The invention has the beneficial effects as follows: this crucible comprises mixture and the high temperature resistant inorganic CPS glue of graphite frame, corundum sheet, graphite paper, zirconium English powder and Ludox.Described graphite paper is hollow type, is placed between the measure-alike corundum sheet of two panels, and place Cosan in the hollow type cavity of graphite paper, the space between graphite paper and two panels corundum sheet uses the mixture of zirconium English powder and Ludox to fill.Put into the graphite frame of hollow belt groove after graphite paper and two panels corundum sheet assemble, the groove vicinity of graphite paper and graphite frame is filled with the mixture of zirconium English powder and Ludox, is coated with one deck high temperature resistant inorganic CPS glue after solidification again.The present invention adopts BN spray coated corundum sheet and graphite paper, and magnesium alloy can not be reacted with corundum sheet and graphite paper; The mixture of zirconium English powder and Ludox and the double-layer seal of high temperature resistant inorganic CPS glue, make magnesium alloy and air completely isolated; Crucible inside is put into appropriate Cosan and can be consumed residual oxygen; the not oxidated pollution of sulphur dioxide reduction gas shield magnesium alloy produced; at high temperature can also produce certain vapour pressure; suppress the volatilization of magnesium alloy; by multilayer proofing technology, solve the technical problem of magnesium alloy high-temperature oxydation.
The present invention is described in detail below in conjunction with drawings and Examples.
Accompanying drawing explanation
Fig. 1 is the structural representation of crucible of the present invention.
Fig. 2 is the crucible using the present invention to prepare, the photomacrograph after Mg-28wt.%Gd thin slice heating remelting.
Fig. 3 is the crucible using the present invention to prepare, and Mg-28wt.%Gd thin slice is at G=6K/mm, and cooldown rate is the synchrotron radiation video interception under 5K/s.
Fig. 4 is the crucible using the present invention to prepare, and Mg-28wt.%Gd thin slice is at G=12K/mm, and cooldown rate is the synchrotron radiation video interception under 5K/s.
Fig. 5 is that technical background solidifies the structural representation of synchrotron radiation real time imagery crucible for metal alloy.
In figure, 1-graphite frame, 2-corundum sheet, 3-graphite paper, the mixture of 4-zirconium English powder and Ludox, 5-high temperature resistant inorganic CPS glue, 6-quartz glass plate, 7-ptfe sheet, 8-clip.
Detailed description of the invention
Following examples are with reference to Fig. 1-4.
Embodiment 1: the present invention is magnesium alloy in course of solidification synchrotron radiation real time imagery research crucible and preparation method thereof.Crucible comprises mixture 4 and the high temperature resistant inorganic CPS glue 5 of graphite frame 1, corundum sheet 2, graphite paper 3 thin slice of hollow, zirconium English powder and Ludox.The graphite paper thin slice 3 of hollow is placed between the measure-alike corundum sheet 2 of two panels, and puts into appropriate Cosan in this cavity, and space around uses the pasty mixture 4 of zirconium English powder and Ludox to fill.This entirety is being put into the graphite frame 1 of hollow belt groove, the mixture 4 of surrounding zirconium English powder and Ludox is filled, and is coated with last layer high temperature resistant inorganic CPS glue 5 after solidification around it.
The above-mentioned preparation method for magnesium alloy in course of solidification synchrotron radiation real time imagery research crucible is:
(1) the graphite paper interlayer between corundum sheet and corundum sheet sprays one deck BN spray, at room temperature place about 2 minutes, can use after its bone dry;
(2) by zirconium English powder and Ludox mixing and stirring to pasty state, give over to encapsulant and use, modulation ratio is that 1mL Ludox is about 4.5g zirconium English powder;
(3) the Mg-28wt.%Gd alloy sheet of equal for two sides polishing is put into the graphite paper of hollow, Mg-28wt.%Gd alloy sheet is of a size of 35*15*0.2mm, is clamped with two panels corundum sheet, forms sandwich structure.Void area around Mg-28wt.%Gd alloy sheet and graphite paper puts into appropriate Cosan, fills the mixture of zirconium English powder and Ludox subsequently, tamped by hole on corundum sheet four limit;
(4) said structure is put into the graphite frame of hollow, fill out the mixture of zirconium English powder and Ludox on graphite frame four limit, sample and outside air are isolated, at room temperature makes the mixture solidified of zirconium English powder and Ludox;
(5) be coated with last layer high temperature resistant inorganic CPS glue at the zirconium English powder of solidification and the surface of Ludox mixture, impregnation ratio is that 1mL liquid phase is about 4.5g solid phase, for sealing zirconium English powder and Ludox solidifies the pore produced, is at room temperature cured process.
Packaged Mg-28wt.%Gd alloy sheet is placed in resistance furnace and is heated to 700 DEG C, with stove cooling after insulation 30min, when temperature is down to 500 DEG C, take out sample.Fig. 2 is the photomacrograph of Mg-28wt.%Gd alloy sheet remelting after coagulation prepared by embodiment 1 method.Before experiment, the quality of sample is 0.1411g, and after test, the quality of sample is 0.1501g, shows that sample oxidation is less, only has the sample of tiny area and oxygen to there occurs reaction; Meanwhile, before experiment, the thickness bottom sample is 0.18mm, slightly thickening, and this creates sinking because liquation is subject to Action of Gravity Field.
Embodiment 2: the present invention is magnesium alloy in course of solidification synchrotron radiation real time imagery research crucible and preparation method thereof.Crucible comprises mixture 4 and the high temperature resistant inorganic CPS glue 5 of graphite frame 1, corundum sheet 2, graphite paper 3 thin slice of hollow, zirconium English powder and Ludox.The graphite paper thin slice 3 of hollow is placed between the measure-alike corundum sheet 2 of two panels, and puts into appropriate Cosan in this cavity, and space around uses the pasty mixture 4 of zirconium English powder and Ludox to fill.This entirety is being put into the graphite frame 1 of hollow belt groove, the mixture 4 of surrounding zirconium English powder and Ludox is filled, and is coated with last layer high temperature resistant inorganic CPS glue 5 after solidification around it.
The above-mentioned preparation method for magnesium alloy in course of solidification synchrotron radiation real time imagery research crucible is:
(1) the graphite paper interlayer between corundum sheet and corundum sheet sprays one deck BN spray, at room temperature place about 2 minutes, can use after its bone dry;
(2) by zirconium English powder and Ludox mixing and stirring to pasty state, give over to encapsulant and use, modulation ratio is that 1mL Ludox is about 4g zirconium English powder;
(3) the Mg-28wt.%Gd alloy sheet of equal for two sides polishing is put into the graphite paper of hollow, Mg-28wt.%Gd alloy sheet is of a size of 35*15*0.2mm, is clamped with two panels corundum sheet, forms sandwich structure.Void area around Mg-28wt.%Gd alloy sheet and graphite paper puts into appropriate Cosan, fills the mixture of zirconium English powder and Ludox subsequently, tamped by hole on corundum sheet four limit;
(4) said structure is put into the graphite frame of hollow, fill out the mixture of zirconium English powder and Ludox on graphite frame four limit, Mg-28wt.%Gd alloy sheet and outside air are isolated, at room temperature makes the mixture solidified of zirconium English powder and Ludox;
(5) be coated with last layer high temperature resistant inorganic CPS glue at the zirconium English powder of solidification and the surface of Ludox mixture, impregnation ratio is that 1mL liquid phase is about 4.5g solid phase, for sealing zirconium English powder and Ludox solidifies the pore produced, is at room temperature cured process.
Packaged Mg-28wt.%Gd alloy sheet is placed on heat fused in directional solidification furnace, thermograde is set to 6K/mm, close heating power supply after insulation 30min, the stove up and down of directional solidification furnace is cooled with the cooldown rate of 5K/s, observe the process of setting of Mg-28wt.%Gd alloy sheet.Fig. 3 is Mg-28wt.%Gd alloy sheet prepared by embodiment 2 method synchrotron radiation video interception when solidifying.Can see, the secondary dendrite of this alloy and once interdendritic angle are 60 °, and primary tiller crystals growth direction and thermograde direction are departed to some extent.
Embodiment 3: the present invention is magnesium alloy in course of solidification synchrotron radiation real time imagery research crucible and preparation method thereof.Crucible comprises mixture 4 and the high temperature resistant inorganic CPS glue 5 of graphite frame 1, corundum sheet 2, graphite paper 3 thin slice of hollow, zirconium English powder and Ludox.The graphite paper thin slice 3 of hollow is placed between the measure-alike corundum sheet 2 of two panels, and puts into appropriate Cosan in this cavity, and space around uses the pasty mixture 4 of zirconium English powder and Ludox to fill.This entirety is being put into the graphite frame 1 of hollow belt groove, the mixture 4 of surrounding zirconium English powder and Ludox is filled, and is coated with last layer high temperature resistant inorganic CPS glue 5 after solidification around it.
The above-mentioned preparation method for magnesium alloy in course of solidification synchrotron radiation real time imagery research crucible is:
(1) the graphite paper interlayer between corundum sheet and corundum sheet sprays one deck BN spray, at room temperature place about 2 minutes, can use after its bone dry;
(2) by zirconium English powder and Ludox mixing and stirring to pasty state, give over to encapsulant and use, modulation ratio is that 1mL Ludox is about 5g zirconium English powder;
(3) the Mg-28wt.%Gd alloy sheet of equal for two sides polishing is put into the graphite paper of hollow, Mg-28wt.%Gd alloy sheet is of a size of 35*15*0.2mm, is clamped with two panels corundum sheet, forms sandwich structure.Void area around Mg-28wt.%Gd alloy sheet and graphite paper puts into appropriate Cosan, fills the mixture of zirconium English powder and Ludox subsequently, tamped by hole on corundum sheet four limit;
(4) said structure is put into the graphite frame of hollow, fill out the mixture of zirconium English powder and Ludox on graphite frame four limit, Mg-28wt.%Gd alloy sheet and outside air are isolated, at room temperature makes the mixture solidified of zirconium English powder and Ludox;
(5) be coated with last layer high temperature resistant inorganic CPS glue at the zirconium English powder of solidification and the surface of Ludox mixture, impregnation ratio is that 1mL liquid phase is about 4.5g solid phase, for sealing zirconium English powder and Ludox solidifies the pore produced, is at room temperature cured process.
Packaged Mg-28wt.%Gd alloy sheet is placed on heat fused in directional solidification furnace, thermograde is set to 12K/mm, close heating power supply after insulation 30min, the stove up and down of directional solidification furnace is cooled with the cooldown rate of 5K/s, observe the process of setting of Mg-28wt.%Gd alloy sheet.Fig. 4 is Mg-28wt.%Gd alloy sheet prepared by embodiment 2 method synchrotron radiation video interception when solidifying.Can see, the secondary dendrite of this alloy and once interdendritic angle are 60 °, and be the dendritic growth process of 6K/mm compared to thermograde, primary tiller crystals growth direction is closer to thermograde direction.
The present invention adopts Cosan to burn and consumes residual oxygen in crucible; produce the not oxidated pollution of sulphur dioxide reduction gas shield magnesium alloy; a certain amount of sulfur dioxide gas at high temperature produces certain vapour pressure simultaneously, inhibits magnesium alloy to volatilize, makes a concrete analysis of as follows.
The burning point of Cosan about 248 DEG C, and the melting point of magnesium about 650 DEG C, so first Cosan will burn generation sulfur dioxide in crucible heating process, suppress magnesium alloy and oxygen reaction, effectively can stop oxidation and the burning of magnesium alloy as seen under Cosan existent condition.
The saturated vapour pressure variation with temperature rule of metal can represent with Clausius-Clapeyron equation,
In formula, p vapour pressure (Pa), T melt temperature (K); L evaporation latent heat (J/mol); V liquid, V gasbe respectively the volume (m after the liquid volume of 1mol and the evaporation of 1mol liquid 3/ mol).
Ignore liquid phase volume, the saturated vapour pressure can trying to achieve metal according to perfect gas law is,
lgp=AT -1+BlgT+C
In formula, A, B, C are respectively integral constant.Look into corresponding metals handbook, A, B and C value of metallic element can be obtained, fusing point at metal can be obtained to the saturated vapour pressure of metal in boiling temperature interval.For magnesium metal, A=-7550, B=-1.41, C=12.79.
Can obtain thus, as 800 DEG C time, the saturated vapour pressure of metal M g is 30.30torr, about 4039.31Pa.
Following reaction is there is in Cosan in sealing ventilation pipe III,
S+O 2→SO 2
SO 2gas follows perfect gas law, i.e. pv=nRT, and wherein p is pressure, and v is volume, and n is the amount of gaseous matter, R gas molar constant, T absolute temperature.
From crucible structure body, volume v is corundum sheet and the interbedded volume of graphite paper, then crucible volume is, v=abc, a, b, c are respectively the inside casing size of graphite paper.
Namely known thus, the Cosan of nmol can produce the sulfur dioxide gas of nmol, and the pressure that can produce in crucible is, p=nRT/ (abc).Suppress the volatilization of magnesium to sulfur dioxide, then need the vapour pressure that sulfur dioxide is produced to be more than or equal to the saturated vapour pressure of magnesium generation, then required minimum Cosan amount is,
x = n M = p v R T M = 32 a b c R T 10 AT - 1 + B lg T + C
Be respectively 36mm, 16mm and 0.2mm for the inner cavity size of crucible and temperature is 800 DEG C, the producible vapour pressure of bright sulfur sulphur of 1g is about 2.42 × 10 9pa.Find under crucible interior size is respectively 36mm, 16mm and 0.2mm and temperature is the condition of 800 DEG C after calculating, need to put into be more than or equal to 1.71 × 10 -6the sulphur of g can suppress the volatilization of magnesium alloy.
For ensureing that oxygen is all consumed in crucible body, supposes to be oxygen in crucible body, then the amount of Cosan is needed to be,
x = 32 v R = 32 a b c R
For the present invention, be respectively 36mm, 16mm and 0.2mm for crucible interior size, run out of whole oxygen in crucible body and need 4.43 × 10 -7g Cosan.
To sum up Cosan use amount is relevant with crucible volume, and its use amount is,
x ≥ 32 a b c R T 10 AT - 1 + B lg T + C
Cosan may have partition losses in actual use, is respectively 36mm, 16mm and 0.2mm for crucible interior size, uses the amount of Cosan to be about 0.1g.
The BN spray that the present invention uses has superior film forming adhesion at 800 DEG C, and and motlten metal, as aluminum bronze steel etc., or glass melts slurry any reaction does not occur.
The mixture of the zirconium English powder that the present invention uses and Ludox can bear more than 800 DEG C high temperature, does not react, seal after solidification with magnesium alloy.
The present invention uses the graphite frame of hollow to play fixation, and is convenient to sealing.Meanwhile, hollow structure avoids X-ray by decay during graphite, improves the contrast of photo, thus is convenient to from photo, obtain required information.
The heat resisting temperature of the high temperature resistant inorganic CPS glue that the present invention uses is 980 DEG C, and linear expansion coefficient is close with iron and steel slightly to be shunk, and it is water-fast, oil resistant, does not react with magnesium alloy and corundum sheet.

Claims (3)

1. a magnesium alloy in course of solidification synchrotron radiation real time imagery research crucible, is characterized in that: the mixture (4) and the high temperature resistant inorganic CPS glue (5) that comprise graphite frame (1), corundum sheet (2), graphite paper (3), zirconium English powder and Ludox; Described graphite paper (3) is hollow type, be placed between the measure-alike corundum sheet (2) of two panels, place Cosan in the hollow type cavity of graphite paper (3), the space between graphite paper (3) and two panels corundum sheet (2) uses the mixture (4) of zirconium English powder and Ludox to fill; The graphite frame (1) of hollow belt groove is put into after graphite paper (3) and two panels corundum sheet (2) assemble, graphite paper (3) is filled with the mixture (4) of zirconium English powder and Ludox with the groove vicinity of graphite frame (1), is coated with one deck high temperature resistant inorganic CPS glue (5) after solidification again.
2. a preparation method for crucible described in claim 1, is characterized in that comprising the following steps:
Step one, spray one deck BN spray, at room temperature placement 2 minutes corundum sheet (2) and graphite paper (3) are upper;
Step 2, by zirconium English powder and Ludox mixing and stirring, make the mixture (4) of zirconium English powder and Ludox, modulation ratio is that 4 ~ 5g zirconium English powder joined by 1mL Ludox;
Step 3, the magnesium alloy thin slice of equal for two sides polishing is put into the graphite paper (3) of hollow, clamp with two panels corundum sheet (2); Void area around magnesium alloy thin slice and graphite paper (3) puts into Cosan, fills the mixture (4) of zirconium English powder and Ludox subsequently on corundum sheet (2) four limit;
The graphite frame (1) of hollow belt groove is put into after step 4, graphite paper (3) and two panels corundum sheet (2) assemble, graphite paper (3) is filled with the mixture (4) of zirconium English powder and Ludox with the groove vicinity of graphite frame (1), at room temperature makes the mixture (4) of zirconium English powder and Ludox solidify;
Mixture (4) surface of step 5, zirconium English powder after hardening and Ludox is coated with last layer high temperature resistant inorganic CPS glue (5), mixture (4) for sealing zirconium English powder and Ludox solidifies the pore produced, and is at room temperature cured process.
3. the preparation method of crucible according to claim 2, is characterized in that: described magnesium alloy thin chip size is 35*15* (0.15 ~ 0.2) mm.
CN201510874462.0A 2015-12-03 2015-12-03 Crucible for magnesium alloy solidification synchrotron radiation real-time imaging study and preparation method of crucible Active CN105413774B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201510874462.0A CN105413774B (en) 2015-12-03 2015-12-03 Crucible for magnesium alloy solidification synchrotron radiation real-time imaging study and preparation method of crucible

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201510874462.0A CN105413774B (en) 2015-12-03 2015-12-03 Crucible for magnesium alloy solidification synchrotron radiation real-time imaging study and preparation method of crucible

Publications (2)

Publication Number Publication Date
CN105413774A true CN105413774A (en) 2016-03-23
CN105413774B CN105413774B (en) 2017-04-12

Family

ID=55492574

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201510874462.0A Active CN105413774B (en) 2015-12-03 2015-12-03 Crucible for magnesium alloy solidification synchrotron radiation real-time imaging study and preparation method of crucible

Country Status (1)

Country Link
CN (1) CN105413774B (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110064454A (en) * 2019-05-24 2019-07-30 郑州轻工业学院 Magnesium alloy in course of solidification experiment crucible and packaging method under synchrotron radiation state
CN112098466A (en) * 2020-09-14 2020-12-18 大连理工大学 Sample electrifying module suitable for synchrotron radiation in-situ imaging below 600 DEG C

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20020139143A1 (en) * 2001-03-08 2002-10-03 Gabriele Korus Method of producing a quartz glass crucible
WO2004110951A1 (en) * 2003-06-06 2004-12-23 Goodrich Corporation Multi-layer fire-barrier systems
CN1565778A (en) * 2003-06-13 2005-01-19 闵小兵 Method and anti-sticking paper for preventing hard metal article from sticking to container in high sintering process
CN102744366A (en) * 2012-06-19 2012-10-24 北京百慕航材高科技股份有限公司 Preparation method of titanium aluminium-based and niobium silicon-based alloy directional solidification investment precision casting mold shell
CN102978551A (en) * 2012-11-30 2013-03-20 东北大学 Heat treatment method for preventing Li removal and oxidization of Mg-Li based magnesium alloy surface
CN202913087U (en) * 2012-10-30 2013-05-01 烟台核晶陶瓷新材料有限公司 Ceramic crucible for polycrystalline silicon ingot
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
CN203960266U (en) * 2014-07-10 2014-11-26 河南科技大学 A kind of thermal treatment unit that prevents Mg alloy surface oxidation

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20020139143A1 (en) * 2001-03-08 2002-10-03 Gabriele Korus Method of producing a quartz glass crucible
WO2004110951A1 (en) * 2003-06-06 2004-12-23 Goodrich Corporation Multi-layer fire-barrier systems
CN1565778A (en) * 2003-06-13 2005-01-19 闵小兵 Method and anti-sticking paper for preventing hard metal article from sticking to container in high sintering process
CN102744366A (en) * 2012-06-19 2012-10-24 北京百慕航材高科技股份有限公司 Preparation method of titanium aluminium-based and niobium silicon-based alloy directional solidification investment precision casting mold shell
CN202913087U (en) * 2012-10-30 2013-05-01 烟台核晶陶瓷新材料有限公司 Ceramic crucible for polycrystalline silicon ingot
CN102978551A (en) * 2012-11-30 2013-03-20 东北大学 Heat treatment method for preventing Li removal and oxidization of Mg-Li based magnesium alloy surface
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
CN203960266U (en) * 2014-07-10 2014-11-26 河南科技大学 A kind of thermal treatment unit that prevents Mg alloy surface oxidation

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
东青: "Al-Cu合金定向凝固过程中的形态演化", 《中国博士学位论文全文数据库 工程科技Ⅰ辑》 *
刘晟初等: "带有电磁扰动的Bridgman定向凝固装置设计", 《大连理工大学学报》 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110064454A (en) * 2019-05-24 2019-07-30 郑州轻工业学院 Magnesium alloy in course of solidification experiment crucible and packaging method under synchrotron radiation state
CN112098466A (en) * 2020-09-14 2020-12-18 大连理工大学 Sample electrifying module suitable for synchrotron radiation in-situ imaging below 600 DEG C

Also Published As

Publication number Publication date
CN105413774B (en) 2017-04-12

Similar Documents

Publication Publication Date Title
Witusiewicz et al. The Ag–Al–Cu system: Part I: Reassessment of the constituent binaries on the basis of new experimental data
Chartrand et al. Critical evaluation and optimization of the thermodynamic properties and phase diagrams of the Al-Mg, Al-Sr, Mg-Sr, and Al-Mg-Sr systems
CN105413774A (en) Crucible for magnesium alloy solidification synchrotron radiation real-time imaging study and preparation method of crucible
Pershin et al. Synthesis of silumins in KF-AlF3-SiO2 melts
CN103781922B (en) For equipment and the method for condensing metal steam
JP2011058096A (en) Method for electrically producing alkali metal from alkali metal amalgam
Ge et al. Hot corrosion behavior of NbSi2/SiO2-Nb2O5 multilayer coating on Nb alloy
US9112193B2 (en) Sealing arrangement for high-temperature fuel cell stack
Lichtenstein et al. Thermodynamic properties of rare‐earth alloys by electrochemical emf measurements
Judge et al. Electrochemical characteristics of molten iron electrodes in slag and electrochemical properties of their interface
Yuan et al. Deoxidation of Molten Metals by Short Circuiting Yttria‐Stabilized Zirconia Electrolyte Cell
AU594966B2 (en) Aluminium reduction cells
Wu et al. Microstructure and Thickness of 55 pct Al-Zn-1.6 pct Si-0.2 pct RE hot-dip coatings: experiment, thermodynamic, and first-principles study
CN103506770A (en) Aluminum alloy sheet laser welding auxiliary weld-joint forming material and preparation method thereof
Veleckis et al. Solubility of lithium deuteride in liquid lithium
JP5649405B2 (en) Aluminum alloy brazing sheet for fluxless brazing and fluxless brazing method of aluminum material
RU2252981C2 (en) Electrolytic element for producing alkali metal
Borom et al. Reactions Between Metallic Iron and Cobalt Oxide‐Bearing Sodium Disilicate Glass
Baclig Eutectic liquids for high-energy density flow batteries
Oyarzabal et al. Deuterium retention of liquid Sn and SnLi in a CPS target under plasma exposure at high temperatures
Elrefaie et al. Thermodynamic properties of the ionic conducting phases of Na-Al-O system between 800 and 1200 K
Wiencke et al. The influence of iron concentration on the anodic charge transfer in molten oxide electrolysis
Liao et al. Study on surface tension of Dy-Cu intermediate alloy prepared using LiF-DyF3 molten salt system
CN207689222U (en) A kind of anti-metal sample high-temperature oxidization equipment
Bloembergen et al. A new approach to the determination of the liquidus and solidus points associated with the melting curve of the eutectic Co–C, taking into account the thermal inertia of the furnace

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant