CN105413774B - 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 PDFInfo
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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
Technical field
The present invention relates to a kind of crucible, more particularly to a kind of magnesium alloy in course of solidification synchrotron radiation realtime imaging research earthenware
Crucible.Further relate to the preparation method of this crucible.
Background technology
Reference Fig. 5, document "《Metal alloy solidifies dendritic growth synchrotron radiation realtime imaging research》[D] is permitted lush Dalian
The p19-20 of Polytechnics's master thesis 2010.06 " discloses a kind of for metal alloy solidification synchrotron radiation realtime imaging
With crucible, including quartz glass plate 6, ptfe sheet 7 and clip 8, hollow ptfe sheet with groove 7 is clipped in
In two panels quartz glass plate 6, the outside clip 8 of quartz glass plate 6 is clamped.This crucible can not completely cut off connecing for technic metal and oxygen
Touch, be only applicable to the not oxidizable metal alloy of high temperature, such as Al alloys, Sn-Pb alloys.However, magnesium and magnesium alloy property ten
Divide active, meeting and many metals or nonmetallic and oxide etc. occur chemical reaction, are easily oxidized under high temperature.Therefore, this earthenware
Crucible is not applied for alloy oxidizable under the high temperature such as magnesium and magnesium alloy.
The content of the invention
Easily aoxidize for magnesium alloy to overcome the shortcomings of existing crucible, the present invention provides a kind of magnesium alloy in course of solidification
Synchrotron radiation realtime imaging research crucible.The crucible includes the mixed of graphite frame, corundum piece, graphite paper, zirconium English powder and Ludox
Compound and high temperature resistant inorganic CPS glue.The graphite paper is hollow type, is placed between the equivalently-sized corundum piece of two panels, graphite paper
Hollow molded cavity body in place Cosan, the space between graphite paper and two panels corundum piece using zirconium English powder and Ludox mixing
Thing is filled.It is put in hollow graphite frame with groove after graphite paper and the assembling of two panels corundum piece, the groove of graphite paper and graphite frame
Surrounding is filled with zirconium English powder with the mixture of Ludox, and one layer of high temperature resistant inorganic CPS glue is repasted after solidification.The present invention is sprayed using BN
Agent coated corundum piece and graphite paper so that magnesium alloy will not react with corundum piece and graphite paper；Zirconium English powder and Ludox
The double-layer seal of mixture and high temperature resistant inorganic CPS glue so that magnesium alloy is completely isolated with air；It is put into inside crucible appropriate
Cosan can consume the oxygen of residual, the sulphur dioxide reduction gas shield magnesium alloy of generation does not receive oxidation stain,
Certain vapour pressure can also be produced under high temperature, suppresses the volatilization of magnesium alloy, by multilayer proofing technology, solve magnesium alloy high temperature
The technical problem of oxidation.
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 is real-time
Imaging research crucible, is characterized in：Mixture 4 including graphite frame 1, corundum piece 2, graphite paper 3, zirconium English powder and Ludox and
High temperature resistant inorganic CPS glue 5.The graphite paper 3 is hollow type, is placed between the equivalently-sized corundum piece 2 of two panels, graphite paper 3
Cosan is placed in hollow molded cavity body, the space between graphite paper 3 and two panels corundum piece 2 uses the mixing of zirconium English powder and Ludox
Thing 4 is filled.It is put in hollow graphite frame with groove 1 after the assembling of graphite paper 3 and two panels corundum piece 2, graphite paper 3 and graphite frame 1
Groove vicinity zirconium English powder fill with the mixture 4 of Ludox, one layer of high temperature resistant inorganic CPS glue 5 is repasted after solidification.
A kind of preparation method of above-mentioned crucible, is characterized in comprising the following steps：
Step one, on corundum piece 2 and graphite paper 3 one layer of BN spray is sprayed, placed 2 minutes at room temperature.
Step 2, by zirconium English powder and Ludox mixing and stirring, make the mixture 4 of zirconium English powder and Ludox, modulate
Ratio is that 1mL Ludox matches somebody with somebody 4～5g zirconium English powder.
Step 3, the magnesium alloy thin slice for polishing two sides are put in hollow graphite paper 3, are clamped with two panels corundum piece 2.
Void area around magnesium alloy thin slice and graphite paper 3 is put into Cosan, subsequently fills zirconium English powder and silicon on the side of corundum piece 2 four
The mixture 4 of colloidal sol.
Be put in hollow graphite frame with groove 1 after the assembling of step 4, graphite paper 3 and two panels corundum piece 2, graphite paper 3 with
The groove vicinity zirconium English powder of graphite frame 1 is filled with the mixture 4 of Ludox, and the mixing of zirconium English powder and Ludox is made at room temperature
Thing 4 solidifies.
The surface of mixture 4 of step 5, zirconium English powder after hardening and Ludox applies last layer high temperature resistant inorganic CPS glue 5,
For sealing the pore that zirconium English powder is produced with the solidification of mixture 4 of Ludox, cured is carried out at room temperature.
The magnesium alloy thin chip size is 35*15* (0.15～0.2) mm.
The invention has the beneficial effects as follows：The crucible includes the mixed of graphite frame, corundum piece, graphite paper, zirconium English powder and Ludox
Compound and high temperature resistant inorganic CPS glue.The graphite paper is hollow type, is placed between the equivalently-sized corundum piece of two panels, graphite paper
Hollow molded cavity body in place Cosan, the space between graphite paper and two panels corundum piece using zirconium English powder and Ludox mixing
Thing is filled.It is put in hollow graphite frame with groove after graphite paper and the assembling of two panels corundum piece, the groove of graphite paper and graphite frame
Surrounding is filled with zirconium English powder with the mixture of Ludox, and one layer of high temperature resistant inorganic CPS glue is repasted after solidification.The present invention is sprayed using BN
Agent coated corundum piece and graphite paper so that magnesium alloy will not react with corundum piece and graphite paper；Zirconium English powder and Ludox
The double-layer seal of mixture and high temperature resistant inorganic CPS glue so that magnesium alloy is completely isolated with air；It is put into inside crucible appropriate
Cosan can consume the oxygen of residual, the sulphur dioxide reduction gas shield magnesium alloy of generation does not receive oxidation stain,
Certain vapour pressure can also be produced under high temperature, suppresses the volatilization of magnesium alloy, by multilayer proofing technology, solve magnesium alloy high temperature
The technical problem of oxidation.
The present invention is described in detail below in conjunction with drawings and Examples.
Description of the drawings
Fig. 1 is the structural representation of crucible of the present invention.
Fig. 2 is the crucible prepared using the present invention, and Mg-28wt.%Gd thin slices heat the photomacrograph after remelting.
Fig. 3 is the crucible prepared using the present invention, and in G=6K/mm, cooldown rate is under 5K/s to Mg-28wt.%Gd thin slices
Synchrotron radiation video interception.
Fig. 4 is the crucible prepared using the present invention, and in G=12K/mm, cooldown rate is 5K/s to Mg-28wt.%Gd thin slices
Under synchrotron radiation video interception.
Fig. 5 is that technical background is used for the structural representation that metal alloy solidifies synchrotron radiation realtime imaging crucible.
In figure, 1- graphite frames, 2- corundum pieces, 3- graphite papers, the mixture of 4- zirconium English powder and Ludox, 5- high temperature resistant inorganics
CPS glue, 6- quartz glass plates, 7- ptfe sheets, 8- clips.
Specific embodiment
Following examples reference picture 1-4.
Embodiment 1：The present invention is magnesium alloy in course of solidification synchrotron radiation realtime imaging research crucible and preparation method thereof.
Crucible includes the mixture 4 and high temperature resistant inorganic of graphite frame 1, corundum piece 2, the hollow thin slice of graphite paper 3, zirconium English powder and Ludox
CPS glue 5.Hollow graphite paper sheet 3 is placed between the equivalently-sized corundum piece 2 of two panels, and is put in this cavity appropriate
Filled using the pasty mixture 4 of zirconium English powder and Ludox in Cosan, the space of surrounding.This entirety is being put into into hollow belt groove
Graphite frame 1 in, around filled with the mixture 4 of zirconium English powder and Ludox, after solidification around it apply last layer high temperature resistant without
Machine CPS glue 5.
The above-mentioned preparation method for magnesium alloy in course of solidification synchrotron radiation realtime imaging research crucible is：
(1) one layer of BN spray is sprayed on the graphite paper interlayer between corundum piece and corundum piece, about 2 points is placed at room temperature
Clock, after it is completely dried by use；
(2) zirconium English powder and Ludox mixing and stirring are given over to encapsulant and is used to pasty state, modulation ratio is 1mL
Ludox about 4.5g zirconium English powder；
(3) the Mg-28wt.%Gd alloy sheets for polishing two sides are put in hollow graphite paper, Mg-28wt.%Gd
Alloy sheet size is 35*15*0.2mm, is clamped with two panels corundum piece, forms sandwich structure.In Mg-28wt.%Gd
Void area around alloy sheet and graphite paper is put into appropriate Cosan, subsequently fills zirconium English powder and silicon on the side of corundum piece four
The mixture of colloidal sol, hole is tamped；
(4) said structure is put in hollow graphite frame, on the side of graphite frame four mixing of zirconium English powder and Ludox is filled out
Thing, makes sample isolate with outside air, zirconium English powder is solidified with the mixture of Ludox at room temperature；
(5) last layer high temperature resistant inorganic CPS glue, impregnation ratio are applied in the zirconium English powder of solidification and the surface of Ludox mixture
For 1mL liquid phases about 4.5g solid phases, the pore for producing is solidified with Ludox for sealing zirconium English powder, carried out at room temperature at solidification
Reason.
Packaged Mg-28wt.%Gd alloy sheets are placed in resistance furnace and are heated to 700 DEG C, with stove after insulation 30min
Cooling, when temperature is down to 500 DEG C sample is taken out.Fig. 2 is Mg-28wt.%Gd alloy sheet remeltings prepared by the method for embodiment 1
The photomacrograph for solidifying afterwards.The quality of sample is 0.1411g before experiment, and the quality of sample is 0.1501g after test, shows sample
Oxidation is less, and only the sample of tiny area there occurs reaction with oxygen；Meanwhile, before experiment, the thickness of sample bottom
For 0.18mm, slightly thickening, this is because liquation is generated sinking by action of gravity.
Embodiment 2：The present invention is magnesium alloy in course of solidification synchrotron radiation realtime imaging research crucible and preparation method thereof.
Crucible includes the mixture 4 and high temperature resistant inorganic of graphite frame 1, corundum piece 2, the hollow thin slice of graphite paper 3, zirconium English powder and Ludox
CPS glue 5.Hollow graphite paper sheet 3 is placed between the equivalently-sized corundum piece 2 of two panels, and is put in this cavity appropriate
Filled using the pasty mixture 4 of zirconium English powder and Ludox in Cosan, the space of surrounding.This entirety is being put into into hollow belt groove
Graphite frame 1 in, around filled with the mixture 4 of zirconium English powder and Ludox, after solidification around it apply last layer high temperature resistant without
Machine CPS glue 5.
The above-mentioned preparation method for magnesium alloy in course of solidification synchrotron radiation realtime imaging research crucible is：
(1) one layer of BN spray is sprayed on the graphite paper interlayer between corundum piece and corundum piece, about 2 points is placed at room temperature
Clock, after it is completely dried by use；
(2) zirconium English powder and Ludox mixing and stirring are given over to encapsulant and is used to pasty state, modulation ratio is 1mL
Ludox about 4g zirconium English powder；
(3) the Mg-28wt.%Gd alloy sheets for polishing two sides are put in hollow graphite paper, Mg-28wt.%Gd
Alloy sheet size is 35*15*0.2mm, is clamped with two panels corundum piece, forms sandwich structure.In Mg-28wt.%Gd
Void area around alloy sheet and graphite paper is put into appropriate Cosan, subsequently fills zirconium English powder and silicon on the side of corundum piece four
The mixture of colloidal sol, hole is tamped；
(4) said structure is put in hollow graphite frame, on the side of graphite frame four mixing of zirconium English powder and Ludox is filled out
Thing, makes Mg-28wt.%Gd alloy sheets isolate with outside air, zirconium English powder is solidified with the mixture of Ludox at room temperature；
(5) last layer high temperature resistant inorganic CPS glue, impregnation ratio are applied in the zirconium English powder of solidification and the surface of Ludox mixture
For 1mL liquid phases about 4.5g solid phases, the pore for producing is solidified with Ludox for sealing zirconium English powder, carried out at room temperature at solidification
Reason.
Packaged Mg-28wt.%Gd alloy sheets are placed in directional solidification furnace plus heat fusing, thermograde is set to
6K/mm, after insulation 30min heating power supply is closed, and the stove up and down for making directional solidification furnace is cooled down with the cooldown rate of 5K/s, observation
The process of setting of Mg-28wt.%Gd alloy sheets.Fig. 3 is Mg-28wt.%Gd alloy sheets solidification prepared by the method for embodiment 2
When synchrotron radiation video interception.Can see, the secondary dendrite of the alloy is 60 ° with once interdendritic angle, primary tiller
Deviate with thermograde direction in crystals growth direction.
Embodiment 3：The present invention is magnesium alloy in course of solidification synchrotron radiation realtime imaging research crucible and preparation method thereof.
Crucible includes the mixture 4 and high temperature resistant inorganic of graphite frame 1, corundum piece 2, the hollow thin slice of graphite paper 3, zirconium English powder and Ludox
CPS glue 5.Hollow graphite paper sheet 3 is placed between the equivalently-sized corundum piece 2 of two panels, and is put in this cavity appropriate
Filled using the pasty mixture 4 of zirconium English powder and Ludox in Cosan, the space of surrounding.This entirety is being put into into hollow belt groove
Graphite frame 1 in, around filled with the mixture 4 of zirconium English powder and Ludox, after solidification around it apply last layer high temperature resistant without
Machine CPS glue 5.
The above-mentioned preparation method for magnesium alloy in course of solidification synchrotron radiation realtime imaging research crucible is：
(1) one layer of BN spray is sprayed on the graphite paper interlayer between corundum piece and corundum piece, about 2 points is placed at room temperature
Clock, after it is completely dried by use；
(2) zirconium English powder and Ludox mixing and stirring are given over to encapsulant and is used to pasty state, modulation ratio is 1mL
Ludox about 5g zirconium English powder；
(3) the Mg-28wt.%Gd alloy sheets for polishing two sides are put in hollow graphite paper, Mg-28wt.%Gd
Alloy sheet size is 35*15*0.2mm, is clamped with two panels corundum piece, forms sandwich structure.In Mg-28wt.%Gd
Void area around alloy sheet and graphite paper is put into appropriate Cosan, subsequently fills zirconium English powder and silicon on the side of corundum piece four
The mixture of colloidal sol, hole is tamped；
(4) said structure is put in hollow graphite frame, on the side of graphite frame four mixing of zirconium English powder and Ludox is filled out
Thing, makes Mg-28wt.%Gd alloy sheets isolate with outside air, zirconium English powder is solidified with the mixture of Ludox at room temperature；
(5) last layer high temperature resistant inorganic CPS glue, impregnation ratio are applied in the zirconium English powder of solidification and the surface of Ludox mixture
For 1mL liquid phases about 4.5g solid phases, the pore for producing is solidified with Ludox for sealing zirconium English powder, carried out at room temperature at solidification
Reason.
Packaged Mg-28wt.%Gd alloy sheets are placed in directional solidification furnace plus heat fusing, thermograde is set to
12K/mm, after insulation 30min heating power supply is closed, and the stove up and down for making directional solidification furnace is cooled down with the cooldown rate of 5K/s, observation
The process of setting of Mg-28wt.%Gd alloy sheets.Fig. 4 is Mg-28wt.%Gd alloy sheets solidification prepared by the method for embodiment 2
When synchrotron radiation video interception.Can see, the secondary dendrite of the alloy is 60 ° with once interdendritic angle, compared to
Thermograde is the dendritic growth process of 6K/mm, and a dendritic growth direction is closer to thermograde direction.
The present invention consumes residual oxygen in crucible using Cosan burning, produces sulphur dioxide reduction gas shield magnesium and closes
Gold does not receive oxidation stain, while a certain amount of sulfur dioxide gas produce at high temperature certain vapour pressure, it is suppressed that magnesium alloy
Volatilization, makes a concrete analysis of as follows.
About 248 DEG C of the burning point of Cosan, and about 650 DEG C of the melting point of magnesium, so the Cosan in crucible heating process
To first be burnt generation sulfur dioxide, suppress magnesium alloy and oxygen reaction, it is seen that can be effectively under conditions of Cosan is present
Prevent the oxidation and burning of magnesium alloy.
The saturated vapour pressure variation with temperature rule of metal can represent with Clausius-Clapeyron equations,
In formula, p vapour pressures (Pa), T melt temperatures (K)；L evaporation latent heats (J/mol)；VLiquid、VGasThe respectively liquid of 1mol
Volume (m after volume and 1mol liquid evaporations3/mol)。
Ignore liquid phase volume, be according to the saturated vapour pressure that metal is tried to achieve by perfect gas law,
Lgp=AT-1+BlgT+C
In formula, A, B, C are respectively integral constant.Corresponding metals handbook is looked into, A, B and C value of metallic element can be obtained, you can
Obtain the saturated vapour pressure of the metal in the fusing point of metal is interval to boiling temperature.For magnesium metal, A=-7550, B=-
1.41, C=12.79.
Thus can obtain, such as at 800 DEG C, the saturated vapour pressure of metal Mg is 30.30torr, about 4039.31Pa.
There is following reaction in sealing ventilation pipe III in Cosan,
S+O2→SO2
SO2Gas follows perfect gas law, i.e. pv=nRT, and wherein p is pressure, and v is volume, and n is gaseous matter
Amount, R gas molar constants, T absolute temperature.
From crucible structure body, volume v is corundum piece 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.
Thus understand, the Cosan of n mol can produce the sulfur dioxide gas of n mol, can produce in crucible
Pressure is, p=nRT/ (abc).Suppress the volatilization of magnesium to sulfur dioxide, then need the vapour pressure for producing sulfur dioxide to be more than etc.
In magnesium produce saturated vapour pressure, then required minimum Cosan amount be,
So that the interior chamber size of crucible is respectively 36mm, 16mm and 0.2mm and temperature for 800 DEG C as an example, the bright sulfur sulphur of 1g
Producible vapour pressure is about 2.42 × 109Pa.Find to be respectively 36mm, 16mm and 0.2mm in crucible interior size after calculating
And temperature is under conditions of 800 DEG C, needs are put into more than or equal to 1.71 × 10-6The sulfur of g can suppress the volatilization of magnesium alloy.
To ensure that oxygen is all consumed in crucible body, it is assumed that oxygen is in crucible body, then needs Cosan
Measure and be,
For the present invention, so that crucible interior size is respectively 36mm, 16mm and 0.2mm as an example, run out of in crucible body
Whole oxygen need 4.43 × 10-7G Cosans.
To sum up Cosan usage amount is relevant with crucible volume, and its usage amount is,
In actual use Cosan may have partition losses, and with crucible interior size 36mm, 16mm and 0.2mm are respectively
As a example by, it is about 0.1g using the amount of Cosan.
The BN sprays that the present invention is used have a superior film forming adhesion at 800 DEG C, and and motlten metal, such as aluminum bronze
Steel etc., or there is no any reaction in the molten slurry of glass.
The zirconium English powder and the mixture of Ludox that the present invention is used can bear 800 DEG C of high temperature above, not occur with magnesium alloy
Reaction, seals after solidification.
The present invention plays fixation using hollow graphite frame, and is easy to sealing.Meanwhile, hollow structure avoids X and penetrates
Line passes through decay during graphite, improves the contrast of photo, consequently facilitating obtaining required information from photo.
The heat resisting temperature of the high temperature resistant inorganic CPS glue that the present invention is used is 980 DEG C, and linear expansion coefficient is close slightly with iron and steel
Shrink, its is water-fast, oil resistant, does not react with magnesium alloy and corundum piece.
Claims (3)
1. a kind of magnesium alloy in course of solidification synchrotron radiation realtime imaging research crucible, it is characterised in that：Including graphite frame (1),
The mixture (4) and high temperature resistant inorganic CPS glue (5) of corundum piece (2), graphite paper (3), zirconium English powder and Ludox；The graphite paper
(3) it is hollow type, Mg-28wt.%Gd magnesium alloy thin slices are put in hollow graphite paper (3), is placed in equivalently-sized firm of two panels
Between Semen Arecae (2), Mg-28wt.%Gd magnesium alloys thin slice places Cosan, graphite paper with the void area around graphite paper (3)
(3) filled with the mixture (4) of Ludox using zirconium English powder in the space and between two panels corundum piece (2)；Graphite paper (3) and two panels
It is put in hollow graphite frame with groove (1) after corundum piece (2) assembling, the groove vicinity zirconium of graphite paper (3) and graphite frame (1)
English powder is filled with the mixture (4) of Ludox, and one layer of high temperature resistant inorganic CPS glue (5) is repasted after solidification.
2. the preparation method of crucible described in a kind of claim 1, it is characterised in that comprise the following steps：
Step one, on corundum piece (2) and graphite paper (3) one layer of BN spray is sprayed, placed 2 minutes at room temperature；
Step 2, by zirconium English powder and Ludox mixing and stirring, make the mixture (4) of zirconium English powder and Ludox, modulation ratio
Example matches somebody with somebody 4～5g zirconium English powder for 1mL Ludox；
Step 3, the Mg-28wt.%Gd magnesium alloy thin slices for polishing two sides are put in hollow graphite paper (3), firm with two panels
Semen Arecae (2) is clamped；Void area around Mg-28wt.%Gd magnesium alloys thin slice and graphite paper (3) is put into Cosan, subsequently
The mixture (4) of zirconium English powder and Ludox is filled on the side of corundum piece (2) four；
It is put in hollow graphite frame with groove (1) after step 4, graphite paper (3) and two panels corundum piece (2) assembling, graphite paper
(3) filled with the mixture (4) of zirconium English powder and Ludox with the groove vicinity of graphite frame (1), zirconium English powder and silicon are made at room temperature
Mixture (4) solidification of colloidal sol；
Mixture (4) surface of step 5, zirconium English powder after hardening and Ludox applies last layer high temperature resistant inorganic CPS glue (5),
For sealing the pore that zirconium English powder is produced with mixture (4) solidification of Ludox, cured is carried out at room temperature.
3. the preparation method of crucible according to claim 2, it is characterised in that：The Mg-28wt.%Gd magnesium alloys thin slice chi
It is very little for 35*15* (0.15～0.2) mm.
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