CN108796253A - A kind of preparation of reactive infiltration Si-Y alloys and tissue modulation method - Google Patents
A kind of preparation of reactive infiltration Si-Y alloys and tissue modulation method Download PDFInfo
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- CN108796253A CN108796253A CN201810742279.9A CN201810742279A CN108796253A CN 108796253 A CN108796253 A CN 108796253A CN 201810742279 A CN201810742279 A CN 201810742279A CN 108796253 A CN108796253 A CN 108796253A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/03—Making non-ferrous alloys by melting using master alloys
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C28/00—Alloys based on a metal not provided for in groups C22C5/00 - C22C27/00
Abstract
A kind of preparation of reactive infiltration Si-Y alloys and tissue modulation method, in process of setting, solidification rate changes for the demand of different microscopic structures, temperature gradient is maintained at 150~240K/cm, as solidification rate changes from 0.1mm/min to 3.0mm/min, uniform full banded structure, the band-like transition tissue developed to island and uniform full island structure can be obtained respectively.The obtained smelting parameter section of the present invention is not limited to the method for smelting of directional solidification, resistance melting, induction melting, the methods of laser melting is applicable in, various techniques can adjust present situation in conjunction with the solidification rate of itself and are adjusted in solidification rate section proposed by the invention, obtain the full eutectic structure of the uniform not primary Si phase of different-shape.
Description
Technical field
The present invention relates to the organizational controls field of alloy, the banded structure of specifically a kind of reactive infiltration Si-Y alloys,
The regulation and control of transition tissue, island structure.
Background technology
Reactive infiltration method is the method for preparing SiC fiber reinforcements SiC ceramic matrix composite material most industrialization potential.But due to passing
The fusing point of the infiltration Si alloys of system is higher, if Si-Zr eutectic composition alloy melting points are 1370 DEG C, Si-Ti eutectic composition alloys
Fusing point is 1330 DEG C, Si-Mo eutectic composition alloy melting points are 1400 DEG C, is higher than the resistance to ablation temperature (1300 DEG C) of SiC fibers, meeting
The SiC fibers in infiltration process are caused to be failed by serious ablation.Compared to above traditional infiltration alloy, Si-Y alloys exist
There is 1215 DEG C of lower fusing point at eutectic composition Si-18at%Y, the temperature of reactive infiltration can be substantially reduced, to effectively
Protect SiC fibers not ablated.For traditional Si based alloy, domestic and international researcher has carried out research work.
Document " I Mayer, E Yanir, I Shidlovsky Dimorphism in rare earth
Disilicides [J] Inorg Chem6 (1967) 842-844 " utilizes PM technique, and heating is mixed with Hg in vacuum tube
Si, Y powder of conjunction, have been made α-YSi2.But powder metallurgic method method can not accomplish that alloy is completely fine and close, alloy hole defect
It is more, limit the application of alloy.
Document " TS Verkhoglyadova, LA Dvorina High temperature oxidation of
Silicides of rare earth metals [J] Zh Fiz Khim, 40 (1966) 2250 " pass through electric arc melting technique system
For Si-Y alloys." Wang Hong builds reactive infiltration and prepares continuous fiber reinforced SiC based composites and its performance study [D] document
Changsha:The National University of Defense Technology, 2012 " also use high vacuum electric arc melting technique, are made by arc discharge each in alloy
Constituent element fully melts, and obtains Si-22wt%Ti, Si-24wt%Zr and Si-226wt%Zr- by overturning melting repeatedly
Tri- kinds of eutectic Si alloys of 01wt%B.However arc melting method temperature gradient is relatively low and cooling rate is slower, causes alloy structure thick
Greatly.
Document " thanks the preparation of sharp silicon-base alloy negative material and Wuhan research [D] of chemical property：Wuhan science and technology is big
It learns, the two-step method being combined by the melting of high-frequency electromagnetic induction stove and high-energy ball milling in 2011 " is prepared for Si-25at%Ni, Si-
Tri- kinds of Si alloys of 30at%Ni, Si-50at%Ni, and have studied the chemical property of alloy.However induction melting direction of heat flow
Property unobvious, alloy structure poor orientation, component segregation are more serious.
The studies above merely relates to the preparation of the alloy, is not directed to the research of its microstructure homogenization regulation and control method.Because
Although Si-Y alloys have much advantage in terms of reducing reaction temperature, as the matrix alloy of reactive infiltration, Si-Y alloys
Primary silicon residual seriously can cause reactive infiltration uneven in tissue, while dramatically increase the risk of composite material high temperature brittle.
Therefore it realizes that the regulation and control of Si-Y alloy structures homogenization become to prepare and meets SiC fiber reinforcement SiC ceramic matrix composite material reactive infiltrations
It is required that infiltration alloy key technology.Currently, the problem of Si-Y alloy structure lack of homogeneity, is not solved effectively yet, it is domestic
Si-Y alloy structures homogenization regulation and control method is rarely reported outside.In view of solidifying in the solidified structure and process of setting of Si-Y alloys
Gu rate and temperature gradient are directly related, therefore, it is necessary to clearly go out the solidification rate of Si-Y alloys and temperature gradient is precisely adjusted
Section is controlled, the even tissue of Si-Y alloys is made, primary Si phase is not present, to realize engineer application.
Invention content
To overcome the shortcomings of that Si-Y alloy structures lack of homogeneity existing in the prior art, the present invention propose a kind of reaction
The preparation of infiltration Si-Y alloys and tissue modulation method.
The present invention detailed process be：
Step 1：It is prepared by base material.
It is Si powder and Y powder as raw material using purity, female ingot raw material of Si-18at%Y is made according to eutectic composition.Batch mixing
Briquetting is placed in vacuum non-consumable arc-melting furnace, is carried out melt back four times to female ingot raw material, is obtained Si-Y eutectic alloys
Female ingot.The melting electric current is 100A, and the melt time is 2min.
The purity of the Si powder is 99999%, and the purity of the Y powder is 99999%.
Step 2：Clamping assembles.
Step 3：Melting and solidification.Vacuum degree in directional solidification furnace is evacuated to 1 × 10-3Pa is simultaneously kept, and is filled with Ar gas.It beats
Heating power supply heating sample is opened, melting electric current is gradually increased and is heated to 1300~1570 DEG C in a manner of ladder-elevating temperature, heat preservation
40min.Start pull rod device after heat preservation, sample is solidified with the rate of 0.1~3.0mm/min, temperature ladder in draw process
Degree is maintained at 150~240K/cm, realizes the continuous solidification of material.Directional solidification process is until whole alundum tubes submerge cooling bay
Middle end.
When clamping assembles, Si-Y eutectic alloy mother's ingots are broken into fritter and are placed in alundum tube.To being equipped with Si-Y eutectics
The downward pull of alundum tube of alloy mother's ingot, makes alundum tube lower end 10mm be immersed in the cooling bay equipped with Ga-In-Sn aluminium alloys.
There is muff on the alundum tube, to realize the temperature gradient more than 140K/cm.
The detailed process of ladder-elevating temperature is to keep the melting electric current of 20A when the melting, makes to rise to 500 DEG C in stove, and protect
Warm 15min.Make to continue to rise to 900 DEG C in stove with the melting electric current of 50A after heat preservation, and keeps the temperature 15min；Continue with 100~
140A melting electric currents make to rise to 1300~1570 DEG C in stove.
In the process of setting of the present invention, solidification rate changes for the demand of different microscopic structures, and temperature gradient is protected
It holds in 150~240K/cm, as solidification rate changes from 0.1mm/min to 3.0mm/min, uniform full band can be obtained respectively
Shape tissue, the band-like transition tissue developed to island, uniform full island structure.
Due to the poor fluidity of Si-Y alloys, and belong to facet-facet alloy system, it is each in process of setting mutually to grow
Mechanism is complicated, and regulation and control difficulty is big, solidified structure lack of homogeneity, and primary phase roughening is serious.It is rational solidifying it is therefore desirable to clearly go out
Gu rate and temperature gradient section, make the even tissue of Si-Y alloys, primary Si phase is not present, to realize engineer application.Manager
By the research method calculated and directional solidification experiment is combined, the smelting technology parameter area of Si-Y alloys is finally determined：It is solidifying
Gu rate can obtain uniform banded structure, transition group in 0.1~3.0mm/min, temperature gradient in 150~240K/cm
It knits, island structure etc..
The advantage of the invention is that：
1. melting and process of setting in refractory brick muff installation can ensure in Si-Y alloy graining process have compared with
High temperature gradient, to make alloy form stable continuous solidification tissue.
2. attached drawing 1,2 is the longitudinal section of directional solidificating alloy ingot casting, cross section respectively, it can be seen that alloy inner homogeneous,
Densification, it is bright, without apparent crackle.By microstructure observation's (attached drawing 3) it can be seen that the even tissue of alloy, in eutectic
Si phases and YSi2Mutually neat arrangement coupled growth, completely eliminates coarse primary Si phase, has reached the mark of infiltration alloy
It is accurate.
3. micro- group of different Si-Y alloys can be obtained by controlling solidification rate and temperature gradient, accuracy controlling
It knits.By theoretical research and a large amount of repeated experiments are combined, are found：0.1~0.5mm/min of solidification rate, temperature gradient 150~
Under the conditions of 180K/cm, uniform ribbon tissue can be obtained, tissues observed fiber morphology can be found that Si phases and YSi in alloy2Phase
Growth vigor difference very little, grow mutually restrict, by stablize it is band-like in a manner of Coupled Growth, form uniform eutectic structure；It is solidifying
Gu under the conditions of 0.5~1.6mm/min of rate, 180~210K/cm of temperature gradient, the band-like transition developed to island can be obtained
Tissue, Si phases and YSi2Growth vigor gap between phase starts to show, and Si phases are because larger growth vigor starts in part
Region makes YSi2The growth of phase is hindered, forms discontinuous island structure, but tissue still maintains good equal at this time
Even property, primary Si phase do not occur；It, can under the conditions of 1.6~3.0mm/min of solidification rate, 210~240K/cm of temperature gradient
To obtain uniform full island structure, Si phases have larger growth vigor, have interrupted YSi completely2The longitudinal growth of phase, makes
YSi2Mutually become island from band-like, but within the scope of the solidification rate, tissue is still eutectic structure to alloy entirely, is not found thick
Big primary Si phase.The microstructure figure of three kinds of tissues is shown in attached drawing 3~5 respectively.
4. the obtained smelting parameter section of the present invention is not limited to the method for smelting of directional solidification, resistance melting, sense
Melting, the methods of laser melting is answered to be applicable in, various techniques can adjust present situation in institute of the present invention in conjunction with the solidification rate of itself
It is adjusted in the solidification rate section of proposition, obtains the full eutectic structure of the uniform not primary Si phase of different-shape.
Description of the drawings
Fig. 1 is Si-Y alloy microscopic structure shape appearance figures prepared by the present invention.
Fig. 2 is Si-Y alloy ribbon tissue microstructure figures prepared by the present invention.
Fig. 3 is Si-Y alloy transition tissue microstructure figures prepared by the present invention.
Fig. 4 is Si-Y alloy island structure microstructure figures prepared by the present invention.
Fig. 5 is the flow chart of the present invention.
Specific implementation mode
Embodiment one
The present embodiment is a kind of preparation of reactive infiltration Si-Y alloys and tissue modulation method.In preparation process, it will coagulate
Gu rate control is in the range of 0.1~0.5mm/min, temperature gradient 150K/cm, the leaching of uniform full banded structure is obtained
It oozes and Si-Y eutectic alloys, detailed process is used to include the following steps：
Step 1：It is prepared by base material.The Y powder that the Si powder and purity that are 99999% using purity are 99999% is pressed as raw material
Female ingot raw material of Si-18at%Y is made according to eutectic composition.Batch mixing briquetting is placed in vacuum non-consumable arc-melting furnace, and
Vacuum degree in stove is set to be consistently less than 1 × 10-3Pa.Melting electric current is set as 100A, the melt time is 2min, is carried out to female ingot raw material
First time melting.After first time melting, melting electric current is set herein as 100A, the melt time is 2min, to female ingot raw material
Carry out second of melting.It repeats the fusion process four times, obtains Si-Y eutectic alloy mother's ingots.
Step 2：Clamping assembles.Si-Y eutectic alloy mother's ingots are broken for fritter of the equivalent diameter less than 3mm to be placed in just
In beautiful pipe.Corundum pipe size isWall thickness is 1mm.Corundum equipped with Si-Y eutectic alloy mother's ingots is effective
Stainless joint is fixed in the lever base of directional solidification furnace, and downward pull in advance, and alundum tube lower end 10mm is made to be immersed in
In cooling bay equipped with Ga-In-Sn aluminium alloys.The muff that refractory brick is made is set around alundum tube.
Step 3：Melting and solidification.Vacuum degree in directional solidification furnace is evacuated to 1 × 10-3Pa is simultaneously kept, and is filled with Ar gas.
Heating power supply heating sample is opened, detailed process is：With the melting electric current of 20A, in-furnace temperature is set to rise to 500 DEG C, and keep the temperature
15min；Make in-furnace temperature continue to rise to 900 DEG C with the melting electric current of 50A after heat preservation, and keeps the temperature 15min；After heat preservation
Continue, with 100A melting electric currents, in-furnace temperature to be made to rise to 1300 DEG C, keeps the temperature 40min.Start pull rod device after heat preservation, makes examination
Sample is moved from top to bottom with the rate of 0.1mm/min, and temperature gradient is maintained at 150K/cm, realizes the continuous solidification of material.Institute
The continuous solidification process stated, which lasts up to whole alundum tubes and submerges in cooling bay, to be terminated.
After solidification, microexamination is carried out to tissue, is all organized as uniform band-like eutectic structure, and do not have in organizing
With the presence of any coarse primary Si phase, meet infiltration alloy requirement.
Embodiment two
The present embodiment be it is a kind of by solidification rate control in the range of 0.1~0.5mm/min, temperature gradient 160K/
Cm, obtains the infiltration Si-Y eutectic alloys of uniform full banded structure, and detailed process includes the following steps：
Step 1：It is prepared by base material.The Y powder that the Si powder and purity that are 99999% using purity are 99999% is pressed as raw material
Female ingot raw material of Si-18at%Y is made according to eutectic composition.Batch mixing briquetting is placed in vacuum non-consumable arc-melting furnace, and
Vacuum degree in stove is set to be consistently less than 1 × 10-3Pa.Melting electric current is set as 100A, the melt time is 2min, and melt back 4 times obtains
To Si-Y eutectic alloy mother's ingots.
Step 2：Clamping assembles.Si-Y eutectic alloy mother's ingots are broken for fritter of the equivalent diameter less than 3mm to be placed in just
In beautiful pipe.Corundum pipe size isWall thickness is 1mm.Corundum equipped with Si-Y eutectic alloy mother's ingots is effective
Stainless joint is fixed in the lever base of directional solidification furnace, and downward pull in advance, and alundum tube lower end 10mm is made to be immersed in
In cooling bay equipped with Ga-In-Sn aluminium alloys.The muff that refractory brick is made is set around alundum tube.
Step 3：Melting and solidification.Vacuum degree in directional solidification furnace is evacuated to 1 × 10-3Pa is simultaneously kept, and is filled with Ar gas.
Heating power supply heating sample is opened, detailed process is：With the melting electric current of 20A, make to rise to 500 DEG C in stove, and keep the temperature 15min；
Make to rise to 900 DEG C in stove with the melting electric current of 50A after heat preservation, and keeps the temperature 15min；Continue, with 105A melting electric currents, to make stove
1350 DEG C are inside risen to, 45min is kept the temperature.Start pull rod device after heat preservation, make sample with the rate of 0.3mm/min from top to bottom
It is mobile, temperature gradient is maintained at 160K/cm, realizes the continuous solidification of material.The continuous solidification process lasts up to entirely
Portion's alundum tube, which submerges in cooling bay, to be terminated.
After solidification, microexamination is carried out to tissue, is all organized as uniform band-like eutectic structure, and do not have in organizing
With the presence of any coarse primary Si phase, meet infiltration alloy requirement.
Embodiment three
The present embodiment be it is a kind of by solidification rate control in the range of 0.1~0.5mm/min, temperature gradient 170K/
Cm, obtains the infiltration Si-Y eutectic alloys of uniform full banded structure, and detailed process includes the following steps：
Step 1：It is prepared by base material.The Y powder that the Si powder and purity that are 99999% using purity are 99999% is pressed as raw material
Female ingot raw material of Si-18at%Y is made according to eutectic composition.Batch mixing briquetting is placed in vacuum non-consumable arc-melting furnace, and
Vacuum degree in stove is set to be consistently less than 1 × 10-3Pa.Melting electric current is set as 100A, the melt time is 2min, and melt back 4 times obtains
To Si-Y eutectic alloy mother's ingots.
Step 2：Clamping assembles.Si-Y eutectic alloy mother's ingots are broken for fritter of the equivalent diameter less than 3mm to be placed in just
In beautiful pipe.Corundum pipe size isWall thickness is 1mm.Corundum equipped with Si-Y eutectic alloy mother's ingots is effective
Stainless joint is fixed in the lever base of directional solidification furnace, and downward pull in advance, and alundum tube lower end 10mm is made to be immersed in
In cooling bay equipped with Ga-In-Sn aluminium alloys.The muff that refractory brick is made is set around alundum tube.
Step 3：Melting and solidification.Vacuum degree in directional solidification furnace is evacuated to 1 × 10-3Pa is simultaneously kept, and is filled with Ar gas.
Heating power supply heating sample is opened, detailed process is：With the melting electric current of 20A, make to rise to 500 DEG C in stove, and keep the temperature 15min；
Make to rise to 900 DEG C in stove with the melting electric current of 50A after heat preservation, and keeps the temperature 15min；Continue, with 110A melting electric currents, to make stove
1380 DEG C are inside risen to, 45min is kept the temperature.Start pull rod device after heat preservation, make sample with the rate of 0.4mm/min from top to bottom
It is mobile, temperature gradient is maintained at 170K/cm, realizes the continuous solidification of material.The continuous solidification process lasts up to entirely
Portion's alundum tube, which submerges in cooling bay, to be terminated.
After solidification, microexamination is carried out to tissue, is all organized as uniform band-like eutectic structure, and do not have in organizing
With the presence of any coarse primary Si phase, meet infiltration alloy requirement.
Example IV
The present embodiment be it is a kind of by solidification rate control in the range of 0.5~1.6mm/min, temperature gradient 190K/
Cm, obtains the infiltration Si-Y eutectic alloys of uniform transition tissue, and detailed process includes the following steps：
Step 1：It is prepared by base material.The Y powder that the Si powder and purity that are 99999% using purity are 99999% is pressed as raw material
Female ingot raw material of Si-18at%Y is made according to eutectic composition.Batch mixing briquetting is placed in vacuum non-consumable arc-melting furnace, and
Vacuum degree in stove is set to be consistently less than 1 × 10-3Pa.Melting electric current is set as 100A, the melt time is 2min, and melt back 4 times obtains
To Si-Y eutectic alloy mother's ingots.
Step 2：Clamping assembles.Si-Y eutectic alloy mother's ingots are broken for fritter of the equivalent diameter less than 3mm to be placed in just
In beautiful pipe.Corundum pipe size isWall thickness is 1mm.Corundum equipped with Si-Y eutectic alloy mother's ingots is effective
Stainless joint is fixed in the lever base of directional solidification furnace, and downward pull in advance, and alundum tube lower end 10mm is made to be immersed in
In cooling bay equipped with Ga-In-Sn aluminium alloys.The muff that refractory brick is made is set around alundum tube.
Step 3：Melting and solidification.Vacuum degree in directional solidification furnace is evacuated to 1 × 10-3Pa is simultaneously kept, and is filled with Ar gas.
Heating power supply heating sample is opened, detailed process is：With the melting electric current of 20A, make to rise to 500 DEG C in stove, and keep the temperature 15min；
Make to rise to 900 DEG C in stove with the melting electric current of 50A after heat preservation, and keeps the temperature 15min；Continue, with 115A melting electric currents, to make stove
1400 DEG C are inside risen to, 50min is kept the temperature.Start pull rod device after heat preservation, make sample with the rate of 0.6mm/min from top to bottom
It is mobile, temperature gradient is maintained at 190K/cm, realizes the continuous solidification of material.The continuous solidification process lasts up to entirely
Portion's alundum tube, which submerges in cooling bay, to be terminated.
After solidification, microexamination is carried out to tissue, it is total with island eutectic structure that tissue shows band-like eutectic structure
The transition tissue that the pattern deposited, i.e. banded structure are developed to island structure.There is no any coarse primary Si phase to exist in tissue,
Meet infiltration alloy requirement.
Embodiment five
The present embodiment be it is a kind of by solidification rate control in the range of 0.5~1.6mm/min, temperature gradient 200K/
Cm, obtains the infiltration Si-Y eutectic alloys of uniform transition tissue, and detailed process includes the following steps：
Step 1：It is prepared by base material.The Y powder that the Si powder and purity that are 99999% using purity are 99999% is pressed as raw material
Female ingot raw material of Si-18at%Y is made according to eutectic composition.Batch mixing briquetting is placed in vacuum non-consumable arc-melting furnace, and
Vacuum degree in stove is set to be consistently less than 1 × 10-3Pa.Melting electric current is set as 100A, the melt time is 2min, and melt back 4 times obtains
To Si-Y eutectic alloy mother's ingots.
Step 2：Clamping assembles.Si-Y eutectic alloy mother's ingots are broken for fritter of the equivalent diameter less than 3mm to be placed in just
In beautiful pipe.Corundum pipe size isWall thickness is 1mm.Corundum equipped with Si-Y eutectic alloy mother's ingots is effective
Stainless joint is fixed in the lever base of directional solidification furnace, and downward pull in advance, and alundum tube lower end 10mm is made to be immersed in
In cooling bay equipped with Ga-In-Sn aluminium alloys.The muff that refractory brick is made is set around alundum tube.
Step 3：Melting and solidification.Vacuum degree in directional solidification furnace is evacuated to 1 × 10-3Pa is simultaneously kept, and is filled with Ar gas.
Heating power supply heating sample is opened, detailed process is：With the melting electric current of 20A, make to rise to 500 DEG C in stove, and keep the temperature 15min；
Make to rise to 900 DEG C in stove with the melting electric current of 50A after heat preservation, and keeps the temperature 15min；Continue, with 120A melting electric currents, to make stove
1450 DEG C are inside risen to, 50min is kept the temperature.Start pull rod device after heat preservation, make sample with the rate of 1.0mm/min from top to bottom
It is mobile, temperature gradient is maintained at 200K/cm, realizes the continuous solidification of material.The continuous solidification process lasts up to entirely
Portion's alundum tube, which submerges in cooling bay, to be terminated.
After solidification, microexamination is carried out to tissue, it is total with island eutectic structure that tissue shows band-like eutectic structure
The transition tissue that the pattern deposited, i.e. banded structure are developed to island structure.There is no any coarse primary Si phase to exist in tissue,
Meet infiltration alloy requirement.
Embodiment six
The present embodiment be it is a kind of by solidification rate control in the range of 0.5~1.6mm/min, temperature gradient 210K/
Cm, obtains the infiltration Si-Y eutectic alloys of uniform transition tissue, and detailed process includes the following steps：
Step 1：It is prepared by base material.The Y powder that the Si powder and purity that are 99999% using purity are 99999% is pressed as raw material
Female ingot raw material of Si-18at%Y is made according to eutectic composition.Batch mixing briquetting is placed in vacuum non-consumable arc-melting furnace, and
Vacuum degree in stove is set to be consistently less than 1 × 10-3Pa.Melting electric current is set as 100A, the melt time is 2min, and melt back 4 times obtains
To Si-Y eutectic alloy mother's ingots.
Step 2：Clamping assembles.Si-Y eutectic alloy mother's ingots are broken for fritter of the equivalent diameter less than 3mm to be placed in just
In beautiful pipe.Corundum pipe size isWall thickness is 1mm.Corundum equipped with Si-Y eutectic alloy mother's ingots is effective
Stainless joint is fixed in the lever base of directional solidification furnace, and downward pull in advance, and alundum tube lower end 10mm is made to be immersed in
In cooling bay equipped with Ga-In-Sn aluminium alloys.The muff that refractory brick is made is set around alundum tube.
Step 3：Melting and solidification.Vacuum degree in directional solidification furnace is evacuated to 1 × 10-3Pa is simultaneously kept, and is filled with Ar gas.
Heating power supply heating sample is opened, detailed process is：With the melting electric current of 20A, make to rise to 500 DEG C in stove, and keep the temperature 15min；
Make to rise to 900 DEG C in stove with the melting electric current of 50A after heat preservation, and keeps the temperature 15min；Continue, with 122A melting electric currents, to make stove
1470 DEG C are inside risen to, 50min is kept the temperature.Start pull rod device after heat preservation, make sample with the rate of 1.5mm/min from top to bottom
It is mobile, temperature gradient is maintained at 210K/cm, realizes the continuous solidification of material.The continuous solidification process lasts up to entirely
Portion's alundum tube, which submerges in cooling bay, to be terminated.
After solidification, microexamination is carried out to tissue, it is total with island eutectic structure that tissue shows band-like eutectic structure
The transition tissue that the pattern deposited, i.e. banded structure are developed to island structure.There is no any coarse primary Si phase to exist in tissue,
Meet infiltration alloy requirement.
Embodiment seven
The present embodiment be it is a kind of by solidification rate control in the range of 1.6~3.0mm/min, temperature gradient 210K/
Cm, obtains the infiltration Si-Y eutectic alloys of uniform full island structure, and detailed process includes the following steps：
Step 1：It is prepared by base material.The Y powder that the Si powder and purity that are 99999% using purity are 99999% is pressed as raw material
Female ingot raw material of Si-18at%Y is made according to eutectic composition.Batch mixing briquetting is placed in vacuum non-consumable arc-melting furnace, and
Vacuum degree in stove is set to be consistently less than 1 × 10-3Pa.Melting electric current is set as 100A, the melt time is 2min, and melt back 4 times obtains
To Si-Y eutectic alloy mother's ingots.
Step 2：Clamping assembles.Si-Y eutectic alloy mother's ingots are broken for fritter of the equivalent diameter less than 3mm to be placed in just
In beautiful pipe.Corundum pipe size isWall thickness is 1mm.Corundum equipped with Si-Y eutectic alloy mother's ingots is effective
Stainless joint is fixed in the lever base of directional solidification furnace, and downward pull in advance, and alundum tube lower end 10mm is made to be immersed in
In cooling bay equipped with Ga-In-Sn aluminium alloys.The muff that refractory brick is made is set around alundum tube.
Step 3：Melting and solidification.Vacuum degree in directional solidification furnace is evacuated to 1 × 10-3Pa is simultaneously kept, and is filled with Ar gas.
Heating power supply heating sample is opened, detailed process is：With the melting electric current of 20A, make to rise to 500 DEG C in stove, and keep the temperature 15min；
Make to rise to 900 DEG C in stove with the melting electric current of 50A after heat preservation, and keeps the temperature 15min；Continue, with 125A melting electric currents, to make stove
1490 DEG C are inside risen to, 55min is kept the temperature.Start pull rod device after heat preservation, make sample with the rate of 1.9mm/min from top to bottom
It is mobile, temperature gradient is maintained at 210K/cm, realizes the continuous solidification of material.The continuous solidification process lasts up to entirely
Portion's alundum tube, which submerges in cooling bay, to be terminated.
After solidification, microexamination is carried out to tissue, is all organized as uniform island eutectic structure, and do not have in organizing
With the presence of any coarse primary Si phase, meet infiltration alloy requirement.
Embodiment eight
The present embodiment be it is a kind of by solidification rate control in the range of 1.6~3.0mm/min, temperature gradient 225K/
Cm, obtains the infiltration Si-Y eutectic alloys of uniform full island structure, and detailed process includes the following steps：
Step 1：It is prepared by base material.The Y powder that the Si powder and purity that are 99999% using purity are 99999% is pressed as raw material
Female ingot raw material of Si-18at%Y is made according to eutectic composition.Batch mixing briquetting is placed in vacuum non-consumable arc-melting furnace, and
Vacuum degree in stove is set to be consistently less than 1 × 10-3Pa.Melting electric current is set as 100A, the melt time is 2min, and melt back 4 times obtains
To Si-Y eutectic alloy mother's ingots.
Step 2：Clamping assembles.Si-Y eutectic alloy mother's ingots are broken for fritter of the equivalent diameter less than 3mm to be placed in just
In beautiful pipe.Corundum pipe size isWall thickness is 1mm.Corundum equipped with Si-Y eutectic alloy mother's ingots is effective
Stainless joint is fixed in the lever base of directional solidification furnace, and downward pull in advance, and alundum tube lower end 10mm is made to be immersed in
In cooling bay equipped with Ga-In-Sn aluminium alloys.The muff that refractory brick is made is set around alundum tube.
Step 3：Melting and solidification.Vacuum degree in directional solidification furnace is evacuated to 1 × 10-3Pa is simultaneously kept, and is filled with Ar gas.
Heating power supply heating sample is opened, detailed process is：With the melting electric current of 20A, make to rise to 500 DEG C in stove, and keep the temperature 15min；
Make to rise to 900 DEG C in stove with the melting electric current of 50A after heat preservation, and keeps the temperature 15min；Continue, with 130A melting electric currents, to make stove
1520 DEG C are inside risen to, 55min is kept the temperature.Start pull rod device after heat preservation, make sample with the rate of 2.5mm/min from top to bottom
It is mobile, temperature gradient is maintained at 225K/cm, realizes the continuous solidification of material.The continuous solidification process lasts up to entirely
Portion's alundum tube, which submerges in cooling bay, to be terminated.
After solidification, microexamination is carried out to tissue, is all organized as uniform island eutectic structure, and do not have in organizing
With the presence of any coarse primary Si phase, meet infiltration alloy requirement.
Embodiment nine
The present embodiment be it is a kind of by solidification rate control in the range of 1.6~3.0mm/min, temperature gradient 240K/
Cm, obtains the infiltration Si-Y eutectic alloys of uniform full island structure, and detailed process includes the following steps：
Step 1：It is prepared by base material.The Y powder that the Si powder and purity that are 99999% using purity are 99999% is pressed as raw material
Female ingot raw material of Si-18at%Y is made according to eutectic composition.Batch mixing briquetting is placed in vacuum non-consumable arc-melting furnace, and
Vacuum degree in stove is set to be consistently less than 1 × 10-3Pa.Melting electric current is set as 100A, the melt time is 2min, and melt back 4 times obtains
To Si-Y eutectic alloy mother's ingots.
Step 2：Clamping assembles.Si-Y eutectic alloy mother's ingots are broken for fritter of the equivalent diameter less than 3mm to be placed in just
In beautiful pipe.Corundum pipe size isWall thickness is 1mm.Corundum equipped with Si-Y eutectic alloy mother's ingots is effective
Stainless joint is fixed in the lever base of directional solidification furnace, and downward pull in advance, and alundum tube lower end 10mm is made to be immersed in
In cooling bay equipped with Ga-In-Sn aluminium alloys.The muff that refractory brick is made is set around alundum tube.
Step 3：Melting and solidification.Vacuum degree in directional solidification furnace is evacuated to 1 × 10-3Pa is simultaneously kept, and is filled with Ar gas.
Heating power supply heating sample is opened, detailed process is：With the melting electric current of 20A, make to rise to 500 DEG C in stove, and keep the temperature 15min；
Make to rise to 900 DEG C in stove with the melting electric current of 50A after heat preservation, and keeps the temperature 15min；Continue, with 140A melting electric currents, to make stove
1570 DEG C are inside risen to, 55min is kept the temperature.Start pull rod device after heat preservation, make sample with the rate of 3.0mm/min from top to bottom
It is mobile, temperature gradient is maintained at 240K/cm, realizes the continuous solidification of material.The continuous solidification process lasts up to entirely
Portion's alundum tube, which submerges in cooling bay, to be terminated.
After solidification, microexamination is carried out to tissue, is all organized as uniform island eutectic structure, and do not have in organizing
With the presence of any coarse primary Si phase, meet infiltration alloy requirement.
According to embodiment result it can be concluded that obtaining the melting for meeting the Si-Y eutectic alloys uniform formation that infiltration requires
Technological parameter is：0.1~3.0mm/min of solidification rate, temperature gradient are 150~240K/cm.The wherein solidification speed of banded structure
Rate range is 0.1~0.5mm/min, 150~180K/cm of temperature gradient；Obtain the solidifying of the band-like transition tissue developed to island
Gu speed range is 0.5~1.6mm/min, 180~210K/cm of temperature gradient；Obtaining the solidification rate of uniform island structure is
1.6~3.0mm/min, 210~240K/cm of temperature gradient.
Claims (5)
1. a kind of preparation of reactive infiltration Si-Y alloys and tissue modulation method, which is characterized in that detailed process is：
Step 1：It is prepared by base material；
Step 2：Clamping assembles；
Step 3：Melting and solidification：Vacuum degree in directional solidification furnace is evacuated to 1 × 10-3Pa is simultaneously kept, and is filled with Ar gas；It opens and adds
Thermoelectric generator heating sample is gradually increased melting electric current and is heated to 1300~1570 DEG C in a manner of ladder-elevating temperature, keeps the temperature 40min；
Start pull rod device after heat preservation, sample is solidified with the rate of 0.1~3.0mm/min, and temperature gradient is kept in draw process
In 150~240K/cm, the continuous solidification of material is realized；Directional solidification process is until whole alundum tubes submerge in cooling bay and terminate.
2. the preparation of reactive infiltration as described in claim 1 Si-Y alloys and tissue modulation method, which is characterized in that base material system
When standby, it is Si powder and Y powder as raw material using purity, female ingot raw material of Si-18at%Y is made according to eutectic composition；Batch mixing pressure
Block is placed in vacuum non-consumable arc-melting furnace, carries out melt back four times to female ingot raw material, it is female to obtain Si-Y eutectic alloys
Ingot；The melting electric current is 100A, and the melt time is 2min.
3. the preparation of reactive infiltration as claimed in claim 2 Si-Y alloys and tissue modulation method, which is characterized in that the Si
The purity of powder is 99999%, and the purity of the Y powder is 99999%.
4. the preparation of reactive infiltration as described in claim 1 Si-Y alloys and tissue modulation method, which is characterized in that clamping fills
Si-Y eutectic alloy mother's ingots are broken into fritter and are placed in alundum tube by timing；To the corundum equipped with Si-Y eutectic alloy mother's ingots
Downward pull is managed, alundum tube lower end 10mm is made to be immersed in the cooling bay equipped with Ga-In-Sn aluminium alloys；Have on the alundum tube
Muff, to realize the temperature gradient more than 140K/cm.
5. the preparation of reactive infiltration as described in claim 1 Si-Y alloys and tissue modulation method, it is characterised in that described molten
The detailed process of ladder-elevating temperature is to keep the melting electric current of 20A when melting, and makes to rise to 500 DEG C in stove, and keep the temperature 15min；Heat preservation knot
Make to continue to rise to 900 DEG C in stove with the melting electric current of 50A after beam, and keeps the temperature 15min；Continue, with 100~140A melting electric currents, to make
1300~1570 DEG C are risen in stove.
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|---|---|---|---|---|
| CN116789465A (en) * | 2023-07-19 | 2023-09-22 | 西北工业大学 | Preparation method of quaternary Si-Y-B-Yb coating with self-healing and corrosion resistance |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102051668A (en) * | 2010-11-04 | 2011-05-11 | 西北工业大学 | 10<5> K/cm temperature gradient directional solidification device and directional solidification method |
| CN102888649A (en) * | 2012-10-10 | 2013-01-23 | 西北工业大学 | Method for preparing Si-TaSi2 eutectic in-situ composite material |
| CN107523733A (en) * | 2017-09-04 | 2017-12-29 | 北京航空航天大学 | A kind of directional solidification Nb Si based multicomponent alloys |
-
2018
- 2018-07-09 CN CN201810742279.9A patent/CN108796253A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102051668A (en) * | 2010-11-04 | 2011-05-11 | 西北工业大学 | 10<5> K/cm temperature gradient directional solidification device and directional solidification method |
| CN102888649A (en) * | 2012-10-10 | 2013-01-23 | 西北工业大学 | Method for preparing Si-TaSi2 eutectic in-situ composite material |
| CN107523733A (en) * | 2017-09-04 | 2017-12-29 | 北京航空航天大学 | A kind of directional solidification Nb Si based multicomponent alloys |
Non-Patent Citations (1)
| Title |
|---|
| JINGUANG LI ET AL: "Competitive growth of Si and YSi2 phases in a eutectic Si-Y alloy prepared by the Bridgeman method", 《CERAMICS INTERNATIONAL》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116789465A (en) * | 2023-07-19 | 2023-09-22 | 西北工业大学 | Preparation method of quaternary Si-Y-B-Yb coating with self-healing and corrosion resistance |
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