CN110487788A - A kind of assessment method of single crystal super alloy low-angle boundary formability - Google Patents
A kind of assessment method of single crystal super alloy low-angle boundary formability Download PDFInfo
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- CN110487788A CN110487788A CN201910631742.7A CN201910631742A CN110487788A CN 110487788 A CN110487788 A CN 110487788A CN 201910631742 A CN201910631742 A CN 201910631742A CN 110487788 A CN110487788 A CN 110487788A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/84—Systems specially adapted for particular applications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/84—Systems specially adapted for particular applications
- G01N2021/8477—Investigating crystals, e.g. liquid crystals
Abstract
The present invention relates to Investment casting technology field, specially a kind of assessment method of single crystal super alloy low-angle boundary formability.Specific step is as follows for the assessment method: (1) design has the mold of the variable cross-section of different platform length and constant altitude, ceramic material and wax is combined, and corresponding formwork is made；(2) the single crystal super alloy casting of a variety of alloys is made in directional solidification furnace；(3) single crystal super alloy of different cross section is subjected to crystal orientation test；(4) angle difference of low angle boundary in each cross section, the low angle boundary Forming ability of quantitative assessment single crystal super alloy are analyzed.Differential seat angle between crystal boundary is bigger, shows that the formation low angle boundary tendentiousness of alloy is stronger.Thus under the premise of not using analogue technique, it can be with the Forming ability of quantitatively characterizing difference single crystal super alloy low-angle boundary.
Description
Technical field:
The present invention relates to Investment casting technology field, specially a kind of single crystal super alloy low-angle boundary formability
Assessment method.
Background technique:
Single crystal super alloy is in Aeronautics and Astronautics, the energy, nuclear industry, petrochemical industry, national defence weapon equipment and the development of the national economy
Indispensable key structure material.Due to the increasingly promotion of engine efficiency, higher want is proposed to the structure of single crystal blade
It asks, due to single crystal super alloy modular construction complex, the deflection and phase of multiple dendrite is related in directional solidification process
It meets, and forms low-angle boundary.Low-angle boundary is reintroduced back to transverse grain boundaries as a kind of defect(ive) structure, destroys monocrystalline high temperature
The tissue integrity of alloy vane significantly reduces the mechanical behavior under high temperature of alloy, becomes the major hidden danger during blade is on active service.
The formability of single crystal super alloy low-angle boundary becomes a FAQs in single crystal super alloy R&D process,
Thus dead head setting, seeding work in single crystal super alloy research and development, component selection, modular construction design, component preparation process
The processes such as skill need to evaluate the formability of the low-angle boundary of single crystal super alloy, be conducive to improve yield rate and
Reduce production cost.
Summary of the invention:
The purpose of the present invention is to provide a kind of assessment method of single crystal super alloy low-angle boundary formability, solutions
Certainly single crystal super alloy low-angle boundary formability is difficult to the problem of evaluating, and uses this method that can be conducive to for monocrystalline high temperature
The selection of alloy material provides foundation, and guides the design and production of single crystal super alloy component, reduce single crystal components research and development at
Sheet and lead time.
The technical scheme is that
A kind of assessment method of single crystal super alloy low-angle boundary formability is managed according to the classics of directional solidification
By dendrite can deflect in alloy graining process, just will form low-angle boundary when two dendrites meet, in monocrystalline
High temperature alloy by the growth course of design single crystal super alloy dendrite, make to occur between dendrite it is different degrees of meet,
So that it forms low angle boundary when the dendrite of homogeneous does not meet in process of setting, using forming not highly single crystal super alloy
The mold of casting so that low order dendrite meets from different high order dendrites, and is formed by adjusting the direction of growth of dendrite
Low-angle boundary carries out orientation detection and evaluation by the region met to dendrite, and evaluation single crystal super alloy low-angle is brilliant
The formability on boundary.
The assessment method of the single crystal super alloy low-angle boundary formability, the angular values of low-angle boundary
It is bigger, show that the formability of the low-angle boundary of alloy is stronger.
The assessment method of the single crystal super alloy low-angle boundary formability, the mould of single crystal super alloy casting
Tool is that variable cross-section is step-like, and the vertical main solidification path side of mold has the platform of different length, neighbouring two sections of differences
It is connected between length platform outer end by vertical high order dendrite growth channel, for connecting neighbouring two sections of different lengths
The high order dendrite growth channel sized of platform is identical, position staggers successively.
The assessment method of the single crystal super alloy low-angle boundary formability, the cross section ruler of main solidification path
Very little is 2~20mm, and the shape of cross section is square, rectangle, diamond shape, polygon, circle, ellipse or revolving body；
The shape of platform cross section is square, rectangle, diamond shape, polygon, ellipse or revolving body；High order dendrite growth is logical
The shape of road cross section is square, rectangle, diamond shape, polygon, ellipse or revolving body, and cross sectional dimensions is 10~
30mm is highly 25~40mm.
The assessment method of the single crystal super alloy low-angle boundary formability, each mold have different put down
10~30mm of platform length, having constant altitude between neighbouring two sections of platforms is 25~40mm.
The assessment method of the single crystal super alloy low-angle boundary formability, along directional solidification from bottom to top
The land lengths in direction, mold are gradually reduced to 10mm along stairstepping by 30mm；Wherein, make different idols after land lengths variation
The dendrite of number meets in platform.
The assessment method of the single crystal super alloy low-angle boundary formability, being assessed material is nickel-based monocrystal
High temperature alloy, the influence that low-angle boundary is formed for evaluation platform length.
The assessment method of the single crystal super alloy low-angle boundary formability, the specific steps are as follows:
(1) mold design
The step-like variable section structure of mold, mold have different land lengths and constant altitude, along determining from bottom to top
To solidification direction, land lengths are gradually reduced to 10mm along stairstepping by 30mm, and the height of every section of platform is 25~40mm；
(2) prepared by cere mould group
Using mold wax is suppressed into wax-pattern together, wax-pattern is placed in water bath, water temperature is 20~25 DEG C, the time 30
~60 minutes, wax-pattern is assembled into cere mould group by radial circumferentially disposing way and running gate system bonding；
(3) prepared by ceramic shell mould
Using the nano-oxide for adding mass fraction 0.1~1% in traditional ceramics formwork composition proportion, pass through hanging
Technique prepares formwork, and then formwork is put into Muffle furnace and is heated, and is heated to be 600~1000 DEG C, heating use heats up step by step
Heating means are warming up to 100~150 DEG C from room temperature with the heating rate of 2~5 DEG C/min, 0.1~1 hour are kept the temperature, then by mould
Shell, which verts 3~45 °, continues heat preservation 0.1~1 hour, and then formwork verts 6~90 ° to opposite direction again, and it is small to continue heat preservation 0.1~1
When；Muffle furnace is warming up to 280~320 DEG C again with the heating rate of 5~10 DEG C/min, keeps the temperature 0.5~2 hour, with 10~20 DEG C/
The heating rate of min is warming up to 800~1000 DEG C, keeps the temperature 0.5~3 hour, obtains qualified ceramic shell mould；
(4) alloy is poured
Under identical curing condition, it is poured single crystal super alloy, prepares the single crystal super alloy casting of ingredient；
(5) in platform low-angle boundary observation
Single crystal super alloy casting is subjected to macrocorrosion and crystal orientation test, low-angle boundary angle in observation platform
The size of difference；The angle of small angle grain boundary in land lengths and platform by comparing different single crystal super alloy low-angle boundaries
Difference, the tendentiousness of quantitative analysis single crystal super alloy low-angle boundary.
The assessment method of the single crystal super alloy low-angle boundary formability, nano-oxide be aluminium oxide,
The one or more of yttrium oxide, hafnium oxide, zirconium oxide, calcium oxide, titanium oxide, chromium oxide, the size of nano-oxide are 5
~50nm.
Design philosophy of the invention is:
The method of the present invention is based on that a degree of deflection can be generated in dendrite branching process in alloy graining process, in list
The even numbers generation dendrites such as 2 dendrites of brilliant superalloy design and 4,6,8 are grown into platform simultaneously, then phase occurs in platform
It meets, it, can be with quantitatively characterizing heterogeneity, the list of different generation dendrites under the premise of not changing curing condition and analogue technique
The Forming ability of the low-angle boundary of brilliant high temperature alloy.Therefore, the maximum feature of the present invention be can quantitative assessment monocrystalline high temperature close
The formability of golden low-angle boundary.
The invention has the advantages and beneficial effects that:
1, the present invention meeting and easily form low-angle according to generation dendrites different in single crystal super alloy process of setting
The phenomenon that crystal boundary, design have different platform length and height mold, by the variation of land lengths and the adjustment of height, 2 times
The even numbers generation dendrite such as dendrite and 4,6,8 meets and forms low-angle boundary, and evaluation single crystal super alloy low-angle is brilliant
Boundary at tendentiousness, the evaluation result of this method can be used as alloy selection, monocrystalline component preparation technology parameter and dead head are set
The foundation of meter.
2, single crystal super alloy casting of the present invention has different land lengths and height, can study podium level to small angle
Spend crystal boundary at tendentious influence, can also different branch crystal phases when preparing single crystal samples under identical orientation curing condition
Influence of the case where chance to low-angle boundary formability is conducive to instruct monocrystalline component production technology.
3, operation of the present invention is simple, design rationally, strong operability, can significantly reduce single crystal super alloy component research and development and
Cost in production process, and this method is at low cost, is conducive to promote and apply.
Detailed description of the invention:
Fig. 1 is single crystal super alloy low-angle boundary evaluation structure schematic diagram.In figure, 1 is main solidification path, and 2 platforms are used
2 dendrites or 4,6,8 inferior dendrites in different length platform meet, and 3 be high order dendrite growth channel, use
In offer high order dendrite.
Fig. 2 is single crystal super alloy low-angle boundary macro morphology.
Fig. 3 is the microstructure of single crystal super alloy low-angle boundary.
Fig. 4 is the relationship of dendrite number and low-angle boundary.
Specific embodiment:
In the specific implementation process, for the present invention according in single crystal super alloy process of setting, low order dendrite branches out height
Secondary dendrite, high order dendrite and low order dendrite form low-angle boundary when meeting, and 2 trees are designed in single crystal super alloy
The even numbers generation dendrite such as dendrite and 4,6,8 is grown into platform simultaneously, by platform the differential seat angle of low-angle boundary it is big
It is small, evaluate the formability of single crystal super alloy low-angle boundary.This method comprises: (1) design has different platform length
With the mold of the variable cross-section of constant altitude, ceramic material and wax are combined, and corresponding formwork is made；(2) solidifying in orientation
Gu the single crystal super alloy casting of a variety of alloys is made in furnace；(3) single crystal super alloy of different cross section is subjected to crystal orientation
Test；(4) angle difference of low angle boundary in each cross section is analyzed, the low angle boundary of quantitative assessment single crystal super alloy forms energy
Power.Differential seat angle between crystal boundary is bigger, shows that the formation low angle boundary tendentiousness of alloy is stronger.To not use analogue technique
Under the premise of, it can be with the Forming ability of quantitatively characterizing difference single crystal super alloy low-angle boundary.
The assessment method of single crystal super alloy recrystallization formability of the present invention, the specific steps are as follows:
1. mold design
As shown in Figure 1, the mold of single crystal super alloy casting is that variable cross-section is step-like, the vertical main solidification path 1 of mold
Side has the platform 2 of different length, passes through vertical high order dendrite between 2 outer end of neighbouring two sections of different length platforms
Channel 3 is grown to be connected, 3 sizes of high order dendrite growth channel for connecting neighbouring two sections of different length platforms 2 are identical,
Position staggers successively.Along directional solidification direction from bottom to top, different land lengths are gradually reduced by 30mm along stairstepping
Having constant altitude to 10mm, between neighbouring two sections of platforms is 25~40mm, brilliant for single crystal super alloy low-angle
Boundary's formability influences.
2. prepared by cere mould group
Paraffin is pressed into wax-pattern using mold, the wax-pattern of each single crystal super alloy casting is placed in water bath,
Water temperature is 20~25 DEG C, and the time is 30~60 minutes, and wax-pattern is filled by radial circumferentially disposing way and running gate system bonding
It is made into cere mould group.
3. prepared by ceramic shell mould
Using the nano-oxide for adding mass fraction 0.1~1% in traditional ceramics formwork composition proportion, nano-oxide
Effect be: reduce the sintering temperature of ceramic shell, to control the deflection of shell, reduce the deformation of platform, exclude by type
Shell deforms and introduces dendritic growth and deflect, and introduces low angle boundary.Nano-oxide can be aluminium oxide, yttrium oxide, oxidation
The size of hafnium, zirconium oxide, calcium oxide, titanium oxide or chromium oxide etc., nano-oxide is 5~50nm, passes through the technique system of hanging
Formwork, is then put into Muffle furnace and heats by standby formwork, is heated to be 600~1000 DEG C, heating is using the heating side heated up step by step
Method: 100~150 DEG C are warming up to from room temperature with the heating rate of 2~5 DEG C/min, 0.1~1 hour is kept the temperature, then formwork verts
3~45 ° are continued heat preservation 0.1~1 hour, and formwork verts 6~90 ° to opposite direction again then and continues heat preservation 0.1~1 hour.Horse
Not furnace rises 300 DEG C again with the heating rate of 5~10 DEG C/min, keeps the temperature 1 hour, rises 800 with the heating rate of 10~20 DEG C/min
~1000 DEG C, 0.5~3 hour is kept the temperature, obtains qualified ceramic shell mould；Wherein, the effect of heating of heating up step by step is: promoting shell
The abundant sintering of middle ceramic material, and after shell verts certain angle, be conducive to the exclusion of the materials such as residual carbon in wax material,
Be conducive to exclude the interference of residual carbon in wax material.
4. alloy is poured
Under identical curing condition, it is poured different single crystal super alloys, the monocrystalline high temperature for preparing different wall thickness closes
Golden casting.
5. the observation of low-angle boundary in platform
Single crystal super alloy casting is subjected to macrocorrosion and crystal orientation test, low-angle boundary angle in observation platform
The size of difference；The angle of small angle grain boundary in land lengths and platform by comparing different single crystal super alloy low-angle boundaries
Difference, the tendentiousness of quantitative analysis single crystal super alloy low-angle boundary.
In the following, being further elaborated on by embodiment and attached drawing to the present invention.
Embodiment
In the present embodiment, according to designed casting single crystal high temperature alloy, macro morphology is shown in that Fig. 2, mold are variable cross-section platform
Scalariform, mold have constant altitude between different land lengths and adjacent platforms, along directional solidification direction from bottom to top,
Its land lengths is gradually reduced to 10mm along stairstepping by 30mm, and the height between neighbouring two sections of platforms is 30mm.
Using the nano-oxide for adding mass fraction 0.5% in traditional ceramics formwork composition proportion, nano-oxide can
Think aluminium oxide, yttrium oxide, hafnium oxide, zirconium oxide, calcium oxide, titanium oxide or chromium oxide etc., the size of nano-oxide is 5~
50nm prepares formwork by the technique of hanging, then formwork is put into Muffle furnace and is heated, and is heated to be 900 DEG C, heating using by
The heating means of grade heating are warming up to 120 DEG C from room temperature with the heating rate of 3 DEG C/min, 0.5 hour are kept the temperature, then by formwork
It verts 30 ° and continues heat preservation 0.5 hour, formwork verts 30 ° to opposite direction again then and continues heat preservation 0.5 hour.Muffle furnace is again with 8
DEG C/heating rate of min rises 300 DEG C, 1 hour is kept the temperature, 900 DEG C is risen with the heating rate of 15 DEG C/min, keeps the temperature 2 hours, obtain
Qualified ceramic shell mould.
By taking DD407 nickel-base high-temperature single crystal alloy as an example, the shadow of single crystal super alloy low-angle boundary formability is introduced
It rings.
Single crystal hollow casting is 1500 DEG C in upper and lower area's temperature, and pulling rate is the list for preparing under the conditions of 3mm/min technological parameter
Brilliant high-temperature alloy casting.
As shown in Fig. 2-Fig. 3, after the pattern of Jing Dinggao macrocorrosion and electron backscattered Determination of Orientation, it can be seen that In
On first order platform, 2 dendrites meet with 4 dendrites, and the numerical value of low-angle boundary is about 0.5 degree, and with
The increase of podium level, 2 dendrites meet with 6 times, 8 inferior even-times dendrites respectively in platform, with platform height
The increase of degree, the angle of low-angle boundary is increasing in platform.
The course of work and result of the present invention are as follows:
The present invention has the mold of constant altitude between different platform length and adjacent platforms by design, and according to the mould
Tool prepares single crystal super alloy casting, and that realizes high order dendrite meets and forms low-angle boundary in platform, and analysis is not
With the size of the differential seat angle of low-angle boundary in level platform, the Forming ability of the low-angle boundary of quantitative assessment alloy is real
Selection low-angle boundary provides foundation at the weaker single crystal super alloy of tendentiousness in the production of border, while this method also helps list
Solidifying process optimizes in the research and development and monocrystalline components preparation process of brilliant high-temperature alloy material, reduces production cost.
As shown in figure 4, with the increase of platform, small angle it can be seen from the relationship of dendrite number and low-angle boundary
The angle of degree crystal boundary gradually increases, by about 0.5 ° of deflection angle of low-angle boundary on first order platform, to the tenth level-one platform
2.8 ° of deflection angle or so.
Embodiment the result shows that, the present invention have preparation process it is simple, it is low in cost the features such as, can solve monocrystalline high temperature
Alloy low-angle boundary is difficult to the problem of evaluating at tendentiousness, different single crystal super alloys in quantitative assessment directional solidification process
The Forming ability of low-angle boundary to be conducive to single crystal high-temperature alloy material research and development, and is optimization solidification work in actual production
Skill provides foundation.
Claims (9)
1. a kind of assessment method of single crystal super alloy low-angle boundary formability, which is characterized in that according to directional solidification
Classical theory, dendrite can deflect in alloy graining process, just will form low-angle crystalline substance when two dendrites meet
Boundary in single crystal super alloy by the growth course of design single crystal super alloy dendrite makes that different journeys occur between dendrite
Degree meets, so that it forms low angle boundary when the dendrite of homogeneous does not meet in process of setting, it is highly not single using being formed
The mold of brilliant high-temperature alloy casting, by adjusting the direction of growth of dendrite, so that low order dendrite and different high order dendrites
It meets, and forms low-angle boundary, orientation detection and evaluation are carried out by the region met to dendrite, evaluation monocrystalline high temperature closes
The formability of golden low-angle boundary.
2. the assessment method of single crystal super alloy low-angle boundary formability described in accordance with the claim 1, feature exist
In the angular values of low-angle boundary are bigger, show that the formability of the low-angle boundary of alloy is stronger.
3. the assessment method of single crystal super alloy low-angle boundary formability described in accordance with the claim 1, feature exist
In the mold of single crystal super alloy casting is that variable cross-section is step-like, and the vertical main solidification path side of mold has different length
Platform, be connected between neighbouring two sections of different length platforms outer end by vertical high order dendrite growth channel, be used for
The high order dendrite growth channel sized for connecting neighbouring two sections of different length platforms is identical, position staggers successively.
4. the assessment method of single crystal super alloy low-angle boundary formability described in accordance with the claim 3, feature exist
Be 2~20mm in the cross sectional dimensions of, main solidification path, the shape of cross section is square, rectangle, diamond shape, polygon,
Round, ellipse or revolving body；The shape of platform cross section is square, rectangle, diamond shape, polygon, ellipse or
Revolving body；The shape of high order dendrite growth channel cross-section is square, rectangle, diamond shape, polygon, ellipse or returns
Swivel, cross sectional dimensions are 10~30mm, are highly 25~40mm.
5. the assessment method of single crystal super alloy low-angle boundary formability described in accordance with the claim 3, feature exist
There is different 10~30mm of land lengths in, each mold, have between neighbouring two sections of platforms constant altitude be 25~
40mm。
6. the assessment method of single crystal super alloy low-angle boundary formability, feature exist according to claim 5
In along directional solidification direction from bottom to top, the land lengths of mold are gradually reduced to 10mm along stairstepping by 30mm；Wherein,
After land lengths variation the dendrite of different even numbers is met in platform.
7. the assessment method of single crystal super alloy low-angle boundary formability described in accordance with the claim 1, feature exist
In being assessed material is nickel-base high-temperature single crystal alloy, the influence formed for evaluation platform length to low-angle boundary.
8. the assessment method of single crystal super alloy low-angle boundary formability described in accordance with the claim 1, feature exist
In, the specific steps are as follows:
(1) mold design
The step-like variable section structure of mold, mold have different land lengths and constant altitude, solidifying along orientation from bottom to top
Gu direction, land lengths are gradually reduced to 10mm along stairstepping by 30mm, and the height of every section of platform is 25~40mm；
(2) prepared by cere mould group
Using mold wax is suppressed into wax-pattern together, wax-pattern is placed in water bath, water temperature is 20~25 DEG C, and the time is 30~60
Minute, wax-pattern is assembled into cere mould group by radial circumferentially disposing way and running gate system bonding；
(3) prepared by ceramic shell mould
Using the nano-oxide for adding mass fraction 0.1~1% in traditional ceramics formwork composition proportion, pass through the technique of hanging
Formwork is prepared, then formwork is put into Muffle furnace and is heated, is heated to be 600~1000 DEG C, heating is using the heating to heat up step by step
Method is warming up to 100~150 DEG C from room temperature with the heating rate of 2~5 DEG C/min, keeps the temperature 0.1~1 hour, then formwork inclines
Turn 3~45 ° and continue heat preservation 0.1~1 hour, formwork verts 6~90 ° to opposite direction again then and continues heat preservation 0.1~1 hour；
Muffle furnace is warming up to 280~320 DEG C again with the heating rate of 5~10 DEG C/min, 0.5~2 hour is kept the temperature, with 10~20 DEG C/min
Heating rate be warming up to 800~1000 DEG C, keep the temperature 0.5~3 hour, obtain qualified ceramic shell mould；
(4) alloy is poured
Under identical curing condition, it is poured single crystal super alloy, prepares the single crystal super alloy casting of ingredient；
(5) in platform low-angle boundary observation
Single crystal super alloy casting is subjected to macrocorrosion and crystal orientation test, low-angle boundary differential seat angle in observation platform
Size；The differential seat angle of small angle grain boundary in land lengths and platform by comparing different single crystal super alloy low-angle boundaries
It is different, the tendentiousness of quantitative analysis single crystal super alloy low-angle boundary.
9. the assessment method of single crystal super alloy low-angle boundary formability, feature exist according to claim 8
In, nano-oxide be aluminium oxide, yttrium oxide, hafnium oxide, zirconium oxide, calcium oxide, titanium oxide, chromium oxide one or two with
On, the size of nano-oxide is 5~50nm.
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