CN104975248B - Solution treatment method of third generation nickel-base single crystal high temperature alloy - Google Patents

Solution treatment method of third generation nickel-base single crystal high temperature alloy Download PDF

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CN104975248B
CN104975248B CN201510374344.3A CN201510374344A CN104975248B CN 104975248 B CN104975248 B CN 104975248B CN 201510374344 A CN201510374344 A CN 201510374344A CN 104975248 B CN104975248 B CN 104975248B
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temperature
solid solution
solution treatment
single crystal
uphill diffusion
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CN104975248A (en
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刘林
张琰斌
黄太文
杨振宇
张军
郭敏
苏海军
傅恒志
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Northwestern Polytechnical University
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Abstract

The invention discloses a solution treatment method of third generation nickel-base single crystal high temperature alloy. According to the solution treatment method, a conventional solution treatment of third generation nickel-base single crystal high temperature alloy is improved so as to avoid incipient melting of alloy in solution treatment processes, improve product mechanical properties, and increase finished product yield. According to the solution treatment method, in solution treatment processes, solution temperature after uphill diffusion is reduced, and the solution temperature is maintained to be lower than an incipient melting temperature which is reduced because of uphill diffusion, so that incipient melting is avoided. The solution treatment method is capable of avoiding incipient melting caused by uphill diffusion, eliminating holes and residual eutectic caused by incipient melting, and improving alloy mechanical properties; and in addition, finished product yield is increased obviously because of avoiding of incipient melting.

Description

A kind of solid solution treatment method of third generation nickel-base high-temperature single crystal alloy
Technical field
The present invention relates to third generation nickel-base high-temperature single crystal alloy Field of Heat-treatment, specifically change the solution treatment work of alloy Skill, it is to avoid the generation of incipient melting, improves yield rate and the properties of product of heat treated article.
Background technology
Third generation nickel-base high-temperature single crystal alloy refers to that the mass fraction of wherein re element is 4%~6%, and creep rupture life More than 100h under 1100 DEG C, load 150mpa.In recent years, China's space flight and aviation technology achieved the progress advanced by leaps and bounds, and Engine is the core component of space flight and aviation aircraft, therefore improves increasing it using temperature and having an high regard for specific potential of engine material Must go.Nickel-base high-temperature single crystal alloy is having good mechanical property at a temperature of the use of fusing point, thus extensive It is applied to engine.China have begun at present to research and develop energetically third generation nickel base single crystal high-temperature alloy material and achieve important enter Exhibition.Single crystal super alloy is done in dendrite after directional solidification has segregation with interdendritic, and interdendritic also has eutectic, and main Hardening constituent γ ' size and distribution are also very uneven, so before being taken into use will be through by solution treatment and Ageing Treatment The organization and performance to improve alloy for the heat treatment of composition.And the development with alloy, in alloy, refractory element content constantly carries Height, significantly improves the interdiffusion coefficient of each element in alloy, increases the as cast condition segregation of alloy, increases the difficulty of subsequent solution treatment Degree.Become big additionally, due to as cast condition segregation, interdendritic is easier incipient melting, reduces heat treatment window.And refractory element itself Diffusion coefficient exceeds the several order of magnitude of other elements, and the time that Homogenization Process needs and temperature greatly increase.
The incipient melting producing during solution treatment not only can form the lifting surface area that hole reduces material, and can produce very Many residual eutectic structures, substantially reduce the mechanical behavior under high temperature of alloy.Biography currently for third generation nickel-base high-temperature single crystal alloy System technique is to step up solid solubility temperature and temperature retention time, thus step up the initial melting temperature of alloy, in the generation of incipient melting Under the premise of higher temperature solid solution is carried out to alloy.Even if but the multistep that solution treatment is divided into solid solubility temperature continuous improvement is admittedly Molten, still it may happen that incipient melting.
Through to prior art literature search find: document " karunaratne m s a, cox d c, et al. The modelling of the microsegregation in cmsx-4superalloy that superalloys 2000 delivers And its homogenisation during heat treatment " have studied the problems such as incipient melting and uphill diffusion but not Refer to relation between the two.
Document " hegde, s.r., r.m.kearsey et al. in materials science and engineering:a, The designing homogenization solution heat treatments for single that 2010.527 deliver Crystal superalloys " is found that the incipient melting that uphill diffusion produces during leading to solution treatment, but does not specifically beg for By the change of just fusing point, but attempt to avoid uphill diffusion with higher temperature solution treated, this way there is no theoretical foundation, And do not homogenized in low temperature and likely result in the direct incipient melting in low melting point region in the higher direct solid solution of temperature.
A kind of third generation nickel-based monocrystal is all proposed high in Chinese patent cn1966750a, United States Patent (USP) us8696979b2 Temperature alloy solid solution treatment process, but do not refer to the incipient melting problem that uphill diffusion causes.
Chinese patent cn103352192a refers to solid solution treatment process design problem, but it does not refer to that uphill diffusion causes Incipient melting problem.
Content of the invention
There is incipient melting for during overcoming solution treatment present in prior art, lead to mechanical property and the finished product of product The deficiency that rate declines, the present invention proposes a kind of solid solution treatment method of third generation nickel-base high-temperature single crystal alloy.
The present invention comprises the concrete steps that:
Step 1, prepares third generation nickel-base high-temperature single crystal alloy coupon.
Step 2, time and its end time that simulation al element uphill diffusion occurs.Described simulation al element uphill diffusion The time occurring and its end time are to simulate third generation nickel-base high-temperature single crystal alloy coupon in multistep admittedly by dictra software The situation of diffusion under temperature conditionss in molten process.
Step 3, determines the temperature of solution treatment.When determining the temperature of solution treatment, it is first determined the uphill diffusion time The initial melting temperature of alloy in section, and this initial melting temperature is compared with the temperature of al element uphill diffusion time period in solution treatment, Decide whether to adjust the temperature of solution treatment according to comparing result.Detailed process is:
The first step. input third generation nickel-base high-temperature single crystal alloy at the end of the al element uphill diffusion obtaining by step 2 The content of each element at al constituent content maximum position in coupon, obtains this al unit according to the criterion of minimization of Gibbs free energy Melting temperature at cellulose content maximum position.Gone up a slope using the melting temperature at described al constituent content maximum position as al element The initial melting temperature of diffusion time section alloy.
Second step. by the solid solution temperature of the initial melting temperature obtaining and al element uphill diffusion time period in solution treatment It is compared, if solid solution temperature is less than initial melting temperature, incipient melting does not occur it was demonstrated that this solid solution temperature need not adjust, Enter step 4 and carry out solution treatment.If solid solution temperature is higher than described initial melting temperature, there is incipient melting, upward slope need to be reduced and expand The solid solution temperature of scattered time period is to described initial melting temperature 10 DEG C.
3rd step. whether the solid solution temperature after inspection reduces again is feasible.Replaced with the solid solution temperature after reducing Change the solid solution temperature of uphill diffusion time period in step 2, the process of repeat step 2, redefine al element uphill diffusion The time occurring and its end time, the first step and the second step laid equal stress in duplicate step, until the uphill diffusion time period is first Melting temperatur is less than this time period solid solution temperature, then choose the solution treatment that this temperature is the solution treatment uphill diffusion time period Temperature.
Step 4, solution treatment.Solid solution temperature according to determining is carried out to third generation nickel-base high-temperature single crystal alloy coupon Solution treatment.
Described third generation nickel-base high-temperature single crystal alloy coupon is placed in heat-treatment furnace.In heat-treatment furnace, by the third generation Nickel-base high-temperature single crystal alloy coupon rises to the solid solution temperature of the first step of routine and is incubated 1h from room temperature;Insulation is dropped after terminating The warm solid solubility temperature determining to step 3 is simultaneously incubated 2h;The solid solubility temperature of described determination is than the solid solution of the described conventional first step Treatment temperature is low 10 DEG C;Insulation is warmed up to the solid solution temperature of second step after terminating and is incubated 2h;Insulation terminates follow-up of continuing rising The warm solid solution temperature to the 3rd step is simultaneously incubated 3h;Insulation is warmed up to the solid solution temperature of the 4th step after terminating and is incubated 5h;Insulation terminates follow-up continuous to be warmed up to the solid solution temperature of the 5th step and be incubated 10h;Insulation terminates rear blow-on, by described the Three generations's nickel-base high-temperature single crystal alloy coupon is air cooled to room temperature, obtains the third generation nickel-base high-temperature single crystal alloy examination through solution treatment Rod.Described heating rate is 10 DEG C/min.
The purpose of the present invention is to improve a kind of third generation nickel-base high-temperature single crystal alloy solid solution treatment process, it is to avoid alloy is solid There is incipient melting, thus improving mechanical property and the yield rate of product in molten processing procedure.
The present invention, by the research to incipient melting mechanism of production, finds that not all elements are all during solution treatment From the big regional diffusion of constituent content to the little region of constituent content, but as the be shown with element of Fig. 1 is anti-from the low region of content It is diffused into the high region of content, makes this constituent content in the high region of constituent content further up, this phenomenon is referred to as going up a slope Diffusion.Although this phenomenon in high temperature alloy advantageously, it has been found that but its to solution treatment produce impact be often ignored, low The uphill diffusion of melting element al element particularly as shown in Figure 1 can reduce the fusing point of interdendritic fusing point script very low area, from And reducing the just fusing point of whole alloy, this just fusing point temperature is likely lower than solid solution temperature, and now solid solution temperature If still rising or remaining unchanged, incipient melting can occur.
The present invention is using a kind of work gradually rising different from solid solution temperature in traditional multistep solid solution treatment process Skill, but consider the reduction situation of initial melting temperature after uphill diffusion generation during solution treatment, according to the incipient melting temperature reducing Degree, to reduce solid solution temperature, is not to improve solid solution temperature always according to traditional solution treatment scheme.This fall The method of low solid solution temperature makes solid solution temperature be less than the initial melting temperature reducing due to uphill diffusion, it is to avoid incipient melting Produce.It is avoided that using the method for the present invention and is occurred by the incipient melting that uphill diffusion causes, thus eliminating the hole being produced by incipient melting And remnants eutectic, and then put forward heavy alloyed mechanical property, and avoiding additionally, due to incipient melting, the yield rate of product will significantly improve.
Organizing Fig. 5, Fig. 6, Fig. 7 and using the tissue Fig. 2 after solution treatment of the present invention, figure after contrast traditional solution process 3rd, Fig. 4 finds out, finds a large amount of holes significantly being produced by incipient melting using traditional solution in Fig. 5, Fig. 6, the Fig. 7 after processing, and All there is not incipient melting in Fig. 2, Fig. 3, Fig. 4 using solution treatment of the present invention.Illustrate that the solid solution treatment method of the present invention can be effective The generation avoiding incipient melting.
Brief description
Fig. 1 is the schematic diagram by uphill diffusion during the calculated solution treatment of simulation, and wherein a segment table shows upward slope Diffuser.
Fig. 2 is organization chart after embodiment 1 solution treatment.
Fig. 3 is organization chart after embodiment 2 solution treatment.
Fig. 4 is organization chart after embodiment 3 solution treatment.
Fig. 5 is alloy in embodiment 1 organization chart after traditional solution process, and wherein a represents the hole that incipient melting produces Hole.
Fig. 6 is alloy in embodiment 2 organization chart after traditional solution process, and wherein a represents the hole that incipient melting produces Hole.
Fig. 7 is alloy in embodiment 3 organization chart after traditional solution process, and wherein a represents the hole that incipient melting produces Hole.
Fig. 8 is the flow chart of the present invention.
Specific embodiment
Embodiment 1
In the present embodiment alloy, cr be 3.5%, mo be 1.5%, al be 6%, co be 9%, w be 6%, re be 4%, ta For 8%, hf be 1%, c be≤0.02%, balance of ni.Described percentage is mass percent.
The implementation steps of the described third generation nickel-base high-temperature single crystal alloy solution treatment that the present embodiment proposes are:
Step 1, prepares third generation nickel-base high-temperature single crystal alloy coupon.By by 3.5% cr, 1.5% mo, 6% al, 9% co, 6% w, 4% re, 8% ta, 1% hf ,≤0.02% c, and the foundry alloy of balance of ni composition passes through Conventional directional freeze method preparation becomes third generation nickel-base high-temperature single crystal alloy coupon.
Step 2, time and its end time that simulation al element uphill diffusion occurs.Described simulation al element uphill diffusion The time occurring and its end time are to simulate third generation nickel-base high-temperature single crystal alloy coupon in multistep admittedly by dictra software The situation of diffusion under temperature conditionss in molten process.Specifically:
The process of simulation conventional solid solution processing method and parameter, by third generation nickel-base high-temperature single crystal alloy coupon from room temperature liter 1290 DEG C of insulation 1h of solid solution temperature to the first step;It is warming up to 1300 DEG C of insulation 2h of solid solution temperature of second step, protect After temperature terminates, continue to be warmed up to 1310 DEG C of the solid solution temperature of the 3rd step and be incubated 3h;Continue to be warmed up to the solid solution of the 4th step 1320 DEG C for the treatment of temperature is simultaneously incubated 5h, is incubated 10h after being warmed up to 1330 DEG C of the solid solution temperature of the 5th step;Insulation is opened after terminating Stove, third generation nickel-base high-temperature single crystal alloy coupon is air cooled to room temperature, described heating rate is 10 DEG C/min.
Obtain the process of all elements phase counterdiffusion in third generation nickel-base high-temperature single crystal alloy coupon, Yi Ji by simulation In three generations's nickel-base high-temperature single crystal alloy coupon, the al constituent content of position occurs uphill diffusion to become with the process of solution treatment Change.Record the time of described al constituent content uphill diffusion, at the end of obtaining al element uphill diffusion, third generation nickel-based monocrystal is high The content of each element at al constituent content maximum position in temperature alloy coupon.
Al element in the present embodiment, after solution treatment to 717.2s, in third generation nickel-base high-temperature single crystal alloy coupon Start uphill diffusion, and reach maximum when 5464.8s, subsequent uphill diffusion terminates.
Step 3, determines the temperature of solution treatment.When determining the temperature of solution treatment, it is first determined the uphill diffusion time The initial melting temperature of alloy in section, and this initial melting temperature is compared with the temperature of al element uphill diffusion time period in solution treatment, Decide whether to adjust the temperature of solution treatment according to comparing result.Specific practice is:
The first step. input third generation nickel-base high-temperature single crystal alloy at the end of the al element uphill diffusion obtaining by step 2 The content of each element at al constituent content maximum position in coupon, obtains this al unit according to the criterion of minimization of Gibbs free energy Melting temperature at cellulose content maximum position.Gone up a slope using the melting temperature at described al constituent content maximum position as al element The initial melting temperature of diffusion time section.
Second step. by the solid solution temperature of the initial melting temperature obtaining and al element uphill diffusion time period in solution treatment It is compared, if solid solution temperature is less than initial melting temperature, incipient melting does not occur it was demonstrated that this solid solution temperature need not adjust, Enter step 4 and carry out solution treatment.If solid solution temperature is higher than described initial melting temperature, there is incipient melting, upward slope need to be reduced and expand The solid solution temperature of scattered time period is to described initial melting temperature 10 DEG C.
3rd step. whether the solid solution temperature after inspection reduces again is feasible.Replaced with the solid solution temperature after reducing Change the solid solution temperature of uphill diffusion time period in step 2, the process of repeat step 2, redefine al element uphill diffusion The time occurring and its end time, the first step and the second step laid equal stress in duplicate step, until the uphill diffusion time period is first Melting temperatur is less than this time period solid solution temperature, then choose the solution treatment that this temperature is the solution treatment uphill diffusion time period Temperature.
In the present embodiment, after 5464.8s, the just fusing point of alloy reaches 1292.6 DEG C of the minimum of a value of this time period, but Now in step 1, the temperature of solution treatment is 1300 DEG C, and this temperature is more than initial melting temperature, if therefore according to traditional solution process side Case alloy will occur incipient melting.So before al element enters the uphill diffusion time period by solid solution temperature adjust to described just 10 DEG C below melting temperatur, that is, al element enter the uphill diffusion time period before by solid solution temperature adjust to 1292.6 DEG C- 10℃;Round as 1283 DEG C.
Solid solution process when simulation is checked again is: third generation nickel-base high-temperature single crystal alloy coupon is risen to 1290 from room temperature DEG C insulation 1h;It is cooled to 1283 DEG C of insulation 2h, after insulation terminates, be warmed up to 1300 DEG C and be incubated 2h;Continue to be warmed up to 1310 DEG C And it is incubated 3h, insulation is continuously heating to 1320 DEG C after terminating and is incubated 5h;It is incubated 10h after continuing to be warmed up to 1330 DEG C;Insulation knot Blow-on after bundle, third generation nickel-base high-temperature single crystal alloy coupon is air cooled to room temperature, described heating rate is 10 DEG C/min.
Step 4, solution treatment.Solid solution temperature according to determining is carried out to third generation nickel-base high-temperature single crystal alloy coupon Solution treatment.
Described third generation nickel-base high-temperature single crystal alloy coupon is placed in heat-treatment furnace.By third generation nickel in heat-treatment furnace Based single-crystal high-temperature alloy coupon is increased to 1290 DEG C from room temperature and is incubated 1h;It is incubated 2h after cooling to 1283 DEG C;After insulation terminates It is warmed up to 1300 DEG C of insulation 2h;Continue to be warmed up to 1310 DEG C of insulation 3h;Rise temperature after insulation terminates and to 1320 DEG C and be incubated 5h;Continue It is warmed up to 1330 DEG C of insulation 10h;Insulation terminates rear blow-on, and described third generation nickel-base high-temperature single crystal alloy coupon is air cooled to room Temperature, obtains the third generation nickel-base high-temperature single crystal alloy coupon through solution treatment.Described heating rate is 10 DEG C/min.Solid solution Tissue after the completion of process is as shown in Figure 2.
Embodiment 2
The present embodiment is a kind of third generation nickel-base high-temperature single crystal alloy solid solution treatment method, described alloy by cr, mo, al, Co, w, re, ta, hf, c and ni form, wherein: cr be 3%, mo be 1%, al be 6%, co be 12%, w be 6%, re be 4%, Ta is 7.95%, hf is≤0.02% for 1%, c, balance of ni.Described percentage is mass percent.
The implementation steps of the described third generation nickel-base high-temperature single crystal alloy solution treatment that the present embodiment proposes are:
Step 1, prepares third generation nickel-base high-temperature single crystal alloy coupon.Will by cr be 3.2%, mo be 1.2%, al be 6%, Co be 10%, w be 6%, re be 4%, ta be 7.98%, hf be 0.08%, c be≤0.02%, female conjunction of balance of ni composition Gold becomes the alloy bar of third generation nickel-base high-temperature single crystal alloy by conventional directional freeze method preparation.
Step 2, determines time and its end time of the generation of al element uphill diffusion.Described determination al element uphill diffusion Occur time and its end time be to determine al element in traditional solution processing method uphill diffusion occur time and its End time.Specific practice is to simulate third generation nickel-base high-temperature single crystal alloy coupon at traditional multistep solid solution with dictra software The situation of diffusion under temperature conditionss in reason.Specifically:
The process of simulation conventional solid solution processing method and parameter, by third generation nickel-base high-temperature single crystal alloy coupon from room temperature liter 1290 DEG C of insulation 1h of solid solution temperature to the first step;It is warming up to 1300 DEG C of insulation 2h of solid solution temperature of second step, protect After temperature terminates, continue to be warmed up to 1310 DEG C of the solid solution temperature of the 3rd step and be incubated 3h;Continue to be warmed up to the solid solution of the 4th step 1320 DEG C for the treatment of temperature is simultaneously incubated 5h, is incubated 10h after being warmed up to 1330 DEG C of the solid solution temperature of the 5th step;Insulation is opened after terminating Stove, third generation nickel-base high-temperature single crystal alloy coupon is air cooled to room temperature, described heating rate is 10 DEG C/min.
Obtain the process of all elements phase counterdiffusion in third generation nickel-base high-temperature single crystal alloy coupon, Yi Ji by simulation In three generations's nickel-base high-temperature single crystal alloy coupon, the al constituent content of position occurs uphill diffusion to become with the process of solution treatment Change.Record the time of described al constituent content uphill diffusion, at the end of obtaining al element uphill diffusion, third generation nickel-based monocrystal is high The content of each element at al constituent content maximum position in temperature alloy coupon.
Al element in the present embodiment, after solution treatment to 763.9s, in third generation nickel-base high-temperature single crystal alloy coupon Start uphill diffusion, and reach maximum when 5623.8s, subsequent uphill diffusion terminates.
Step 3, determines the initial melting temperature in the uphill diffusion time period for the alloy.Determine alloy in the uphill diffusion time period just Melting temperatur, and contrast the original solid solution temperature of this initial melting temperature and this uphill diffusion time period, determined according to comparing result Whether adjust the temperature of solution treatment.Specific practice is:
The first step. each element content in the maximum node of al constituent content described in step 2 at the end of reading uphill diffusion, root Calculate the melting temperature in the above-mentioned moment for the above-mentioned node according to the criterion of minimization of Gibbs free energy, because this melting temperature is to go up a slope Melting temperature minimum point in all nodes in diffusion time section, so this melting temperature is at the traditional solution described in step 2 The initial melting temperature of uphill diffusion time period in reason method.
Second step. the traditional solution described in the initial melting temperature of contrast above-mentioned uphill diffusion time period and step 2 is processed at this , if solid solution temperature is less than initial melting temperature, there is not incipient melting it was demonstrated that this solution treatment side in the solid solution temperature of time period Case need not adjust, and jumps directly to step 4;If solid solution temperature is higher than initial melting temperature, there is incipient melting, upward slope need to be reduced and expand The solid solution temperature of scattered time period is to initial melting temperature 10 DEG C.
3rd step. whether the solid solution temperature after inspection reduces again is feasible.Solid solution temperature after reducing is replaced Change the traditional solution treatment temperature in step 2, the process of repeat step 2, redefine the time of al element uphill diffusion generation And its end time, the first step and the second step laid equal stress in duplicate step, until the initial melting temperature of uphill diffusion time period is less than This time period solid solution temperature, then choose the solution treatment temperature that this temperature is the solution treatment uphill diffusion time period of the present invention Degree.
In the present embodiment, after 5623.8s, the just fusing point of alloy reaches 1295.7 DEG C of the minimum of a value of this time period, but The temperature of the traditional multistep solution treatment now listed in step 1 be 1300 DEG C, this temperature be more than initial melting temperature, if therefore according to Traditional solution processing scheme alloy will occur incipient melting.So adjusting the solid solution temperature of above-mentioned slope diffusion time section to than first The solid solution temperature that low 10 DEG C of melting temperatur, that is, 1286 DEG C, repeat step 2~3 finds that no incipient melting occurs.
Step 4, adjusts and implements whole solution treatment process according to the result described in step 3.At solid solution in the present embodiment Reason method is: in heat-treatment furnace, from room temperature, third generation nickel-base high-temperature single crystal alloy coupon is increased to 1290 DEG C, is incubated 1h, fall Temperature, to 1286 DEG C, is incubated 2h, then is warmed up to 1300 DEG C, is incubated 2h, then is warmed up to 1310 DEG C, is incubated 3h, is warmed up to 1320 DEG C, protects Warm 5h, is warmed up to 1330 DEG C, is incubated 10h, last blow-on, third generation nickel-base high-temperature single crystal alloy coupon is air cooled to room temperature, institute State heating rate and be 10 DEG C/min.Tissue after the completion of solution treatment is as shown in Figure 3.
Embodiment 3
The present embodiment is a kind of third generation nickel-base high-temperature single crystal alloy solid solution treatment method, described alloy by cr, mo, al, Co, w, re, ta, hf, c and ni form, wherein: alloying component be cr be 3.2%, mo be 1.2%, al be 6%, co be 10%, w For 6%, re be 4%, ta be 7.98%, hf be 0.08%, c be≤0.02%, balance of ni.Described percentage is quality Percentage.
The implementation steps of the described third generation nickel-base high-temperature single crystal alloy solution treatment that the present embodiment proposes are:
Step 1, prepares third generation nickel-base high-temperature single crystal alloy coupon.By cr for 3%, mo for 1%, al for 6%, co will be 12%, w be 6%, re be 4%, ta be 7.95%, hf be 1%, c be≤0.02%, the foundry alloy of balance of ni composition often passes through The directional freeze method preparation of rule becomes the alloy bar of third generation nickel-base high-temperature single crystal alloy.
Step 2, time and its end time that simulation al element uphill diffusion occurs.Described simulation al element uphill diffusion The time occurring and its end time are to simulate third generation nickel-base high-temperature single crystal alloy coupon in multistep admittedly by dictra software The situation of diffusion under temperature conditionss in molten process.Specifically:
The process of simulation conventional solid solution processing method and parameter, by third generation nickel-base high-temperature single crystal alloy coupon from room temperature liter 1290 DEG C of insulation 1h of solid solution temperature to the first step;It is warming up to 1300 DEG C of insulation 2h of solid solution temperature of second step, protect After temperature terminates, continue to be warmed up to 1310 DEG C of the solid solution temperature of the 3rd step and be incubated 3h;Continue to be warmed up to the solid solution of the 4th step 1320 DEG C for the treatment of temperature is simultaneously incubated 5h, is incubated 10h after being warmed up to 1330 DEG C of the solid solution temperature of the 5th step;Insulation is opened after terminating Stove, third generation nickel-base high-temperature single crystal alloy coupon is air cooled to room temperature, described heating rate is 10 DEG C/min.
Obtain the process of all elements phase counterdiffusion in third generation nickel-base high-temperature single crystal alloy coupon, Yi Ji by simulation In three generations's nickel-base high-temperature single crystal alloy coupon, the al constituent content of position occurs uphill diffusion to become with the process of solution treatment Change.Record the time of described al constituent content uphill diffusion, at the end of obtaining al element uphill diffusion, third generation nickel-based monocrystal is high The content of each element at al constituent content maximum position in temperature alloy coupon.
Al element in the present embodiment, after solution treatment to 784.1s, in third generation nickel-base high-temperature single crystal alloy coupon Start uphill diffusion, and reach maximum when 5793.2s, subsequent uphill diffusion terminates.
Step 3, determines the initial melting temperature in the uphill diffusion time period for the alloy.Determine alloy in the uphill diffusion time period just Melting temperatur, and contrast the original solid solution temperature of this initial melting temperature and this uphill diffusion time period, determined according to comparing result Whether adjust the temperature of solution treatment.Specific practice is:
The first step. each element content in the maximum node of al constituent content described in step 2 at the end of reading uphill diffusion, root Calculate the melting temperature in the above-mentioned moment for the above-mentioned node according to the criterion of minimization of Gibbs free energy, because this melting temperature is to go up a slope Melting temperature minimum point in all nodes in diffusion time section, so this melting temperature is at the traditional solution described in step 2 The initial melting temperature of uphill diffusion time period in reason method.
Second step. the traditional solution described in the initial melting temperature of contrast above-mentioned uphill diffusion time period and step 2 is processed at this , if solid solution temperature is less than initial melting temperature, there is not incipient melting it was demonstrated that this solution treatment side in the solid solution temperature of time period Case need not adjust, and jumps directly to step 4;If solid solution temperature is higher than initial melting temperature, there is incipient melting, upward slope need to be reduced and expand The solid solution temperature of scattered time period is to initial melting temperature 10 DEG C.
3rd step. whether the solid solution temperature after inspection reduces again is feasible.Solid solution temperature after reducing is replaced Change the traditional solution treatment temperature in step 2, the process of repeat step 2, redefine the time of al element uphill diffusion generation And its end time, the first step and the second step laid equal stress in duplicate step, until the initial melting temperature of uphill diffusion time period is less than This time period solid solution temperature, then choose the solution treatment temperature that this temperature is the solution treatment uphill diffusion time period of the present invention Degree.
In the present embodiment, after 5793.2s, the just fusing point of alloy reaches 1297.3 DEG C of the minimum of a value of this time period, but The temperature of the traditional multistep solution treatment now listed in step 1 be 1300 DEG C, this temperature be more than initial melting temperature, if therefore according to Traditional solution processing scheme alloy will occur incipient melting.So adjusting the solid solution temperature of above-mentioned slope diffusion time section to than first The solid solution temperature that low 10 DEG C of melting temperatur, that is, 1287 DEG C, repeat step 2~3 finds that no incipient melting occurs.
Step 4, adjusts and implements whole solution treatment process according to the result described in step 3.At solid solution in the present embodiment Reason method is: in heat-treatment furnace, from room temperature, third generation nickel-base high-temperature single crystal alloy coupon is increased to 1290 DEG C, is incubated 1h, fall Temperature, to 1287 DEG C, is incubated 2h, then is warmed up to 1300 DEG C, is incubated 2h, then is warmed up to 1310 DEG C, is incubated 3h, is warmed up to 1320 DEG C, protects Warm 5h, is warmed up to 1330 DEG C, is incubated 10h, last blow-on, third generation nickel-base high-temperature single crystal alloy coupon is air cooled to room temperature, institute State heating rate and be 10 DEG C/min.Tissue after the completion of solution treatment is as shown in Figure 4.

Claims (3)

1. a kind of solid solution treatment method of third generation nickel-base high-temperature single crystal alloy is it is characterised in that comprise the concrete steps that:
Step 1, prepares third generation nickel-base high-temperature single crystal alloy coupon;
Step 2, time and its end time that simulation al element uphill diffusion occurs;Described simulation al element uphill diffusion occurs Time and its end time be by dictra software simulate third generation nickel-base high-temperature single crystal alloy coupon at multistep solid solution The situation of diffusion under temperature conditionss in reason;
Step 3, determines the temperature of solution treatment;When determining the temperature of solution treatment, it is first determined in the uphill diffusion time period The initial melting temperature of alloy, and this initial melting temperature is compared with the temperature of al element uphill diffusion time period in solution treatment, according to Comparing result decides whether to adjust the temperature of solution treatment;
Step 4, solution treatment;Solid solution temperature according to determining carries out solid solution to third generation nickel-base high-temperature single crystal alloy coupon Process;
Described third generation nickel-base high-temperature single crystal alloy coupon is placed in heat-treatment furnace;In heat-treatment furnace, the third generation is Ni-based Single crystal super alloy coupon rises to the solid solution temperature of the first step of routine and is incubated 1h from room temperature;Insulation is cooled to after terminating In step 3 determine solid solubility temperature and be incubated 2h;The solid solubility temperature of described determination is than the solution treatment of the described conventional first step Temperature is low 10 DEG C;Insulation is warmed up to the solid solution temperature of second step after terminating and is incubated 2h;Insulation terminates follow-up continuous be warmed up to The solid solution temperature of the 3rd step is simultaneously incubated 3h;Insulation is warmed up to the solid solution temperature of the 4th step after terminating and is incubated 5h;Protect Temperature terminates follow-up continuous to be warmed up to the solid solution temperature of the 5th step and be incubated 10h;Insulation terminates rear blow-on, by described third generation nickel Based single-crystal high-temperature alloy coupon is air cooled to room temperature, obtains the third generation nickel-base high-temperature single crystal alloy coupon through solution treatment;Institute State heating rate and be 10 DEG C/min.
2. the solid solution treatment method of third generation nickel-base high-temperature single crystal alloy as claimed in claim 1 is it is characterised in that pass through simulation The process of conventional solid solution processing method and parameter obtain time and its end time that described simulation al element uphill diffusion occurs.
3. the solid solution treatment method of third generation nickel-base high-temperature single crystal alloy as claimed in claim 1 is it is characterised in that determine solid solution The specific practice of the temperature processing is:
The first step. input third generation nickel-base high-temperature single crystal alloy coupon at the end of the al element uphill diffusion obtaining by step 2 The content of each element at middle al constituent content maximum position, obtains this al element according to the criterion of minimization of Gibbs free energy and contains Melting temperature at amount maximum position;Using the melting temperature at described al constituent content maximum position as al element uphill diffusion The initial melting temperature of time period alloy;
Second step. the solid solution temperature of the initial melting temperature obtaining and al element uphill diffusion time period in solution treatment is carried out Relatively, if solid solution temperature is less than initial melting temperature, there is not incipient melting it was demonstrated that this solid solution temperature need not adjust, enter Step 4 carries out solution treatment;If solid solution temperature is higher than described initial melting temperature, there is incipient melting, when need to reduce uphill diffusion Between section solid solution temperature to 10 DEG C below described initial melting temperature;
3rd step. whether the solid solution temperature after inspection reduces again is feasible;Step is replaced with the solid solution temperature after reducing The solid solution temperature of uphill diffusion time period in rapid 2, the process of repeat step 2, redefine al element uphill diffusion and occur Time and its end time, the first step and the second step laid equal stress in duplicate step, until the uphill diffusion time period incipient melting temperature Degree is less than this time period solid solution temperature, then choose the solution treatment temperature that this temperature is the solution treatment uphill diffusion time period Degree.
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* Cited by examiner, † Cited by third party
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CN111074332B (en) * 2019-12-31 2022-08-02 东莞材料基因高等理工研究院 Heat treatment method for rapidly eliminating microsegregation in single crystal high-temperature alloy
CN111440967B (en) * 2020-05-08 2021-12-31 中国科学院金属研究所 High-thermal-stability high-strength Re-free nickel-based single crystal superalloy and preparation process thereof
CN111763897B (en) * 2020-07-24 2021-10-15 中国航发北京航空材料研究院 Method for determining homogenization/solution heat treatment schedule of nickel-based single crystal superalloy
CN112935056B (en) * 2021-02-26 2023-01-06 华南理工大学 Spinning solution treatment composite forming method for nickel-based high-temperature alloy cylinder with bottom
CN113957365A (en) * 2021-10-18 2022-01-21 中国华能集团有限公司 Heat treatment process for casting precipitation strengthening nickel-based high-temperature alloy
CN114250519B (en) * 2022-01-10 2023-05-23 西北工业大学 Solution heat treatment method for reducing content of solution holes of high-rhenium nickel-based single crystal superalloy

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4582548A (en) * 1980-11-24 1986-04-15 Cannon-Muskegon Corporation Single crystal (single grain) alloy
EP2006402A2 (en) * 2006-03-31 2008-12-24 National Institute for Materials Science Ni-BASE SUPERALLOY AND METHOD FOR PRODUCING SAME
CN103352192A (en) * 2013-07-11 2013-10-16 北京航空航天大学 Method for designing single-crystal superalloy solid solution system
CN103866392A (en) * 2014-01-24 2014-06-18 南京理工大学 Low rhenium and nickel-based single crystal high-temperature alloy and preparation method thereof
CN104263998A (en) * 2014-09-18 2015-01-07 中国华能集团公司 Heat treatment process for nickel-iron-chromium-boron high-temperature alloy

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0941058A (en) * 1995-07-31 1997-02-10 Natl Res Inst For Metals Nickel base single crystal alloy

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4582548A (en) * 1980-11-24 1986-04-15 Cannon-Muskegon Corporation Single crystal (single grain) alloy
EP2006402A2 (en) * 2006-03-31 2008-12-24 National Institute for Materials Science Ni-BASE SUPERALLOY AND METHOD FOR PRODUCING SAME
CN103352192A (en) * 2013-07-11 2013-10-16 北京航空航天大学 Method for designing single-crystal superalloy solid solution system
CN103866392A (en) * 2014-01-24 2014-06-18 南京理工大学 Low rhenium and nickel-based single crystal high-temperature alloy and preparation method thereof
CN104263998A (en) * 2014-09-18 2015-01-07 中国华能集团公司 Heat treatment process for nickel-iron-chromium-boron high-temperature alloy

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
Designing homogenization-solution heat treatments for single crystal superalloys;S.R.Hegde等;《Materials Science and Engineering A》;20100820;第527卷(第21-22期);全文 *
Homogenizing a nickel-based superalloys:thermodynamics and kinetic simulation and experimental results;Paul D.Jablonski等;《Metallurgical amd Materials Transactions B》;20090430;第40卷(第2期);全文 *
Solution heat treatment optimization of fourth-generation single-crystal nickel base superallloys;Hon Tong Pang等;《Metellurgical and Materials Transactions A》;20120411;第43卷(第9期);全文 *
固溶处理参数对一种单晶高温合金微观偏析的影响;张胜霞等;《铸造》;20120131;第61卷(第1期);全文 *

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