CN108048769A - A kind of method for improving powder metallurgy superalloy grain size distribution uniformity - Google Patents
A kind of method for improving powder metallurgy superalloy grain size distribution uniformity Download PDFInfo
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- CN108048769A CN108048769A CN201711127785.9A CN201711127785A CN108048769A CN 108048769 A CN108048769 A CN 108048769A CN 201711127785 A CN201711127785 A CN 201711127785A CN 108048769 A CN108048769 A CN 108048769A
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- Prior art keywords
- temperature
- powder metallurgy
- grain size
- metallurgy superalloy
- size distribution
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Classifications
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/10—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of nickel or cobalt or alloys based thereon
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/24—After-treatment of workpieces or articles
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D6/00—Heat treatment of ferrous alloys
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/24—After-treatment of workpieces or articles
- B22F2003/248—Thermal after-treatment
Abstract
The invention belongs to Materials Science and Engineering field, more particularly to a kind of method for improving powder metallurgy superalloy grain size distribution uniformity.The present invention is after powder metallurgy superalloy deformation process, by controlling heat treatment process, can further improve powder metallurgy superalloy grain size distribution uniformity.Optimization heat treatment process can realize effective control of alloy grain size homogeneity, so as to obtain the powder metallurgy superalloy with more excellent properties.Its reason is：In the case that initial grain tissue is identical, powder metallurgy superalloy is heated to identical solid solubility temperature, keep the temperature same time, with the increase of the rate of heat addition, the alloy average grain size of acquisition becomes larger, and even size distribution increases, showing the homogeneity of grain size increases, the narrowed width of Size Distribution, that is to say, that the difference between grain size is reduced, and uniformity increases.
Description
Technical field
The invention belongs to Materials Science and Engineering field, more particularly to a kind of raising powder metallurgy superalloy crystallite dimension point
The method of cloth uniformity.
Background technology
High temperature alloy have good inoxidizability, corrosion resistance, excellent stretching, persistently, fatigue behaviour and long-term
Structure stability is grown up to meet the requirement of the modern aerospace technology under the conditions of various applied at elevated temperature,
Powerful vitality is shown in advanced aerospace engine art.Powder metallurgy high-temperature alloy is using powder metallurgy
High temperature alloy prepared by method compared with traditional casting forging high temperature alloy, has even tissue, no gross segregation and surrender
The advantages that intensity is high, fatigue behaviour is good overcomes the segregation of common process generation, can improve the comprehensive performance of alloy, and energy
Machining amount is reduced, improves the utilization rate of alloy.
Since high temperature alloy requirement has an excellent mechanical behavior under high temperature, and crystal boundary is often weak link in high temperature environments, institute
It is to form more coarse even grained with the requirement to high temperature alloy heterogeneous microstructure.After being processed generally by thermal deformation
It is heat-treated what is realized.
Fig. 1 gives 3 kinds of typicalnesses of high temperature alloy grain size distribution.A is perfect condition, even grain size, grain size
Distribution is very narrow, that is, all crystallite dimensions are more uniform.This makes it possible to the bad shadows crystal boundary to material at high temperature performance
Sound is preferably minimized.But in actual production, such hardly possible realization of state.B be it is general can realize compared with
For preferable state, crystallite dimension is in normal distribution, and is reasonably distributed, and largest grain size is controlled with the smallest grain size difference
Within the specific limits.C is the state being not intended to, and grain size distribution is wider, it sometimes appear that bimodal or multimodal, maximum
Crystallite dimension and the smallest grain size difference are very big.
Since high temperature alloy heterogeneous microstructure has vital influence to its performance, so material science and work always
The researcher of journey has carried out numerous research to the crystallite dimension of high temperature alloy and its control.
Xie Wei (the dynamic recrystallization behavior of Hastelloy C-276 alloy high-temps compression, bao steel technology, 2014 (3)：5) it is right
Hastelloy C-276 alloys have carried out high temperature compressed experiment, and with the rise of deformation temperature, dynamic recrystallization crystallite dimension increases
Greatly, dynamic recrystallization carries out more abundant；With the increase of deformation extent, the increase of dynamic recrystallization volume fraction, crystal grain slightly has
It grows up；Crystal grain is significantly refined in thermal deformation process, and the uniformity of tissue is improved.
Above-mentioned research, being only through the method for adjustment thermal deformation technique parameter improves the homogeneity of grain structure, so
And it is not controlled effectively to the homogeneity of grain structure.
The content of the invention
The purpose of the present invention is：
To solve the above-mentioned problems, the present invention proposes a kind of method for improving powder metallurgy superalloy grain size distribution uniformity,
The present invention technical solution be,
The realization process of this method is divided into four steps：
(1) first stage temperature-rise period
By Ni-based, iron is Ni-based or the pending exemplar of iron-based powder high temperature alloy is heated in heat-treatment furnace with≤10 DEG C/min, rise
To less than the temperature spot T for treating powder metallurgy superalloy solid solution temperature, the difference between temperature spot T and solid solubility temperature is not less than temperature
150℃；
(2) second stage temperature-rise period
It is heated since temperature spot T with 50 DEG C/min~120 DEG C/min, is warming up to the solid solubility temperature of powder metallurgy superalloy exemplar；
(3) insulating process
Powder metallurgy superalloy exemplar under solid solubility temperature is kept the temperature into 3h~6h, completes crystal grain homogenization generating process；
(4) temperature-fall period
Powder metallurgy superalloy exemplar is cooled to room temperature with the speed of air-cooled or other types of cooling.
The start temperature point T being rapidly heated, less than the solid solution temperature of the powder metallurgy superalloy, and between solid solubility temperature
180 DEG C of difference；
The speed that is rapidly heated is 60 DEG C/min~100 DEG C/min.
Heat preservation soaking time 4h~5h under solid solubility temperature.
The present invention has the advantage that and advantageous effect, and the present invention is after powder metallurgy superalloy deformation process, by controlling at heat
Reason process can further improve powder metallurgy superalloy grain size distribution uniformity.Optimization heat treatment process can realize alloy
Effective control of crystallite dimension homogeneity, so as to obtain the powder metallurgy superalloy with more excellent properties.
Its reason is：In the case that initial grain tissue is identical, powder metallurgy superalloy is heated to identical solid solubility temperature,
Same time is kept the temperature, with the increase of the rate of heat addition, the alloy average grain size of acquisition becomes larger, and even size distribution increases
Add, showing the homogeneity of grain size increases, the narrowed width of Size Distribution, that is to say, that the difference between grain size subtracts
Few, uniformity increases.
The rate of heat addition is fast, and in grain growth process, the first γ ' that different intercrystallines play the grain boundaries of pinning effect mixes
The time phase difference very little of solution/back dissolving matrix, so, neighboring die is grown up mutual containing, coordinates to grow up；The rate of heat addition is slow, has
The mutually preferential back dissolvings of first γ ' of grain boundaries, crystal grain are first grown up, and the degree that crystal grain length is made great difference are occurred and are become apparent from.
Compared with prior art, effect of the invention is to rely on simply the control of heating process during to heat treatment, is obtained
Even grain size, the microstructure of desirable particle size narrowly distributing, so as to obtain the excellent comprehensive mechanical property of alloy, effect is bright
It is aobvious, it is easy to implement, it is easy to operate.
Description of the drawings
The three state of Fig. 1 high temperature alloy grain size distributions, wherein, (a) is perfect condition, and (b) is can generally to reach
The state arrived, (c) are the states for being not intended to reach.
The grain size distribution of Fig. 2 embodiments 1.
Specific embodiment
The present invention is described in further details with reference to the accompanying drawings and detailed description.
The realization process of this method is divided into four steps：
(1) first stage temperature-rise period
It, should by Ni-based, iron is Ni-based or the pending exemplar of iron-based powder high temperature alloy is heated in heat-treatment furnace with≤10 DEG C/min
Rate is to be heat-treated the rate of heat addition that temperature-rise period generally uses；It is warming up to be less than and treats powder metallurgy superalloy solid solution temperature
Temperature spot T, the temperature are mutually completely dissolved temperature not higher than the γ ' of alloy, and the difference between temperature spot T and solid solubility temperature is not less than
150℃；
(2) second stage temperature-rise period
It is heated since temperature spot T with 50 DEG C/min~120 DEG C/min, the stepwise heating rate is compared with the notable increasing of first stage
Greatly, it is rapidly heated to the solid solubility temperature of powder metallurgy superalloy exemplar；
(3) insulating process
Powder metallurgy superalloy exemplar is kept the temperature into 3h~6h under solid solubility temperature, the common soaking time of heat treatment process is 2~4h,
The purpose for further extending soaking time is that abundant crystal grain of completing homogenizes generating process；
(4) temperature-fall period
Powder metallurgy superalloy exemplar is cooled to room temperature with the speed of air-cooled or other types of cooling.Other types of cooling such as wind
Cold, oil quenching and water quenching and above-mentioned cooling medium it is compound.
The start temperature point T being rapidly heated, less than the solid solution temperature of the powder metallurgy superalloy, and between solid solubility temperature
180 DEG C of difference；
The speed that is rapidly heated is 60 DEG C/min~100 DEG C/min.
Heat preservation soaking time 4h~5h under solid solubility temperature.
Embodiment 1
Material：Ni-base P/M Superalloy, chemical composition (wt%) be 13Co, 16Cr, 4.0W, 4.0Mo, 0.7Nb, 2.13Al,
3.73Ti, 0.053C, 0.016B, 0.045Zr, remaining Ni.Argon gas is atomized alloyage powder, and powder is deaerated, after dress jacket soldering and sealing,
Hot isostatic pressing is densified；Bar is prepared by extruding, after detection cut-out then isothermal forging is heat-treated into forging.Solid
2 kinds of different heating cycles, solution heat processing 1 are selected in molten heating process：Room temperature is with the heating speed of average 3.5 DEG C/min
Rate is warming up to 1150 DEG C of solid solubility temperature, keeps the temperature air-cooled after 4h；Solution heat processing 2：Room temperature is with the rate of heat addition liter of 3.5 DEG C/min
For temperature to 970 DEG C, the difference between solid solubility temperature is 180 DEG C, is then warming up to 1150 DEG C of solid solubility temperature with 65 DEG C/min, is kept the temperature
It is air-cooled after 4h.Fig. 2 is the grain size distribution of embodiment 1.It obtains：
Solution heat processing 1：Largest grain size is 83.3 μm；Variance 97.7
Solution heat processing 2：Largest grain size is 64.5 μm.Variance 86.4
With the raising of the second stage rate of heat addition after 1030 DEG C, the uniformity of crystallite dimension significantly improves, distribution narrow.
Embodiment 2
Material：Ni-base P/M Superalloy, chemical composition (wt%) be 21Co, 13Cr, 2.1W, 3.8Mo, 0.9Nb, 3.4Al,
3.7Ti, 0.05C, 0.03B, 0.05Zr, remaining Ni.Argon gas is atomized alloyage powder, and powder is deaerated, after dress jacket soldering and sealing, heat etc.
Static pressure be densified, isothermal forging intoCake blank, is then heat-treated.2 kinds are selected during solution heat
Different heating cycles, solution heat processing 1：Room temperature is warming up to 1170 DEG C of solid solubility temperature with the rate of heat addition of average 3 DEG C/min,
After keeping the temperature 3h, oil quenching；Solution heat processing 2：Room temperature is warming up to 1020 DEG C with the rate of heat addition of 3 DEG C/min, with solid solubility temperature it
Between difference for 150 DEG C, be then warming up to 1170 DEG C with 50 DEG C/min, after keeping the temperature 3h, oil quenching.
Solution heat processing 1：Largest grain size is 96.3 μm；Variance 145.6
Solution heat processing 2：Largest grain size is 85.5 μm；Variance 102.4
Equally, with the raising of firing rate, the homogeneity of grain size distribution improves, distribution narrow.
What table 1 was listed is that the tensile property of the alloy after two kinds of solution heats are handled compares.It can be seen that no matter in room temperature
It 25 DEG C or 700 DEG C, is all increased using the tensile strength of solution heat processing 2.
The tensile property of alloy after two kinds of solution heats are handled of table 1 compares.
Embodiment 3
Material：Ni-base P/M Superalloy, chemical composition (wt%) be 21Co, 13Cr, 2.1W, 3.8Mo, 0.9Nb, 3.4Al,
3.7Ti, 0.05C, 0.03B, 0.05Zr, remaining Ni.Argon gas is atomized alloyage powder, and powder is deaerated, after dress jacket soldering and sealing, heat etc.
Static pressure is densified, and prepares bar by extruding, isothermal forging cuts pole sample from forging, carry out at sensing heating into forging
Reason selects 2 kinds of different heating cycles, solution heat processing 1 during solution heat：Room temperature is with average 3.5 DEG C/min's
The rate of heat addition is warming up to 1020 DEG C, and the difference between solid solubility temperature is 150 DEG C, is then warming up to solid solubility temperature with 30 DEG C/min
1170 DEG C, keep the temperature 4h after it is air-cooled；Solution heat processing 2：Room temperature is warming up to 1020 DEG C with the rate of heat addition of 3.5 DEG C/min,
Then 1170 DEG C are warming up to 120 DEG C/min, kept the temperature air-cooled after 4h.
Solution heat processing 1：Largest grain size is 70.5 μm；Variance 98.3
Solution heat processing 2：Largest grain size is 59.4 μm；Variance 77.5
Embodiment 4
Material：Ni-base P/M Superalloy, chemical composition (wt%) be 21Co, 13Cr, 2.1W, 3.8Mo, 0.9Nb, 3.4Al,
3.7Ti, 0.05C, 0.03B, 0.05Zr, remaining Ni.Argon gas is atomized alloyage powder, and powder is deaerated, after dress jacket soldering and sealing, heat etc.
Static pressure is densified, and bar is prepared by extruding, and isothermal forging cuts test block from forging, is heat-treated into forging, with 3.5 DEG C/
The rate of heat addition of min is warming up to 1020 DEG C, and the difference between solid solubility temperature is 150 DEG C, then with the heating speed of 65 DEG C/min
Rate is warming up to 1170 DEG C, keeps the temperature 0.5h and 3h respectively, air-cooled.
When keeping the temperature 0.5h, largest grain size is 106.5 μm；Variance 85.4
When keeping the temperature 3h, largest grain size is 75.0 μm；Variance 79.6
Embodiment 5
Material：Ni-base P/M Superalloy, chemical composition (wt%) be 21Co, 13Cr, 2.1W, 3.8Mo, 0.9Nb, 3.4Al,
3.7Ti, 0.05C, 0.03B, 0.05Zr, remaining Ni.Argon gas is atomized alloyage powder, and powder is deaerated, after dress jacket soldering and sealing, heat etc.
Static pressure is densified, and bar is prepared by extruding, and isothermal forging cuts test block from forging, is heat-treated into forging, with 10 DEG C/
The rate of heat addition of min is warming up to 1020 DEG C, and the difference between solid solubility temperature is 150 DEG C, then with the heating speed of 65 DEG C/min
Rate is warming up to 1170 DEG C, keeps the temperature 3h, air-cooled.Alloy largest grain size is 80.5 μm；Variance 78.6.
The method of the raising powder metallurgy superalloy grain size distribution uniformity of the present invention makes the largest grain size of alloy
Reduce, size distribution ranges narrow, and optimize alloy grain size distribution, are conducive to improve the comprehensive mechanical property of alloy.Separately
Outside, solution heat rate of the present invention is also required to control within the specific limits, on the one hand also to combine to alloy grain ruler
On the other hand very little demand is accounted for sample size itself.
Claims (4)
- A kind of 1. method for improving powder metallurgy superalloy grain size distribution uniformity, it is characterised in that：The realization of this method Journey is divided into four steps：(1) first stage temperature-rise periodBy Ni-based, iron is Ni-based or the pending exemplar of iron-based powder high temperature alloy is heated in heat-treatment furnace with≤10 DEG C/min, rise To less than the temperature spot T for treating powder metallurgy superalloy solid solution temperature, the difference between temperature spot T and solid solubility temperature is not less than temperature 150℃；(2) second stage temperature-rise periodIt is heated since temperature spot T with 50 DEG C/min~120 DEG C/min, is warming up to the solid solubility temperature of powder metallurgy superalloy exemplar；(3) insulating processPowder metallurgy superalloy exemplar under solid solubility temperature is kept the temperature into 3h~6h, completes crystal grain homogenization generating process；(4) temperature-fall periodPowder metallurgy superalloy exemplar is cooled to room temperature with the speed of air-cooled or other types of cooling.
- 2. a kind of method for improving powder metallurgy superalloy grain size distribution uniformity described in accordance with the claim 1, feature It is：The start temperature point T being rapidly heated, less than the solid solution temperature of the powder metallurgy superalloy, and between solid solubility temperature 180 DEG C of difference.
- 3. a kind of method for improving powder metallurgy superalloy grain size distribution uniformity described in accordance with the claim 1, feature It is：The speed that is rapidly heated is 60 DEG C/min~100 DEG C/min.
- 4. a kind of method for improving powder metallurgy superalloy grain size distribution uniformity described in accordance with the claim 1, feature It is：Heat preservation soaking time 4h~5h under solid solubility temperature.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111014682A (en) * | 2019-10-23 | 2020-04-17 | 广州市机电工业研究所 | Powdery stainless steel structure homogenization process |
| CN113388726A (en) * | 2021-06-04 | 2021-09-14 | 中国航发北京航空材料研究院 | Automatic control device and method for solid solution-quenching heat treatment of powder high-temperature alloy disc |
| CN114058988A (en) * | 2021-11-12 | 2022-02-18 | 哈尔滨工业大学（深圳） | Heat treatment method for homogenizing grain size of nickel-based powder superalloy in forging state |
| CN115261755A (en) * | 2022-08-04 | 2022-11-01 | 西部超导材料科技股份有限公司 | Heat treatment process and application of GH2150A high-temperature alloy |
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| CN106702295A (en) * | 2016-12-07 | 2017-05-24 | 陕西宏远航空锻造有限责任公司 | Method for improving structure and high-temperature smooth fatigue performance of GH4698 disk forge piece |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111014682A (en) * | 2019-10-23 | 2020-04-17 | 广州市机电工业研究所 | Powdery stainless steel structure homogenization process |
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| CN113388726A (en) * | 2021-06-04 | 2021-09-14 | 中国航发北京航空材料研究院 | Automatic control device and method for solid solution-quenching heat treatment of powder high-temperature alloy disc |
| CN113388726B (en) * | 2021-06-04 | 2022-07-12 | 中国航发北京航空材料研究院 | Automatic control device and method for solid solution-quenching heat treatment of powder high-temperature alloy disc |
| CN114058988A (en) * | 2021-11-12 | 2022-02-18 | 哈尔滨工业大学（深圳） | Heat treatment method for homogenizing grain size of nickel-based powder superalloy in forging state |
| CN115261755A (en) * | 2022-08-04 | 2022-11-01 | 西部超导材料科技股份有限公司 | Heat treatment process and application of GH2150A high-temperature alloy |
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Application publication date: 20180518 |