CN108588814A - The preparation method of Ni-based 028 single crystal alloy of iron under solid-state - Google Patents
The preparation method of Ni-based 028 single crystal alloy of iron under solid-state Download PDFInfo
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- CN108588814A CN108588814A CN201810569431.8A CN201810569431A CN108588814A CN 108588814 A CN108588814 A CN 108588814A CN 201810569431 A CN201810569431 A CN 201810569431A CN 108588814 A CN108588814 A CN 108588814A
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B1/00—Single-crystal growth directly from the solid state
- C30B1/02—Single-crystal growth directly from the solid state by thermal treatment, e.g. strain annealing
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/04—Ferrous alloys, e.g. steel alloys containing manganese
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
- C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
- C22C38/42—Ferrous alloys, e.g. steel alloys containing chromium with nickel with copper
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- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
- C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
- C22C38/44—Ferrous alloys, e.g. steel alloys containing chromium with nickel with molybdenum or tungsten
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
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Abstract
The technical issues of the invention discloses a kind of preparation methods of Ni-based 028 single crystal alloy of iron under solid-state, preparation method poor practicability for solving monocrystal material under existing solid-state.Technical solution is that Ni-based 028 alloy of iron is carried out higher temperature solid solution first to keep its solute atoms ingredient uniform, secondly it carries out Low Temperature Heat Treatment and obtains precipitated phase in the equally distributed microstructure of transgranular and crystal boundary, finally carry out low strain rate at high temperature and deform to obtain single large scale grain structure.Low Temperature Heat Treatment is combined by the present invention with high temperature deformation technique, prepares Ni-based 028 single crystal alloy of face-centered cubic iron in the solid state.This method carries out and includes deformation in the solid state, and growth temperature is low, and the period is short, pollution-free, does not have the defects of hole, success rate high.
Description
Technical field
The present invention relates to a kind of preparation method of monocrystal material under solid-state, more particularly to iron Ni-based 028 is single under a kind of solid-state
The preparation method of peritectic alloy.
Background technology
Monocrystal material has critical role, preparation side in semiconductor devices, solar cell and engine blade field
Method can be divided into following three kinds：(1) solid-liquid equilibria crystal growth, growth crystal is the monocrystalline being most widely used at present in liquid phase
Preparation method includes mainly directional solidification technique, zone melting method and czochralski method etc., is the large scale metal being most widely used
Method for preparing single crystal, but its preparation temperature is high, is easily introduced impurity, thereby increases and it is possible to coagulation defect occur；(2) solid-solid equilibrium crystal is given birth to
Long, the method is mainly turned by the completion of persistently growing up of single crystal grain, including strain anneal method, sintering growth method and ppolymorphism
Become growth method etc., growth temperature is low, and the period is short, but is difficult to control forming core to form big crystal grain；(3) solid vapor equilibrium crystal growth,
Including physical vapour deposition (PVD) and chemical vapor deposition, it is used to prepare whisker and thin film single crystal material.Therefore, shape is obtained in the solid state
The controllable method for preparing single crystal of core is to prepare pollution-free, large scale, the important method of inexpensive metal single crystal material, is had great
Scientific and engineering meaning.
Document [1-8] Taleff etc. proposes the method for preparing monocrystalline in the solid state, and this method passes through to technical purity
Polycrystalline refractory alloy (Mo and Ta) carries out high temperature low strain rate stretcher strain, obtains one or more abnormal big crystal grains, ruler
Very little reachable long 39mm, wide 6.5mm.But its result is only for the stretcher strain of body-centered cubic simple metal (Mo and Ta), still not applicable
In Face-centred Cubic Metals and alloy (such as Fe, Ni and its alloy).The preparation method of Ni-based 028 single crystal alloy of iron under existing solid-state,
Using the method for heat treatment plus subsequent high temperature deformation, the single large scale grain structure of 028 alloy of face-centered cubic is obtained.
[1]J.Ciulik,E.M.Taleff.Dynamic abnormal grain growth:a new method to
produce single crystals.Scri.Mater.2009,61:895~898.
[2]D.L.Worthington.Characteristics of Dynamic Abnormal Grain Growth
in Commercial-Purity Molybdenum.The University of Texas at Austin.PhD
thesis.2011:46~88.
[3]N.A.Pedrazas.Dynamic Abnormal Grain Growth in Selected Refractory
Metals.The University of Texas at Austin.PhD thesis.2013:71~190.
[4]D.L.Worthington,A.Nicholas,P.J.Noell,E.M.Taleff.Dynamic abnormal
grain growth in molybdenum.Metall.Mater.Trans.A.2013,44A:5025~5038.
[5]E.M.Taleff,N.A.Pedrazas.A new route for growing large grains in
metals.Science.2013,341:1461~1462.
[6]N.A.Pedrazas,T.E.Buchheit,E.A.Holm,E.M.Taleff.Dynamic abnormal
grain growth in tantalum.Mater.Sci.Eng.A.2014,610:76~84.
[7]P.J.Noell,D.L.Worthington,E.M.Taleff.The initiation and
propagation of dynamic abnormal grain growth in
molybdeum.Metall.Mater.Trans.A.2015,46A:5708~5718.
[8]P.J.Noell,E.M.Taleff.Dynamic Abnormal Grain Growth in Refractory
Metals.JOM.2015,67(11):2642~2645.
Invention content
In order to overcome the shortcomings of that the preparation method poor practicability of monocrystal material under existing solid-state, the present invention provide a kind of solid-state
The preparation method of lower Ni-based 028 single crystal alloy of iron.Ni-based 028 alloy of iron is carried out higher temperature solid solution by this method first keeps its molten
Matter atomic component is uniform, secondly carries out Low Temperature Heat Treatment and obtains precipitated phase in the equally distributed microstructure of transgranular and crystal boundary, most
Low strain rate is carried out at high temperature afterwards to deform to obtain single large scale grain structure.The present invention becomes Low Temperature Heat Treatment and high temperature
Shape technique is combined, and prepares Ni-based 028 single crystal alloy of face-centered cubic iron in the solid state.This method carries out and includes in the solid state
Deformation, growth temperature is low, and the period is short, pollution-free, does not have the defects of hole, success rate high.
The technical solution adopted by the present invention to solve the technical problems：The system of Ni-based 028 single crystal alloy of iron under a kind of solid-state
Preparation Method, the ingredient and mass percentage of Ni-based 028 alloy of iron are：Ni 30~34%, Cr 26~28%, Mo 3~
4%, Cu 0.6~1.4%, C≤0.03%, Si≤1%, Mn≤2.5%, P≤0.03%, S≤0.03%, Fe surpluses are special
Point is to include the following steps：
Step 1: after the Ni-based 028 alloy duct products cutting of the iron that steel mill is provided, it is put into the Muffle that temperature is 1200 DEG C
Stove inside holding 2h；
Step 2: being cooled to 1000 DEG C with the rate of 30 DEG C/min, 10h is kept the temperature, room is cooled in rear rapid merging cold water
Temperature；
Step 3: by the way of the crude extra bus bed refine of wire cutting, diameter 8mm, the cylinder of high 12mm is made in material
Compress sample；
Step 4: in 3500 heat simulating testers of Gleeble, the cylinder is compressed into sample with the speed of 30 DEG C/s
Rate is warming up to 1200 DEG C, and 30s is with uniform cylindrical sample internal temperature for heat preservation, then with 5 × 10–5s–1Strain rate compression 15%,
It carries out water quenching rapidly afterwards, obtains Ni-based 028 single crystal alloy of iron.
The beneficial effects of the invention are as follows：Ni-based 028 alloy of iron is carried out higher temperature solid solution by this method first makes its solute
Atomic component is uniform, secondly carries out Low Temperature Heat Treatment and obtains precipitated phase in the equally distributed microstructure of transgranular and crystal boundary, finally
Low strain rate is carried out at high temperature to deform to obtain single large scale grain structure.The present invention is by Low Temperature Heat Treatment and high temperature deformation
Technique is combined, and prepares Ni-based 028 single crystal alloy of face-centered cubic iron in the solid state.This method carries out and includes to become in the solid state
Shape, growth temperature is low, and the period is short, pollution-free, does not have the defects of hole, success rate high.
It elaborates with reference to the accompanying drawings and detailed description to the present invention.
Description of the drawings
Fig. 1 is that Ni-based 028 alloy of iron passes through at solid solution in the preparation method of Ni-based 028 single crystal alloy of iron under solid-state of the present invention
Microstructure photo after reason.
Fig. 2 is that Ni-based 028 alloy of iron passes through Low Temperature Thermal in the preparation method of Ni-based 028 single crystal alloy of iron under solid-state of the present invention
Treated microstructure photo.
Fig. 3 is that Ni-based 028 alloy of iron is warmed by high in the preparation method of Ni-based 028 single crystal alloy of iron under solid-state of the present invention
Deformed microstructure photo.
Specific implementation mode
Following embodiment referring to Fig.1-3.The preparation method specific steps of Ni-based 028 single crystal alloy of iron are such as under solid-state of the present invention
Under：
The method that Ni-based 028 single crystal alloy of iron is prepared under solid-state, the ingredient and quality percentage of Ni-based 028 alloy of iron contain
Amount is：Ni 30~34%, Cr 26~28%, Mo 3~4%, Cu 0.6~1.4%, C≤0.03%, Si≤1%, Mn≤
2.5%, P≤0.03%, S≤0.03%, Fe surplus.Method and step is as follows：
Step 1: solution treatment：The Ni-based 028 alloy duct products of iron that steel mill provides are cut into suitable size,
It is dissolved 2h at 1200 DEG C；
Step 2: Low Temperature Heat Treatment：It is quenched after material after solid solution is kept the temperature 10h at 1000 DEG C；
Step 3: high temperature thermal deformation：The cylinder that material is cut into diameter 8mm, high 12mm compresses sample, in 1200 DEG C of temperature
With 5 × 10 under degree–5s–1Strain rate, compression 15% after water quenching.
Specific embodiment：
Ni-based 028 alloying component of the present embodiment iron and mass percentage are：Ni 32.18%, Cr 27.91%,
Mo3.93%, Cu 0.61%, C≤0.03%, Si≤1%, Mn 0.87%, P≤0.03%, S≤0.03%, Fe surpluses.It is flat
Equal crystallite dimension is 55um.
Preparation process：(1) the Ni-based 028 alloy duct products of iron that steel mill provides are cut into suitable size, are put into temperature
For 1200 DEG C of Muffle furnace inside holding 2h；(2) 1000 DEG C are cooled to the rate of 30 DEG C/min, keep the temperature 10h, is placed in rapidly afterwards cold
It is cooled to room temperature in water；(3) by the way of the crude extra bus bed refine of wire cutting, diameter 8mm, the circle of high 12mm is made in material
Column compresses sample；(4) in 3500 heat simulating testers of Gleeble, compression sample is warming up to the rate of 30 DEG C/s
1200 DEG C, 30s is with uniform sample internal temperature for heat preservation, then with 5 × 10–5s–1Strain rate compression 15%, it is rear rapid to carry out water
It quenches.
Tissue：Crystallite dimension is more uniform in the original structure of material, average-size 55um；Solution treatment (preparation process
Step 1) after, precipitated phase is completely dissolved, and average crystal grain is 63 μm；After Low Temperature Heat Treatment (step of preparation process two), average crystal grain
Size constancy, crystal boundary and transgranular has uniform second phase (γ ') to be precipitated；After high temperature deformation handles (step of preparation process three), tissue
Middle single big crystal grain occur, size grows 4000 μm, and 2489 μm wide, surrounding grains size uniform, average-size is 317 μm.
It will be seen from figure 1 that solute atoms is dissolved in matrix in Ni-based 028 alloy of iron after solution treatment, no precipitated phase is deposited
.
Figure it is seen that precipitated phase is uniformly distributed tissue in transgranular and grain boundaries.
From figure 3, it can be seen that in tissue in addition to a large scale crystal grain, remaining is the little crystal grain of size uniform.
Claims (1)
1. the preparation method of Ni-based 028 single crystal alloy of iron under a kind of solid-state, the ingredient and quality percentage of Ni-based 028 alloy of iron
Content is：Ni 30~34%, Cr 26~28%, Mo 3~4%, Cu 0.6~1.4%, C≤0.03%, Si≤1%, Mn≤
2.5%, P≤0.03%, S≤0.03%, Fe surplus, it is characterised in that include the following steps：
Step 1: after the Ni-based 028 alloy duct products cutting of the iron that steel mill is provided, it is put into the Muffle furnace that temperature is 1200 DEG C
Keep the temperature 2h；
Step 2: being cooled to 1000 DEG C with the rate of 30 DEG C/min, 10h is kept the temperature, is cooled to room temperature in rear rapid merging cold water；
Step 3: by the way of the crude extra bus bed refine of wire cutting, the cylinder that material is made to diameter 8mm, high 12mm compresses
Sample；
Step 4: in 3500 heat simulating testers of Gleeble, the cylinder is compressed into sample with the rate liter of 30 DEG C/s
Temperature is to 1200 DEG C, and 30s is with uniform cylindrical sample internal temperature for heat preservation, then with 5 × 10–5s–1Strain rate compression 15%, it is rear fast
Speed carries out water quenching, obtains Ni-based 028 single crystal alloy of iron.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109136806A (en) * | 2018-11-09 | 2019-01-04 | 中国石油大学(华东) | NiTi monocrystalline cycle heat treatment preparation method under a kind of solid-state |
| CN111926217A (en) * | 2020-08-13 | 2020-11-13 | 煜工(南通)环保设备制造有限公司 | High-temperature-resistant, corrosion-resistant and high-strength 1200-type alloy material and preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103382536A (en) * | 2012-05-03 | 2013-11-06 | 中国科学院金属研究所 | Fourth-generation single-crystal high temperature alloy with high strength and stable structure and preparation method thereof |
| CN103710656A (en) * | 2013-12-28 | 2014-04-09 | 西安热工研究院有限公司 | Deformation machining process for nickel based alloys and iron nickel based alloys |
-
2018
- 2018-06-05 CN CN201810569431.8A patent/CN108588814A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103382536A (en) * | 2012-05-03 | 2013-11-06 | 中国科学院金属研究所 | Fourth-generation single-crystal high temperature alloy with high strength and stable structure and preparation method thereof |
| CN103710656A (en) * | 2013-12-28 | 2014-04-09 | 西安热工研究院有限公司 | Deformation machining process for nickel based alloys and iron nickel based alloys |
Non-Patent Citations (3)
| Title |
|---|
| L. WANG ET AL.: "Prediction of flow stress for N08028 alloy under hot working conditions", 《MATERIALS AND DESIGN》 * |
| QIANG ZUO ET AL.: "Prediction of hot deformation behavior in Ni-based alloy considering the effect of initial microstructure", 《PROGRESS IN NATURAL SCIENCE: MATERIALS INTERNATIONAL》 * |
| 左强: "铁镍基合金中第二相的形成与演化规律研究", 《中国博士学位论文全文数据库工程科技I辑》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109136806A (en) * | 2018-11-09 | 2019-01-04 | 中国石油大学(华东) | NiTi monocrystalline cycle heat treatment preparation method under a kind of solid-state |
| CN109136806B (en) * | 2018-11-09 | 2020-12-25 | 中国石油大学(华东) | Preparation method of NiTi monocrystal in solid state by cyclic heat treatment |
| CN111926217A (en) * | 2020-08-13 | 2020-11-13 | 煜工(南通)环保设备制造有限公司 | High-temperature-resistant, corrosion-resistant and high-strength 1200-type alloy material and preparation method and application thereof |
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