CN105483448B - The preparation method of one seed nucleus nickel base superalloy GH4145 silk materials - Google Patents

The preparation method of one seed nucleus nickel base superalloy GH4145 silk materials Download PDF

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CN105483448B
CN105483448B CN201511001421.7A CN201511001421A CN105483448B CN 105483448 B CN105483448 B CN 105483448B CN 201511001421 A CN201511001421 A CN 201511001421A CN 105483448 B CN105483448 B CN 105483448B
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silk
temperature
alloy
nickel base
base superalloy
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CN105483448A (en
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段春华
石照夏
韩光炜
颜晓峰
赵明汉
陈霞
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Central Iron and Steel Research Institute
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C19/00Alloys based on nickel or cobalt
    • C22C19/03Alloys based on nickel or cobalt based on nickel
    • C22C19/05Alloys based on nickel or cobalt based on nickel with chromium
    • C22C19/058Alloys based on nickel or cobalt based on nickel with chromium without Mo and W
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22FCHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/10Changing 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

Abstract

The preparation method of one seed nucleus nickel base superalloy GH4145 silk materials, belongs to high temperature alloy silk material processing technique field.Step includes:Vacuum induction+vacuum consumable duplex will be carried out after raw material by mass percentage dispensing to smelt and pour into alloy pig;By being forged into alloy ingot blank after homogenization, then carry out the wire rod that hot rolling after flaw detection and finishing is 8~Φ of diameter of phi 12mm;Solution treatment is carried out to wire rod, and carries out returning circle, peeling and overlay film;Drawing and annealing are carried out successively, and wire rod is pulled to required B alloy wire diameter several times, GH4145 alloy wires are obtained.The whole technological process pickling-free of nickel base superalloy silk material produced using patent of the present invention, meets core particular/special requirement, while finished product silk material dimensional accuracy is high, good surface quality, composition and even tissue, mechanical property and processing performance are excellent.This method can be extensively using core nickel base superalloy silk material manufacture field.

Description

The preparation method of one seed nucleus nickel base superalloy GH4145 silk materials
Technical field
The invention belongs to nickel base superalloy silk material processing technique field, more particularly to a seed nucleus nickel base superalloy The preparation method of GH4145 silk materials.
Background technology
The core of nuclear power station is reactor, and presurized water reactor CRDM (abbreviation CRDM) is weight in nuclear reaction system The plant equipment wanted.Various spring members in CRDM are directly contacted with primary Ioops cooling agent, and height is subjected to for a long time The effect such as corrosion of warm (343 DEG C of design temperature), high pressure (design pressure 17.2MPa) and reactor coolant, therefore to spring High requirement is proposed with material:Material should have high temperature resistant, high pressure, again with enough toughness, plasticity and wear-resisting, anti- Impact and the performance such as anticorrosive.Most springs all use high temperature resistant and corrosion resistant in current core CRDM Nickel base superalloy silk material is made.Due to the country to core with nickel base superalloy silk material in the application of control rod driving machine Met without ripe use experience, therefore in the performance of nickel base superalloy production domesticization substitute material GH4145 alloy wires On the basis of AP1000 or CPR1000 usages requirement, examination has all been formulated to grain size, macrostructure and non-metallic inclusion etc. It is required that, wherein the most harsh requirement is that silk material prepares pickling-free in whole flow process.
GH4145 alloys (foreign countries' correspondence trade mark is Inconel X-750) are a kind of age-hardening type nickel base superalloys, The elements such as Co, W, Mn, Cr are to the solution strengthening effect of matrix, and Al, Ti, Nb, Ni are by forming Ni3(Al, Ti, Nb) type γ ' phases The aging precipitation invigoration effect of realization, and trace element Mg, Zr, B add the intercrystalline strengthening effect played, and make the alloy simultaneously Possess three kinds of reinforcing features of high temperature alloy, determine its excellent comprehensive mechanical property.GH4145 alloys have been widely used as Aero-engine works and the part such as intensity requirement higher corrosion resistant annular element, structural member, bolt below 800 DEG C, It is also often used in making the plane spring and helical spring that have compared with low stress and require resistance to relaxation of less than 540 DEG C work Deng.
The maximum feature of GH4145 alloy process is:(1) high-alloying make it that the institutional framework of alloy is complicated, and Working plasticity is reduced with the raising of elevated temperature strength;(2) hot processing temperature narrow range;(3) cold working plasticity is relatively low, and deformation is anti- Power is big, and hot and cold difficulty of processing is larger;(4) requirement of the deformation process to mould and equipment is higher, and the abrasion to mould is compared Greatly.Therefore, the factor of influence GH4145 alloy wires shaping mainly has material, equipment, mould and hot and cold deformation technique etc. many Relation complex between individual aspect, and wherein each parameter.Due to seldom production nuclear power GH4145 alloy wires domestic before this, Pickling-free high-quality nickel base superalloy silk material, the optimization design of reasonable selection, mould for device parameter were not produced And the hot and cold deformation technique control of alloy etc. and mutual matching lack and go deep into systematic research.Further, since core is used The requirement of silk material dimensional accuracy and surface quality is high, though silk material is plastic and meets structure property requirement, but due to chi Very little to be difficult to reach defined precision, easily there are the defects such as folding, slight crack, scuffing, straight way, screw thread, pockmark in surface in addition, causes GH4145 alloy wire scrappages are high.Therefore, pickling-free high-quality GH4145 alloy wires preparation method is developed to realization China nuclear power key domesticizes with material, it is significant to ensure that nuclear power shapes up, and is this area urgent problem to be solved.
The content of the invention
Solved it is an object of the invention to provide a seed nucleus with the preparation method of nickel base superalloy GH4145 silk materials The problems such as GH4145 alloy wire scrappages are high.Nothing in the whole production procedure of GH4145 alloy wires prepared using the present invention Pickling is needed, dimensional accuracy height, good surface quality, even tissue, mechanical performance are excellent, can be widely used for nuclear power pickling-free Ni-based High temperature alloy silk material manufacture field.
The present invention will carry out vacuum induction+vacuum consumable duplex and smelt and pour into conjunction after raw material by mass percentage dispensing Ingot;By being forged into alloy ingot blank after homogenization, then carry out the disk that hot rolling after flaw detection and finishing is 8~Φ of diameter of phi 12mm Bar;Solution treatment is carried out to wire rod, and carries out returning circle, peeling and overlay film;Drawing and annealing are carried out successively, several times draw wire rod To required B alloy wire diameter, GH4145 alloy wire finished products are obtained.Concrete technology step and the technology controlled in process It is as follows:
(1) proportion ingredient of GH4145 alloys, the composition range (percentage by weight) of described GH4145 alloy wires are pressed For:C≤0.08%, Cr:14.0~17.0%, Ti:2.25~2.75%, Al:0.4~1.0%, Ta≤0.05%, Nb:0.7 ~1.2%, Cu≤0.50%, Co≤0.10%, Si≤0.5%, Mn≤1.0%, S≤0.01%, P≤0.015%, Fe:5.0 ~9.0%, surplus is Ni and inevitable impurity;
(2) refined in the dispensing as described in step (1), vacuum drying oven, at 1520~1580 DEG C of temperature, electromagnetic agitation is equal Even, cast obtains resmelting electrode rod;
(3) the resmelting electrode rod described in step (2) obtains alloy pig through vacuum arc remelting (vacuum consumable);
(4) the hot forging squarely ingot blank after Homogenization Treatments of the alloy pig described in step (3), through flaw detection, finishing, by steel billet 1140~1160 DEG C are heated to, 60~120 minutes are incubated, hot rolling of coming out of the stove is diameter of phi 8~Φ 12mm wire rods, rolling temperature exists Between 950~1140 DEG C;
(5) wire rod described in step (4) carries out 1000~1100 DEG C, is incubated 20~80 minutes, the solution treatment of water cooling;
(6) wire rod carries out returning circle, peeling and overlay film after the solution treatment described in step (5);
(7) wire rod described in step (6) carries out drawing and annealing successively, several times by the wire drawing of Φ 8~Φ 12mm wire rods extremely It is required that B alloy wire diameter silk material finished product, per fire time drawing after finishing processing is carried out to silk material, control is per fire time deflection model Enclose for 15~35%, annealing temperature is 1000~1080 DEG C;
(8) the silk material finished product described in step (7) carries out liquid penetration examination according to core level with material relevant criterion.
Refining described in step (2) of the present invention is carried out in two times, and first time refining time is 15~30 minutes, and vacuum is 0.1~5Pa, second of refining time is 10~20 minutes, vacuum≤0.1Pa.
Electromagnetic agitation described in step (2) stirs 1~3 after refining later stage furnace charge is melting down using 400~450kW power Minute;
Homogenizing annealing treatment temperature described in step (4) is 1100~1200 DEG C, and homogenization time is 24~48 hours.
Hot forging heating-up temperature described in step (4) is 1120~1180 DEG C, and soaking time is 30~60 minutes, starting forging temperature More than or equal to 1120 DEG C, final forging temperature is more than or equal to 900 DEG C.
Described silk material finished product preparation process pickling-free, finished surface quality is good, a diameter of 3.0~6.5mm, dimensional accuracy For ± 0.01mm, circularity is that room-temperature mechanical property is as follows after 0.01~0.02mm, timeliness:
Tensile strength is 1250~1327MPa;Yield strength is 985~1049MPa;Elongation after fracture be 18.5~ 24.0%:The contraction percentage of area is 47.0~52.0%.
Silk material finished product has uniform fine grained texture, and mean grain size is narrower than 5 grades.Mechanical property and processing performance are full after timeliness Sufficient core silk material performance requirement, Liquid Penetrant does not find excessive defect, and the performance of spring member after final timeliness can be effectively ensured, Meet the technical requirement of spring in core CRDM.
Beneficial effects of the present invention are:
1) using the nickel base superalloy GH4145 silk materials dimensional accuracy of the invention prepared is high, surface quality is good, composition It is excellent with even tissue, mechanical property and processing performance, finishing processing is carried out to silk material after secondary drawing per fire, silk has been effectively ensured Material dimensional accuracy and surface quality, and whole process is not related to the pickling process of lubricating layer after drawing, and core spring is met comprehensively The strict demand of silk material.
2) silk material simple production process of the invention is controllable, it is easy to accomplish, production process greatly reduces, and production efficiency is carried Height, and avoid pollution of the pickling process to environment.
3) this method can be widely applied to difficult deformation nickel base superalloy silk material manufacture field.
4) using the nickel base superalloy a diameter of 3.0~6.5mm of GH4145 silk materials for preparing of the present invention, dimensional accuracy for ± 0.01mm, circularity is 0.01~0.02mm, and room-temperature mechanical property meets the requirement shown in table 1 after Ageing Treatment, and grain size is 5 Level is thinner.
Room-temperature mechanical property technical requirement of the nuclear power of table 1 after GH4145 silk material timeliness
Brief description of the drawings
Fig. 1 is the finished product silk material figure of embodiment 1.
Fig. 2 is the cold drawn state grain structure figure of silk material of embodiment 1.
Fig. 3 is the finished product silk material figure of embodiment 2.
Fig. 4 is the cold drawn state grain structure figure of silk material of embodiment 2.
Embodiment
Below in conjunction with specific embodiment, the present invention is expanded on further.It is pointed out that following examples are merely to illustrate The present invention, rather than limit protection scope of the present invention.The improvement that technical staff makes according to the present invention in actual applications And adjustment, or the present invention is used for the preparation of other nickel base superalloys (such as GH4169) silk material, still fall within the protection of the present invention Scope.
Embodiment 1
The preparation method of one seed nucleus nickel base superalloy GH4145 silk materials, a diameter of Φ 6.5mm of finished product silk material, including with Lower step:
Step 1):By GH4145 alloying ingredients, chemical composition is by weight percentage:15.5% Cr, 0.75% Al, 2.50% Ti, 0.9% (Nb+Ta), 0.3% Mn, 0.05% C, surplus are Ni.
Step 2):As step 1) described in dispensing, refine in vacuum drying oven, refining is carried out in two times, first time refining time For 20 minutes, vacuum was 2Pa, and second of refining time is 10 minutes, and vacuum is 0.1Pa.Big work(is used after furnace charge is melting down Rate electromagnetic agitation 2 minutes, at 1545 DEG C of temperature, cast obtains resmelting electrode rod;
Step 3):Step 2) described in resmelting electrode rod obtain alloy pig through vacuum arc remelting (vacuum consumable);
Step 4):Step 3) described in alloy pig through temperature be 1150 DEG C, soaking time is the Homogenization Treatments of 36 hours Afterwards, at 1160 DEG C, forging is opened into alloy pig insulation for 45 minutes, starting forging temperature is 1140 DEG C, and final forging temperature is 950 DEG C, after hot forging Into 70 × 70 × l square ingot blank, through flaw detection, finishing, by heating steel billet to 1150 DEG C, 80 minutes are incubated, hot rolling is after coming out of the stove Diameter of phi 12mm wire rod, start rolling temperature is 1140 DEG C, and finishing temperature is 950 DEG C.
Step 5):Step 4) described in wire rod carry out 1050 DEG C, be incubated 60 minutes, the solution treatment of water cooling;
Step 6):Step 5) described in solution treatment after wire rod carry out returning circle, peeling and overlay film;
Step 7):Step 6) described in wire rod carry out drawing and annealing successively, intermediate anneal temperature and end fire time annealing temperature Degree is 1050 DEG C.Drawing process is:Φ 12mm → Φ 10mm → Φ 8.5mm → Φ 7.4mm → Φ 6.5mm, pass deformation It is followed successively by 31%, 28%, 24% and 23%.Finishing processing is carried out to silk material after per fire time drawing;
Step 8):Step 7) described in silk material finished product with material relevant criterion carry out liquid penetration examination according to core level.
Using the core manufactured in the present embodiment nickel base superalloy a diameter of 6.5mm of GH4145 silk materials, dimensional accuracy for ± 0.005mm, circularity is less than or equal to 0.01mm.Silk material is subjected to Ageing Treatment by standard and carries out mechanics properties testing sampling, is obtained As shown in table 2, grain size is 5.7 grades to room-temperature mechanical property.
Embodiment 2
The preparation method of one seed nucleus nickel base superalloy GH4145 silk materials, a diameter of Φ 6.0mm of finished product silk material, including with Lower step:
Step 1):By GH4145 alloying ingredients, chemical composition is by weight percentage:16.0% Cr, 0.55% Al, 2.50% Ti, 1.0% (Nb+Ta), 0.3% Mn, 0.04% C, surplus are Ni.
Step 2):As step 1) described in dispensing, refine in vacuum drying oven, refining is carried out in two times, first time refining time For 25 minutes, vacuum was 3Pa, and second of refining time is 15 minutes, and vacuum is 0.05Pa.Big work(is used after furnace charge is melting down Rate electromagnetic agitation 3 minutes, at 1550 DEG C of temperature, cast obtains resmelting electrode rod;
Step 3):Step 2) described in resmelting electrode rod obtain alloy pig through vacuum arc remelting (vacuum consumable);
Step 4):Step 3) described in alloy pig through temperature be 1150 DEG C, soaking time is the Homogenization Treatments of 40 hours Afterwards, at 1160 DEG C, forging is opened into alloy pig insulation for 50 minutes, starting forging temperature is 1145 DEG C, and final forging temperature is 950 DEG C, after hot forging Into 70 × 70 × l square ingot blank, through flaw detection, finishing, by heating steel billet to 1160 DEG C, 80 minutes are incubated, hot rolling is after coming out of the stove Diameter of phi 10mm wire rod, start rolling temperature is 1150 DEG C, and finishing temperature is 950 DEG C.
Step 5):Step 4) described in wire rod carry out 1060 DEG C, be incubated 70 minutes, the solution treatment of water cooling;
Step 6):Step 5) described in solution treatment after wire rod carry out returning circle, peeling and overlay film;
Step 7):Step 6) described in wire rod carry out drawing and annealing successively, intermediate anneal temperature and end fire time annealing temperature Degree is 1050 DEG C.Drawing process is:Φ 10mm → Φ 8.3mm → Φ 7.3mm → Φ 6.6mm → Φ 6.0mm, pass deformation It is followed successively by 31%, 23%, 18% and 17%.Finishing processing is carried out to silk material after per fire time drawing;
Step 8):Step 7) described in silk material finished product with material relevant criterion carry out liquid penetration examination according to core level.
Using the core manufactured in the present embodiment nickel base superalloy a diameter of 6.0mm of GH4145 silk materials, dimensional accuracy for ± 0.005mm, circularity is less than or equal to 0.005mm.Silk material is subjected to Ageing Treatment by standard and carries out mechanics properties testing sampling, is obtained As shown in table 2, grain size is 6.4 grades to room-temperature mechanical property.
Room-temperature mechanical property of the seed nucleus of 2 embodiment of the present invention of table one after nickel base superalloy GH4145 silk material timeliness

Claims (2)

1. the seed nucleus preparation method of nickel base superalloy GH4145 silk materials, it is characterised in that processing step and in process The technology of control is as follows:
(1) proportion ingredient of GH4145 alloys is pressed;The composition range (percentage by weight) of described GH4145 alloy wires is:C ≤ 0.08%, Cr:14.0~17.0%, Ti:2.25~2.75%, Al:0.4~1.0%, Ta≤0.05%, Nb:0.7~ 1.2%th, Cu≤0.50%, Co≤0.10%, Si≤0.5%, Mn≤1.0%, S≤0.01%, P≤0.015%, Fe:5.0~ 9.0%, surplus is Ni and inevitable impurity;
(2) refined in the dispensing as described in step (1), vacuum drying oven, at 1520~1580 DEG C of temperature, electromagnetic agitation is uniform, pours Note, obtains resmelting electrode rod;
Described refining is carried out in two times, and first time refining time is 15~30 minutes, and vacuum is 0.1~5Pa, second of essence The refining time is 10~20 minutes, vacuum≤0.1Pa;
Described electromagnetic agitation is stirred 1~3 minute after refining later stage furnace charge is melting down using 400~450kW power;
(3) the resmelting electrode rod described in step (2) obtains alloy pig through vacuum arc remelting;
(4) hot forging squarely ingot blank after the alloy pig described in step (3) is handled through homogenizing annealing, through flaw detection, finishing, by steel billet 1140~1160 DEG C are heated to, 60~120 minutes are incubated, hot rolling of coming out of the stove is diameter of phi 8~Φ 12mm wire rods, rolling temperature exists Between 950~1140 DEG C;
Described homogenizing annealing treatment temperature is 1100~1200 DEG C, and homogenization time is 24~48 hours;
Described hot forging heating-up temperature is 1120~1180 DEG C, and soaking time is 30~60 minutes, and starting forging temperature is more than or equal to 1120 DEG C, final forging temperature is more than or equal to 900 DEG C;
(5) wire rod described in step (4) carries out 1000~1100 DEG C, is incubated 20~80 minutes, the solution treatment of water cooling;
(6) wire rod carries out returning circle, peeling and overlay film after the solution treatment described in step (5);
(7) wire rod described in step (6) carries out drawing and annealing successively, several times by 8~Φ of Φ 12mm wire rods wire drawings to requiring B alloy wire diameter silk material finished product, per fire time drawing after finishing processing is carried out to silk material, control the secondary deflection scope per fire to be 15~35%, annealing temperature is 1000~1080 DEG C;
(8) the silk material finished product described in step (7) carries out liquid penetration examination according to core level with material relevant criterion.
2. preparation method according to claim 1, it is characterised in that:Described silk material finished product preparation process pickling-free, directly Footpath is 3.0~6.5mm, and dimensional accuracy is ± 0.01mm, and circularity is 0.01~0.02mm, and room-temperature mechanical property is as follows after timeliness:
Tensile strength is 1250~1327MPa;Yield strength is 985~1049MPa;Elongation after fracture is 18.5~24.0%: The contraction percentage of area is 47.0~52.0%;
Silk material finished product has uniform fine grained texture, and mean grain size is narrower than 5 grades.
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