CN108823382A - A kind of iron-base superalloy accumulation heat treatment process and its performance study - Google Patents
A kind of iron-base superalloy accumulation heat treatment process and its performance study Download PDFInfo
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- CN108823382A CN108823382A CN201810869576.XA CN201810869576A CN108823382A CN 108823382 A CN108823382 A CN 108823382A CN 201810869576 A CN201810869576 A CN 201810869576A CN 108823382 A CN108823382 A CN 108823382A
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- 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
- C21D6/004—Heat treatment of ferrous alloys containing Cr and Ni
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23P—METAL-WORKING NOT OTHERWISE PROVIDED FOR; COMBINED OPERATIONS; UNIVERSAL MACHINE TOOLS
- B23P15/00—Making specific metal objects by operations not covered by a single other subclass or a group in this subclass
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- 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
- C21D6/005—Heat treatment of ferrous alloys containing Mn
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- 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
- C21D6/008—Heat treatment of ferrous alloys containing Si
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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
- C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
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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
- C22C38/04—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
- C22C38/44—Ferrous alloys, e.g. steel alloys containing chromium with nickel with molybdenum or tungsten
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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
- C22C38/46—Ferrous alloys, e.g. steel alloys containing chromium with nickel with vanadium
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Abstract
The invention discloses a kind of iron-base superalloy accumulation heat treatment process and its performance studies, belong to ferroalloy manufacture field, it is accumulation raw material that the present invention, which selects iron-base superalloy D3, iron-base superalloy is heat-treated by the ageing treatment of different temperatures and time, and pass through hardness analysis, Metallographic Analysis and X-ray diffraction analysis are organized after being heat-treated under the conditions of each temperature to the D3 iron-base superalloy and the changing rule of performance is studied, aging state hardness more original built-up welding of D3 under the conditions of each temperature after heat treatment all increases, it is maximum in the hardness number of 750 DEG C of timeliness 10h, and D3 is with M6It need to strengthen phase based on C and Laves phase, when operating temperature is 700-800 DEG C, D3 thermal stability is substantially better than H13 and 3Cr2W8V, has preferable thermal stability.
Description
Technical field
The invention belongs to iron-base superalloy technical field of heat treatment, and in particular at a kind of iron-base superalloy stacking heat
Science and engineering skill and its performance study.
Background technique
Iron-base superalloy be the alloying action of multiple element is equipped with using iron as base come improve its high-temperature mechanical property and
The special alloy of high-temperature corrosion-resistance performance.Iron-base superalloy is cheap for Ni-based and cobalt base superalloy, is
A kind of high-temperature structural material being widely used in the fields such as national defence, the energy, aviation and nuclear reaction.
Hot die steel is the metal material for manufacturing hot-work die (hot-forging die, hot heading mould, hot extruding die and compression mod etc.)
Material.Such mold is contacted with thermometal at work, cavity surface can be heated be warming up to 300~400 DEG C (hot-forging dies), 500~
800 DEG C (hot extruding die), even as high as 1000 DEG C or so (compression mod).Due to hot-work die working condition very severe, be
It works under very harsh condition, such as bears the corrosion of various stress and molten metal to mold working surface, at work
It is repeatedly subjected to the heating of red-hot metal and the thermal cycle alternating action that cooling medium (water, oil, air) is cooling.When red-hot metal
When being put into hot-work die type chamber, mold cavity surface steep temperature rise, surface layer generates compression and compressive strain；When metalwork takes out, type
Chamber surface is acted on due to sharply cooling down by tensile stress and stretching strain, easily generation heat fatigue etc., therefore it is required that mold materials
With high calorific intensity, high temperature hardness, impact flexibility, harden ability and good thermal stability and thermal fatigue resistance energy etc..Currently,
The hot die steel that largely uses of China is H13 steel and 3Cr2W8V, but compared with foreign countries, the die life in China is low, mold system
It makes means to fall behind, new die material is few, and production efficiency is low, and hot-work die is relatively backward, and the status of Chinese hot die steel is made us
Worry, the demand to hot die steel are extremely urgent.
Summary of the invention
According to the above hot die steel the deficiencies in the prior art, the technical problem to be solved by the present invention is to propose a kind of iron
Based high-temperature alloy accumulates heat treatment process and its performance study, by the heat for carrying out different temperatures and time to iron-base superalloy
Process studies the hardening constituent and thermal stability of iron-base superalloy, to solve in the prior art about hot-work die steel
Material provides technical support less.
In order to solve the above-mentioned technical problem, the technical solution adopted by the present invention is：
A kind of iron-base superalloy accumulates heat treatment process, which includes sample preparation, ageing treatment and subsequent processing,
Specific step is as follows：
1) sample preparation：On the steel plate by iron-base superalloy built-up welding, sample then is obtained through cutting, grinding and buffing,
In, overlay cladding is with a thickness of 8-9mm；
2) ageing treatment：The sample of preparation is put into heater box, aging temp is set as 700-800 DEG C, carries out timeliness
1-20h is handled, it is air-cooled to then take out sample progress；High temperature alloy ageing treatment main function is to change the carbonization being precipitated on crystal boundary
Object quantity, form and distribution, to significantly improve creep rupture life and the plasticity of alloy.Ageing treatment can be such that alloy sufficiently uniformly analyses
Hardening constituent out.The dissolution and dimerization that should not cause hardening constituent under aging temp guarantee that the size of hardening constituent is suitable；
3) subsequent processing：Sample after ageing treatment is ground on abrasive paper for metallograph, then the first rough polishing on polishing machine, then
Essence polishing.
Preferably, the iron-base superalloy is D3, and the steel plate is Q235 steel plate, and specification is 150 × 80 × 4mm.
Preferably, described to be welded as manual electric arc pile up welding.
Preferably, the iron-base superalloy includes following mass percent ingredient：C 0.31-0.33%, Si 0.4-
0.8%, Mn 1-1.5%, Cr 10.5-12%, Ni 10.5-12%, W 8-9%, Mo 4-5%, V 0.6-1%, S≤
0.03%, P≤0.03%, Fe surplus.
Preferably, the heater box is chamber type electric resistance furnace, rated power 2.5kw, voltage rating 220V, maximum temperature 1200
℃。
It is a kind of using the described iron-base superalloy accumulation heat treatment process treated iron-base superalloy, hardening constituent with
M6Based on C and Laves phase, and the stable operating temperature of hardening constituent is 700-800 DEG C.
Compared with prior art, present invention has the advantages that：
1. the present invention carries out thermal stability according to the characteristics of service condition and D3 hardfacing alloy of certain body heat drawing die
The changing rule that the aging technique under condition of different temperatures influences the alloy structure and performance is studied in experiment, and in test
On the basis of do mould steel with common heat thermal stability compare, obtain the thermal stability behavior pattern of the alloy, be factory
Actual production certain reference is provided.
2. the D3 that the present invention uses is the Austenitic iron-base superalloy mold materials in alloying direction, which has
Good heat resistance, thermal stability and inoxidizability, for body hot-forming die and heat-resisting, wear-resisting components heap wlding
Material, achieves noticeable achievement, can economically reduce expenses, reduce the utilization of the energy, so as to the Defence business, civilian for China
Huge contribution is made in industry etc., and the interim service life for the mold that iron-based hardfacing alloy D3 is done is considerable, and touches tool work belt position
Intact, economic benefit is very considerable.
Detailed description of the invention
D3 aging temp-hardness curve under Fig. 1 different time；
Aging time-hardness curve of D3 under Fig. 2 different temperatures；
The original built-up welding tissue micro-assembly robot figure of Fig. 3；
The metallographic microstructure of different time timeliness at 750 DEG C of Fig. 4；
The metallographic microstructure of different time timeliness at 800 DEG C of Fig. 5；
X- diffracting spectrum after Fig. 6 D3 difference ageing treatment；
Tissue under Fig. 7 timeliness 750 DEG C × 3h sample different multiples scanning electron microscope；
Tissue under 750 DEG C × 10h of Fig. 8 timeliness sample, 2000 multiple scanning electron microscope；
Tissue under Fig. 9 timeliness 750 DEG C × 20h sample different multiples scanning electron microscope；
M- hardness curve when the lower three kinds of material ages of Figure 10 different temperatures.
4-1, timeliness 750 DEG C × 3h, 500 times, 4-2, timeliness 750 DEG C × 3h, 1000 times, 750 DEG C 4-3, timeliness × 5h,
500 times, 4-4, timeliness 750 DEG C × 5h, 1000 times, 4-5, timeliness 750 DEG C × 10h, 500 times, 750 DEG C 4-6, timeliness × 10h,
1000 times, 4-7, timeliness 750 DEG C × 20h, 500 times, 4-8, timeliness 750 DEG C × 20h, 1000 times, 800 DEG C 5-1, timeliness × 3h,
500 times, 5-2, timeliness 800 DEG C × 3h, 1000 times, 5-3, timeliness 800 DEG C × 20h, 500 times, 800 DEG C 5-4, timeliness × 20h,
1000 times, 7-1,1000 times, 7-2,30000 times, 9-1,4000 times, 9-2,10000 times, 9-3,2000 times.
Specific embodiment
It below by the description to embodiment, is described in further detail, to help those skilled in the art to this hair
Bright inventive concept, technical solution have more complete, accurate and deep understanding.
Embodiment 1
The determination of heat treatment process parameter：
The performance of high temperature alloy depends primarily on its chemical composition and institutional framework, when one timing of alloying component, influences
Alloy structure because being known as metallurgy and foundry, plastic deformation and heat treatment process, wherein influence of the heat treatment process to alloy structure
It is more sensitive.Different heat treatment can make the quantity and particle size, even of the grain size of alloy, hardening constituent, dissolution and precipitated phase
The differences such as grain boundary state.So a kind of alloy has a different tissues after different heat treatment, thus with different performance and
Purposes.The good high temperature alloy of thermal stability has keep higher hardness and strength under the high temperature conditions.So requiring in high temperature
Working environment under, have Second Phase Precipitation and the second mutually tiny, disperse.
High temperature alloy ageing treatment main function is to change carbide quantity, form and the distribution being precipitated on crystal boundary, with aobvious
Write the creep rupture life for improving alloy and plasticity.Ageing treatment can make alloy sufficiently uniform precipitation strength phase.Under aging temp
The dissolution and dimerization that should not cause hardening constituent guarantee that the size of hardening constituent is suitable.Shown by alloy design:The second of Precipitation
Mutually mainly there is M6C, Laves phase, M23C6, MC etc..The Precipitation Temperature of these carbide and intermetallic compound:M6C be 750~
1150 DEG C, Laves phase be 650~1100 DEG C, MC is 600~1 100 DEG C, M23C6It is 650~1100 DEG C.Therefore aging temp is true
It is set to 700,750,800 DEG C；Aging time is selected as 1~20h.
Embodiment 2
The chemical component of hardfacing alloy D3 used in the present embodiment is as shown in table 1：
The design ingredient (%) of 1 hardfacing alloy D3 of table
1) in alloy each element effect
In heating and insulating process both sides variation will occur for metal material：First is that Transformation of Retained Austenite is at horse
Family name's body, second is that alloying element is assembled, grows up, secondary phase is precipitated, to produce post-curing phenomenon.Obviously, in thermal stability
Under test technology, if material is able to maintain higher " post-curing " performance, with regard to thermal stability with higher.
Alloying element W is stronger carbide former, within the temperature range of 500 DEG C~600 DEG C, martensite point
Solution, has been precipitated W, C and WC carbide, and this kind of carbide has high-melting-point, high thermal stability, it is difficult to molten people's solid solution, it is also difficult to
Agglomeration makes carbide keep disperse educt state；Meanwhile W can also be solid-solution in matrix, big atomic radius, high bullet
Property modulus so that W atom and dislocation is generated reciprocation, on dislocation line, lock dislocation makes it difficult to move segregation, is formed big
Solution strengthening, and the binding force of W atom and carbon atom is big, improves the stability of martensite pyrolytic, at high temperature still
Martensite lattice characteristic is kept, high hardness is maintained.These exactly above-mentioned characteristics, make alloy in heating and insulating process, with W
The increase of content, dispersion-strengtherning, solution strengthening are all improved, to determine the ability that W has strong raising thermal stability.
Chromium is the essential element for improving alloy inoxidizability, realizing solution strengthening.It, can be when chrome content is sufficiently high in steel
One layer of fine and close Cr is formed on its surface2O3Oxidation film, this oxidation film can prevent oxygen, sulphur, nitrogen etc. from corroding gas to a certain extent
Body is spread into steel, can also hinder metal ion to external diffusion, and it is good to form protective within the scope of certain temperature
The complex oxide film of good spinel-type, enhances the oxidation-resistance property of steel.In addition, chromium is also the master for improving steel electrode current potential
Element is wanted, therefore chromium is the important element of resistance to high temperature corrosion in heat resisting steel.Chromium is still formed and the element of stable carbide, has very
Strong suction carbon, and solid solution can be formed with iron and strengthen matrix, the intensity of steel, hardness are improved without reducing impact toughness.?
In heat resisting steel, if chromium content is too low, because the Precipitation of chromium containing carbide can generate Cr depletion zone, keep adjacent grain boundary chromium depleted, drops
Low oxidation resistance and corrosion resistance, make steel plasticity, toughness and strength reduction, and brittleness increases.If chromium content is excessively high, shape in Yi Gang
At column crystal and dendritic segregation, chilling tendency increases, and processing performance is poor, and cost increases.And it is very strong ferrite shape
At element, excessively high chromium will lead to the generation of δ brittlement phase, and need to consume Ni to balance matrix, add China's chromium nickel resources sheet
Body is just very poor, so should comprehensively consider the content of chromium.With W principle, Cr can also improve the thermal stability of alloy.But Cr
Carbide is with M7C3Based on, microhardness is lower than the microhardness of WC, and the atomic radius of chromium is small compared with tungsten and the affinity of carbon is compared with tungsten
It is weak, so, the ability ratio W that Cr improves alloy thermal stability is small.In addition, working as W/C>(W when 6>18%), will go out in solidified structure
Existing M23C6Type carbide, and Cr is to promote M23C6Type carbide formed element, this make the tungstenic amount in matrix with
The increase of chrome content and reduce.Heat stabilization test shows that alloying element tungsten can significantly improve the thermal stability of material, and chromium also can
Thermal stability is improved, but acts on and works as Cr less than tungsten<When 15%, W increases in 2%~6% range, and thermal stability significantly improves；
Work as Cr>When 20%, at 2%, thermal stability increases W, and W>When 2% variation, thermal stability increase rate is little；Work as W>16%
When, containing Cr be 2% when alloy thermal stability it is higher, Cr>When 2%, with the increase of chrome content, thermal stability is declined.
Mo is refractory metal element, can be solid-solution in austenite at high temperature, and austenite at high temperature lasting is improved
Intensity and creep resistance, while diffusion coefficient of the chromium in steel is reduced, prevent Cr23O6Formation, strengthen chromium solid solution effect.Molybdenum
It is carbide, therefore has preferable effect to the heat resistance for improving heat resisting steel.Mo be under high temperature solution strengthening and
The main component of Precipitation dispersion-strengtherning improves the essential element of heat resistance.The precipitated phase master of this alloy under high temperature
If intermetallic compound (Fe2W、Fe2MO2) i.e. Laves phase and alloy carbide M6C、M23C6, the hardening constituents such as MC.Due to
Laves phase is a kind of brittlement phase, should generally control content 5% or so.It is confirmed according to the practical work of data and forefathers, individually
Plus W or Mo cannot form Laves phase.(W+Mo) for being added 5% produces Laves phase, and 10% W, Mo is added, and W, Mo
Ratio be 2：More Laves phase is had when 1 generates (5% or so).
Vanadium improves the heat resistance of heat resisting steel by forming the carbide of fine uniform distribution, but it is unable to Intensive intervention body,
The recrystallization temperature of solid solution can not be improved.The carbide of vanadium is a kind of sufficiently stable carbide, there is good creep resistant
Performance.Carbide reinforced phase MC is primarily referred to as VC, and VC can be precipitated in eutectic transformation, can also be precipitated from austenite.VC tool
There is wider solution range, with other Carbide Phases ratios, VC particle is thinner, is more evenly distributed.The presence of VC can be mentioned significantly
High-wearing feature.
Nickel is austenite former in heat resisting steel, plays a part of to facilitate and stable austenite, and it is strong to be able to achieve solid solution
Change, improve elevated temperature strength, plasticity and creep resisting ability, improve processing performance, although therefore nickel is not oxidation resistant effective element,
But it can make material that there are a series of of great value high-temperature behaviors.Nickel is added in Cr steel, can also significantly increase the electricity of matrix
Electrode potential improves wearability.
Carbon is to expand austenitic area element, and carbon is very big on the influence of the performance of steel, generally with the increase of phosphorus content, the room of steel
Warm intensity improves, plasticity decline.Carbon content is general lower (0.1%C) in high temperature alloy, with the increase of phosphorus content, alloy
Plasticity, toughness, thermal fatigue property, antioxygenic property and processing performance all reduce.But in view of the alloy is belonged between metal
What compound L aves phase and alloy carbide were strengthened, it is therefore necessary to there are enough carbons to participate in reaction generation a certain amount of
M6C、M23C6, the alloy carbides such as MC, to improve the high-temperature behavior of alloy.But after being used for a long time at high temperature, carbon content is high,
The Carbide Phases being then precipitated from matrix necessarily increase, and make alloying element dilution in solid solution, reduce alloying element invigoration effect,
Reduce the intensity of material, plasticity, corrosion resistance and inoxidizability, thus phosphorus content be not easy it is too high.
Si, Mn are not the alloy elements being intentionally added, but their presence will not serve harmful, therefore we can
Not consider their influence.A small amount of Si can be improved the antioxygenic property of steel, but more brittleness that will increase steel.Manganese is in steel
It is the element for expanding austenitic area and stable austenite area, facilitation is equivalent to the half of nickel.It is generally believed that manganese is to antioxygen
Change performance to have no significant effect, but too high levels can also impair antioxygenic property and reduce creep limit.In addition, there are also de- for manganese
The thiopectic effect of oxygen, manganese and sulphur form the high MnS of fusing point, can prevent from leading to hot-short phenomenon because generating FeS, but manganese amount is excessively high
Can make solidification when and applied at elevated temperature during organizational coarseness, can also impair antioxygenic property.
A kind of iron-base superalloy accumulates heat treatment process, which includes sample preparation, ageing treatment and subsequent processing,
Specific step is as follows：
1) sample preparation：Test material is D3 surfacing welding, the heap soldering that manual electric arc pile up welding obtains on Q235 steel plate
Gold obtains suitable sample through cutting, grinding and buffing, and the size of Q235 plate is 150 × 80 × 4mm, on Q235 plate
The sample of built-up welding three D3 ferrous alloys uniform in size, overlay cladding is with a thickness of 8mm, and every three samples are in a steel when due to welding
On plate, so they are cut, to carry out experimental implementation, then with grinding wheel the single sample cut is polished, upper
It is round and smooth that lower surface polishes flat, surrounding is polished, until sample becomes regular, round and smooth；
2) ageing treatment：The sample of preparation is put into rated power 2.5kw, voltage rating 220V, 1200 DEG C of maximum temperature
Chamber type electric resistance furnace in, carry out setting aging temp by the technological parameter of table 2, carry out ageing treatment, then take out sample progress
It is air-cooled；High temperature alloy ageing treatment main function is to change carbide quantity, form and the distribution being precipitated on crystal boundary, significantly to mention
The creep rupture life of high alloy and plasticity.Ageing treatment can make alloy sufficiently uniform precipitation strength phase.It is not answered under aging temp
The dissolution and dimerization for causing hardening constituent guarantee that the size of hardening constituent is suitable；
3) subsequent processing：The tissue for the sample being likely to occur in cutting and heat treatment process, ingredient change, and such as occur hard
Change layer, oxide layer etc., careful removing is wanted during grinding sample.The preparation process of sample should be first with from thick to thin
Abrasive paper for metallograph polishing, the then first rough polishing on polishing machine, then essence throws.
2 sample thermal stability technological parameter of table
| Sample number into spectrum | Thermal stability technique | Sample number into spectrum | Thermal stability technique |
| Original heap is as-welded | It does not deal with | 7 | 750 DEG C × 5h of timeliness (air-cooled) |
| 0 | 700 DEG C × 1h of timeliness (air-cooled) | 8 | 800 DEG C × 5h of timeliness (air-cooled) |
| 1 | 750 DEG C × 1h of timeliness (air-cooled) | 9 | 700 DEG C × 10h of timeliness is air-cooled) |
| 2 | 800 DEG C × 1h of timeliness (air-cooled) | 10 | 750 DEG C × 10h of timeliness (air-cooled) |
| 3 | 700 DEG C × 3h of timeliness (air-cooled) | 11 | 800 DEG C × 10h of timeliness (air-cooled) |
| 4 | 750 DEG C × 3h of timeliness (air-cooled) | 12 | 700 DEG C × 20h of timeliness (air-cooled) |
| 5 | 800 DEG C × 3h of timeliness (air-cooled) | 13 | 750 DEG C × 20h of timeliness (air-cooled) |
| 6 | 700 DEG C × 5h of timeliness (air-cooled) | 14 | 800 DEG C × 20h of timeliness (air-cooled) |
Embodiment 3
Performance test：
It is prepared for 21 samples altogether, wherein 2 are the as-welded original sample of heap, 15 are heat treatment sample, remaining 4 works
To be spare, and distinguishable label is all done.
1, hardness analysis, with Rockwell apparatus, the pressure head type used in testing is diamond circular cone, scale HRC.
Rockwell hardness number is calculated with depth of cup h, and H value is bigger, hardness number is lower；Conversely, it is then higher, Rockwell hardness number
Calculating formula：HR=(k-h)/0.002, k takes 0.2mm.
2, Metallographic Analysis：Polished sample surfaces are corroded in chemical erosion agent or are wiped erosion, until surface loses light
Until pool, chemical erosion agent is three sour ethyl alcohol, and constituent is：10% nitric acid, 25% hydrochloric acid, 50% ethyl alcohol, 15% satiety
And picric acid, the time of erosion to shoot metallograph after 4-5min, then analyze the iron-base superalloy according to metallograph
Tissue and the quantity of phase, size, the features such as form and distribution.
3, X-Ray diffraction analysis：Diffraction sample used is the sample after metallographic test, and the related data of diffraction apparatus is such as
Under：Manufacturer：Japan, Rigaku Denki Co., Ltd, device name：XRD-X x ray diffractometer x (D/max-RB type), experiment：Object phase
Qualitative analysis, instrument：Wide-angle angular instrument, condition：Cu target+graphite crystal monochromator, voltage 40Kv100mA, scanning speed：
5 °/min (2 θ), timing point：0.02 °/point (step width), Ds=SS=1 ° of light bar (slit), Rs=0.3.It will when test
Sample is loaded on the special fixture of the D/max-RB type X-ray diffraction instrument of Rigaku Motor Corporation production with 5 °/min progress
Diffraction scans analysis.
4, scanning electron microscope analysis：Using Hitachi SU-1500 compact scanning electron microscope carry out surface topography and
Cross-sectional morphology observation and analysis, analyze the D3 iron-base superalloy sample of built-up welding on Q235 plate, technical indicator：
Amplification factor is 5X~40000X；Acceleration voltage：0.3-30kV；Secondary electron image point resolution nm.
Embodiment 4
Interpretation of result：
1, hardness analysis：What is carried out first is the hardness test of original built-up welding aspect product, and it is hard to arrive it by data processing
Angle value is 24.0HRC, and can 15 samples of direct aging be carried out with hardness test, gained experiment after thermal stability is tested
As a result such as the following table 3 chooses three data therein during data processing in five hardness numbers of each sample testing,
Biggish two data of wherein error are cast out, the average value for then finding out these three hardness numbers has just obtained the knot of data processing
Fruit.After obtaining the hardness number under each aged, and draw hardness and aging temp and the relation curve of time, different time
Lower D3 aging temp-hardness curve such as Fig. 1, aging time-hardness curve such as Fig. 2 of D3 under different temperatures.
3 hardness test data (HRC) of table
From the point of view of Fig. 2 aging time-hardness curve, when aging temp is 700 DEG C, since 1h, as time increases,
Hardness number is an almost unchanged process, and since 3h, hardness number is begun to decline, and after 5h, hardness is steeply risen, and speed is very
Greatly, and in 10h reach maximum value, during 10h to 20h, hardness slowly declines, and when aging temp is 750 DEG C, opens from 1h
Begin, as time increases, hardness number is a continuous raised process, and when the time is 10h, hardness number is maximum, and 10h is arrived
During 20h, hardness slowly declines, and when aging temp is 800 DEG C, since 1h, as time increases, hardness number is one
Continuous raised process, the speed of rising is very big, is 3h when the time, hardness number is maximum, after timeliness 3h, under hardness starts
Drop, substantially linear decline.
It can be seen that as a complete unit by the interpretation of result of above-mentioned hardness test, each timeliness as-welded relative to original heap
State sample hardness is all improved, wherein being maximum in 750 DEG C of timeliness, 10 hours hardness numbers.
2, metallographic structure analysis：As can be seen from Figure 3 it is arborescent structure that original heap is as-welded.Wherein white crystal is austenite
Arborescent structure.Transgranular that a small amount of, black graininess precipitated phase is distributed with, there are more herring-bone form eutectic structures in interdendritic.
This granular precipitated phase is alloy carbide, they are to be precipitated in the cooling procedure of heap postwelding, but measure seldom.
Fig. 4-1 to 4-9 is the metallographic microstructure of different time timeliness at 750 DEG C：4-1,4-2 are 750 DEG C × 3h of timeliness
Ageing treatment metallographic, it can be seen that white austenite dendrites tissue is not eliminated in heap as-welded microstructure, but interdendritic
Herring-bone form eutectic structure significantly reduces, white for austenitic matrix tissue in figure, and black is precipitated phase, precipitated phase in
Granular, rod-short, chain Dispersed precipitate on austenitic matrix and grain boundaries, through X-ray diffraction analysis it is found that graininess or
Quarter butt shape is the Laves phase being precipitated, grain boundaries M6C is with chain and needle-shaped appearance, and crystal boundary at this time is than more visible, grain boundaries
Due to precipitated phase be interconnected to form it is interrupted netted.4-3,4-4 are the metallographic of 750 DEG C × 5h of timeliness, compared to 4-1 and 4-
2 are precipitated that phasors increase and disperse degree on austenitic matrix is bigger, and precipitated phase increases.4-5,4-6 and 4-7,4-8 are respectively
The metallographic of 750 DEG C × 20h of 750 DEG C × 10h of timeliness and timeliness, can be found through observation, grain size is in ageing process
In do not change substantially, the metallographic structure for comparing at 750 DEG C different aging times can be seen that extension with aging time,
Organize basic pattern similar, but the amount of precipitated phase is continuously increased, and the size of precipitated phase is also increased.From timeliness 750
DEG C × 20h metallographic can be seen that granular and acicular precipitated phase constantly increases, matrix significantly blacks, and
And there are also the signs of the agglomeration of precipitated phase, but precipitation at this time still occupies leading position, a large amount of disperses are protected with matrix
The precipitated phase for holding certain symbiosis and epibiosis is constantly formed.Due to M6C and Laves are largely precipitated, under 750 DEG C of aging conditions, with
Matrix compared to its hardness be all it is raised, with the extension of heating time, precipitated phase is increased significantly, and hardness constantly increases, directly
Hardness reaches maximum value when to 10h, too high levels and cause its hardness to be increased to a certain value, and then stablize.
It is the metallographic structure photo of D3 under 800 DEG C of different aging times in Fig. 5, it is identical as 750 DEG C, it is white in heap as-welded microstructure
The austenite dendrites tissue of color is not eliminated, but interdendritic herring-bone form eutectic structure significantly reduces；There is black to be in granular form,
Rod-short, chain precipitated phase Dispersed precipitate are on austenitic matrix and grain boundaries, to form reticular structure；Meanwhile crystal grain is big
It is small not change substantially；4-2, the 4-8 for being respectively compared 5-2,5-4 and Fig. 4 of Fig. 5 can be seen that compared with 750 DEG C, in phase
Under same aging time, the quantity of the precipitated phase of 800 DEG C of ageing treatments has apparent increase, and crystal boundary is more obvious, reticular structure
Also more obvious, meanwhile, precipitated phase particle is slightly grown up, and precipitated phase is become the bulk of aggregation by Dispersed precipitate, and dispersion-strengtherning subtracts
It is weak.Therefore hardness increased dramatically, and when aging time is 3h, reaches maximum, is then declined, and then stablize such as Fig. 2.
3, X-Ray diffraction analysis：From the point of view of X-ray diffracting spectrum Fig. 6, the main composition of each aged alloy is mutually
γ matrix+M6C+Laves phase, other phase spectral lines are faint, illustrate its quantity and its limited.After starting timeliness, alloy precipitated phase
It increased significantly, the as-welded hardness of the more original heap of the alloy under each aged is all to rise, and at different temperatures 750
DEG C × 10h hardness number be peak.Deduced by corresponding tissue and facies analysis, alloy precipitated phase small and dispersed, and and base at this time
It is its essential reason that body, which keeps certain symbiosis and epibiosis,.It can be seen that from the comparison diffracting spectrum of each aged at 750 DEG C
Second phase M under different aging times6The peak value of C and Laves phase first becomes larger, and then has as time increases a degree of
It reduces, is that the crystal grain of matrix becomes smaller, the disperse degree of precipitated phase strengthens, this also simultaneously results in the raising of alloy rigidity.With
The increase of aging time, hardness, which has, significantly to be increased, then steady, is analyzed the reason is that the second phase M6C is largely precipitated, and
The phenomenon that causing.It can could see that there is also the second phase peak value is first in the diffracting spectrum of timeliness 3h and 20h at different temperatures
After becoming larger, after have the sign of reduction, hardness number increase starts to reduce by a small margin to a certain extent afterwards.
4, scanning electron microscope analysis：Scanning electron microscope compared with metallographic microscope can preferably reactive material tissue and
Pattern, therefore it is widely used in the 3 D stereo shape of the tissue after metal fracture, material surface pattern, deep etch and the second phase
The observation of looks.Sample is observed such as Fig. 7-9 under a scanning electron microscope after excessive erosion.
5, the thermal stability comparative analysis of D3 and H13,3Cr2V8W：Two of them curve is that H13,3Cr2W8V exist in Figure 10
When 660 DEG C of timeliness, hardness versus time curve.It can be seen from the figure that H13, through 3h timeliness, hardness fall is
5.5HRC：Through 12h timeliness, hardness fall is 10.2HRC.For 3Cr2W8V through 3h timeliness, hardness fall is 4.1HRC,
Through 12h timeliness, hardness fall is 10.4HRC, but hardness at this time is still 30.7HRC, the hardness higher than H13, explanation
The thermal stability of 3Cr2W8V is better than H13.
D3 can be seen that since 1h in 750 DEG C of time hardness curve from figure, as time increases, hardness number
A continuous raised process, when the time be 10h when, hardness number be maximum, be above timeliness same time H13 and
After 3Cr2W8V, 10h, hardness is begun to decline, and by 10 hours timeliness, hardness fall was 1.3HRC, and H13 and
3Cr2W8V declines the hardness of same magnitude, and time-consuming less than 1 hour, and at this time, the aging temp of D3 is 750 DEG C, be higher than H13 and
90 DEG C of 3Cr2W8V aging temp or so, it can more illustrate that the thermal stability of D3 is good.Since H13 and 3Cr2W8V are martensite steel, D3
It is novel austenite type mold materials, its atomic arrangement density is high compared with general martensite steel sections, and Binding Forces Between Atoms are strong, brilliant
Compartment atom diffusivity is poor, and the Precipitation Temperature of coherence carbide and intermetallic compound is higher than martensite in austenite,
So austenite hot work die steel is significantly better than the heat resistance of martensite type heated die steel.
The present invention is exemplarily described above, it is clear that present invention specific implementation is not subject to the restrictions described above,
As long as using the improvement for the various unsubstantialities that the inventive concept and technical scheme of the present invention carry out, or not improved this is sent out
Bright conception and technical scheme directly apply to other occasions, within the scope of the present invention.Protection of the invention
Range should be determined by the scope of protection defined in the claims.
Claims (6)
1. a kind of iron-base superalloy accumulates heat treatment process, which is characterized in that the technique include sample preparation, ageing treatment and
Subsequent processing, specific step is as follows：
1) sample preparation：On the steel plate by iron-base superalloy built-up welding, sample then is obtained through cutting, grinding and buffing, wherein heap
Layer is with a thickness of 8-9mm；
2) ageing treatment：The sample of preparation is put into heater box, aging temp is set as 700-800 DEG C, carries out ageing treatment
It is air-cooled to then take out sample progress by 1-20h；
3) subsequent processing：Sample after ageing treatment is ground on abrasive paper for metallograph, then the first rough polishing on polishing machine, then essence is thrown
Polishing.
2. iron-base superalloy according to claim 1 accumulates heat treatment process, which is characterized in that the iron-based high temp closes
Gold is D3, and the steel plate is Q235 steel plate, and specification is 150 × 80 × 4mm.
3. iron-base superalloy according to claim 1 accumulates heat treatment process, which is characterized in that described to be welded as craft
Arc surfacing.
4. iron-base superalloy according to claim 1 accumulates heat treatment process, which is characterized in that the iron-based high temp closes
Gold includes following mass percent ingredient：C 0.31-0.33%, Si 0.4-0.8%, Mn 1-1.5%, Cr 10.5-12%,
Ni 10.5-12%, W 8-9%, Mo 4-5%, V 0.6-1%, S≤0.03%, P≤0.03%, Fe surplus.
5. iron-base superalloy according to claim 1 accumulates heat treatment process, which is characterized in that the heater box is case
Formula resistance furnace, rated power 2.5kw, voltage rating 220V, 1200 DEG C of maximum temperature.
6. a kind of using any iron-base superalloy accumulation heat treatment process of claim 1-5 treated iron-based high temp
Alloy, which is characterized in that the iron-base superalloy hardening constituent after heat treatment is with M6Based on C and Laves phase, and hardening constituent is stable
Operating temperature is 700-800 DEG C.
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| CN112903385A (en) * | 2021-01-19 | 2021-06-04 | 大冶特殊钢有限公司 | Preparation method of high-temperature alloy metallographic specimen |
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