CN101654764B - Iron-nickel based highly elastic alloy, capillary pipe thereof and method for manufacturing capillary pipe - Google Patents
Iron-nickel based highly elastic alloy, capillary pipe thereof and method for manufacturing capillary pipe Download PDFInfo
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Abstract
The invention provides an iron-nickel based highly elastic alloy and a method for manufacturing a capillary pipe from the iron-nickel based highly elastic alloy. The iron-nickel based highly elastic alloy contains the following chemical compositions: 0.02 to 0.05 weight percent of C, 0.3 to 1.2 weight percent of Mn, less than 0.8 weight percent of Si, less than 0.02 weight percent of P, less than0.008 weight percent of S, 34.50 to 36.50 weight percent of Ni, 11.00 to 13.50 weight percent of Cr, 2.50 to 3.20 weight percent of Ti, 1.0 to 1.9 weight percent of Al, 3.5 to 5.5 weight percent of Mo, 0.2 to 0.80 weight percent of Nb, less than or equal to 0.3 weight percent of Zr, less than 0.1 weight percent of Ce, and the balance of Fe and inevitable impurities. Vacuum melting plus vacuum consumable double vacuum melting technology and cold processing control process technology are adopted to manufacture the high-precision and high-performance iron-nickel based highly elastic capillary pipe (phi 0.75*0.1mm), and the iron-nickel based high elastic alloy can meet the use requirement of special elastic elements on the market.
Description
Technical field
The present invention relates to field of alloy material, specifically, the present invention relates to a kind of iron-nickel based highly elastic alloy and kapillary thereof and method for manufacturing capillary pipe.
Background technology
In general, we (tubing of≤Φ 2 * 0.30mm) is referred to as kapillary with diameter≤2mm, wall thickness≤0.3mm.Along with the progress of social science and technology, purposes capillaceous is more and more, and is also increasingly high to performance capillaceous (mechanical property) requirement, and its performance and its material, manufacturing have substantial connection.
Find that through retrieval domestic have a following kapillary with better mechanical property:
Φ 0.61 * 0.19mm kapillary that Beijing Inst. of Aeronautical Materials makes with precious metal AuAgPt alloy, its mechanical property б b≤350Mpa.
Shanghai Steel and Iron Research Institute makes kapillary with the 3J1 elastic alloy.So-called elastic alloy is a kind of Precise Alloy, and it can be divided into high elastic modulus alloy and constant modulus alloy.High elastic modulus alloy is a kind of Metallic Functional Materials with special machine physicals, can be used for special purpose, like the capillary tubes made from this alloy, can be widely used in the elastic element of making in aerospace, precision optical machinery and the precision instrumentation etc.The high elastic modulus alloy of using at present mainly contains iron-based, copper base, iron is Ni-based and several big type of cobalt-based etc.; The 3J1 alloy is that NiCrALTi is an alloy, and it is Ni-based to belong to iron, and it is national standard YB/T5256-1993; Its chemical ingredients is seen table 1; With Φ 1.0 * 0.16mm kapillary of its making, its mechanical property is tensile strength б b=980Mpa, unit elongation δ 5=5%.And there is not ys б
0.2,, the performance requriements of elastic modulus E, formability " B " value.
The alloy 3J1 chemical ingredients (wt%) of table 1 national standard YB/T5256-1993 regulation
| Alloying element | C | Mn | Si | P | S | Ni | Cr | Ti | A1 | Fe |
| Alloy 3J1 | 0.05 | ≤1.00 | ≤0.80 | ≤0.020 | ≤0.020 | 34.5/36.5 | 11.5/13.0 | 2.70/3.20 | 1.00/1.80 | Surplus |
The seamless kapillary that existing 3J1 alloy is made, technical essential is: single vacuum melting technique is adopted in (1).(2) the kapillary hollow forging is after electrically contacting 1150～1200 ℃ of solution treatment of heating, through pickling, making less than 60% cold deformation rate and 500～650 ℃ of aging heat treatment complete processings.The kapillary lumber recovery that 3J1 makes is 5～8%.
The deficiency that this technology exists is: (1) adopt the method for single vacuum metling be unfavorable for eliminating in the alloy gas be mingled with content, all will have a negative impact to the processing and the performance of capillary tubes.(2) inclusion in the waste tubing and deposition equate in electrically contacting heating excessively, to receive temperature and speed of cooling to influence, and are difficult to the fully good single phase solid solution of dissolving acquisition, increase the cold worked difficulty of follow-up capillary tubes.(3) preliminary work hardening rate during cold working makes the capillary tubes difficult processing soon, and problems such as easy to crack, tubular control difficulty can occur.
The special elastic element of aircraft engine; Need high performance kapillary; This high-performance mechanical property requirements capillaceous is: tensile strength б b reaches >=and 1340Mpa, ys б 0.2 >=800Mpa, unit elongation δ 5 >=9.0%, elastic modulus E >=180Gpa; (in regime of elastic deformation, normal stress is referred to as Young's modulus with the ratio of corresponding normal strain, representes with letter e in the particular requirement between 0.4～0.5mm to have proposed formability " B " value simultaneously.When kapillary is used for making the special elastic element, need make the rectangle state, the power of a recovery of elasticity is so just arranged, this power makes rectangle to be out of shape, and this deformation extent is controlled in the scope considers, and is referred to as formability " B " value.)。These other dimensional requirements capillaceous are: Φ 0.75 * 0.1mm tolerance+0.01mm, formability " B " value tolerance+0.002mm.And at present, domestic existing kapillary all can not reach this high-performance.
In order to overcome the above problems; The present inventor on the basis of existing 3J1 alloy, adds elements such as alloy strengthening, crystal grain thinning and reinforced alloys tissue through research; Designed a kind of iron-nickel based highly elastic alloy; This alloy can satisfy the request for utilization of market to the special elastic element fully, thereby accomplish the present invention through being processed into kapillary.
First purpose of the present invention is to provide a kind of iron-nickel based highly elastic alloy.
Second purpose of the present invention is to provide the kapillary made from said iron-nickel based highly elastic alloy.
The 3rd purpose of the present invention is to provide said method for manufacturing capillary pipe.
Summary of the invention
First aspect of the present invention provides a kind of iron-nickel based highly elastic alloy; The chemical ingredients of said iron-nickel based highly elastic alloy comprises: < < < 0.008wt%, Ni:34.50～36.50wt%, Cr:11.00～13.50wt%, Ti:2.50～3.20wt%, Al:1.0～1.9wt%, Mo:3.5～5.5wt%, surplus is Fe and unavoidable impurities for 0.02wt%, S for 0.8wt%, P for C:0.02～0.05wt%, Mn:0.3～1.2wt%, Si.
According to iron-nickel based highly elastic alloy of the present invention, also comprise in the chemical ingredients of said iron-nickel based highly elastic alloy: Nb:0.2～0.80wt%, Zr≤0.3wt%, Ce < 0.1wt%.
Iron-nickel based highly elastic alloy of the present invention raises elements such as integrating golden reinforcement, crystal grain thinning and reinforced alloys tissue on Ni36CrALTi alloy basis and forms.Ni, Cr, Al, Ti are the fundamental elements that forms iron-nickel based highly elastic alloy.Mo is the solution strengthening element of alloy of the present invention, adds Mo and strengthens the sosoloid except part Mo is dissolved in the austenite, also can occur new strengthening phase (Fe, Ni, Cr)
2(Mo, Ti) and Fe
2Mo phase, the adding of Mo also can make γ ' more stable mutually.Because the existence that contains the Mo phase has hindered growing up of crystal grain, be heated to 1200 ℃ and tangible grain growth tendency just occurs so add behind the Mo alloy.The adding of Mo has produced the following useful result: 1) improved the alloy aging strengthening effect; 2) machinery and the physicals of alloy have been improved; 3) improved the anti-relaxation stability of alloy.Add Nb, Zr, the Ce element of crystal grain thinning; Can improve alloy processing characteristics, reinforced alloys tissue; Foreign matter contents such as the extremely low S of control, P; Help organizing pure, greatly improve capillary tubes processing characteristics, improve the obdurability of alloy, their effect is on the basis of original ageing strengthening, to increase crystal grain thinning build up and grain-boundary strengthening.
Second aspect of the present invention provides a kind of kapillary; This kapillary is to form with the iron-nickel based highly elastic alloy manufacturing; The chemical ingredients of said iron-nickel based highly elastic alloy comprises: C:0.02～0.05wt%, Mn:0.3～1.2wt%, Si 0.8wt%, P 0.02wt%, S 0.008wt%, Ni:34.50～36.50wt%, Cr:11.00～13.50wt%, Ti:2.50～3.20wt%, Al:1.0～1.9wt%, Mo:3.5～5.5wt%, surplus is Fe and unavoidable impurities; Further, also comprise in the chemical ingredients of said iron-nickel based highly elastic alloy: Nb:0.2～0.80wt%, Zr≤0.3wt%, Ce < 0.1wt%.
The 3rd aspect of the present invention provides with said iron-nickel based highly elastic alloy makes method capillaceous, and this method may further comprise the steps:
(1) adopts after the vacuum melting iron-nickel based highly elastic alloy of vacuum consumable smelting following compositions again;
The chemical ingredients of said iron-nickel based highly elastic alloy comprises: C:0.02～0.05wt%, Mn:0.3～1.2wt%, Si 0.8wt%, P 0.02wt%, S 0.008wt%, Ni:34.50～36.50wt%, Cr:11.00～13.50wt%, Ti:2.50～3.20wt%, Al:1.0～1.9wt%, Mo:3.5～5.5wt%, surplus is Fe and unavoidable impurities;
(2) after the melting, at continuous oven through 1100～1150 ℃ of solution heat treatment;
(3) cold rolling through 16～20 cold rolling passes;
(4) in reducing atmosphere or high vacuum, carry out timeliness thermal treatment.
In a preferred implementation: in said step (3), the cold deformation of preceding 6～7 cold rolling passes is 55～65%, and the cold deformation of 10～13 cold rolling passes in back is 10～25%.
In a preferred implementation: in said step (4), the aging heat treatment temperature is 500～650 ℃, is incubated 2～5 hours.
Below, the technological process of above-mentioned method of manufacture is described in detail.
The first step: vacuum melting+vacuum consumable smelting technology
Harmful element content such as the S that the performance of high elastic modulus alloy capillary tubes and processing request are low, P, N, H, O require S < 0.008wt%, P < 0.02wt%, H, O < 10PPm, N < 20PPm.S, P content can be guaranteed through selecting the high quality starting material, and existing single vacuum melting technology prepares alloy, for N, H, the control of O gas content, and except that H content can be controlled in below the 10PPm, 0 < 20PPm, < 50PPm all can not reach requirement to N.Purified alloy structure is one of committed step of decision iron-nickel based highly elastic alloy performance capillaceous and processing technology, promptly gas be mingled with that content is processed the alloy kapillary and performance has certain influence.The present invention adopts the two vacuum melting technology of vacuum melting+vacuum consumable further to reduce N, H, O gas and impurity such as oxide compound, nitride, sulfide equal size, and the vacuum consumable steel ingot is removed cap mouth, peeling, carries out hot cold working after alloy structure is purified.
Second step: solution heat treatment technology
Existing alloy capillary tubes employing electrically contacts mode and carries out solution heat treatment; It is inhomogeneous to exist Heating temperature; Shortcomings such as heating and temperature control low precision; Make that capillary tubes tissue odds after solution heat treatment is even, capillary tubes is prone to produce phenomenons such as cracking, crackle in follow-up cold working process.The kapillary that the present invention makes adopts the continuous oven solution heat treatment; Guarantee that alloy fully dissolves during through 1100～1150 ℃ of solution treatment at continuous oven; Obtain good single phase solid solution, solved capillary tubes and in follow-up cold working process, be prone to produce problems such as cracking, crackle.
The 3rd step: cold machining process technology
Adopt little milling train to go out the finished product capillary tubes through the capillary tubes base after the continuous oven solution heat treatment through 16～20 cold rolling passes are cold rolling; Cold deformation average out to 60～80%, and the cold deformation that existing alloy capillary tubes adopts is generally 55%.The present invention adopts the cold-rolling process technology of multi-pass small deformation amount behind the first aximal deformation value when cold working; Promptly not that total cold deformation is assigned to 16～20 cold rolling passes uniformly; But adopting 6～7 the cold rolling pass draught in front to reach cold deformation 55～65%, the cold deformation of 10～13 cold rolling passes in back adopts 10～25% draught successive subtraction method technology.This cold-rolling process technology can highly effective solution because preliminary work hardening rate is fast, make the HS capillary tubes in the course of processing, be prone to produce problems such as cracking, crackle.
The 4th step: timeliness thermal treatment
The capillary tubes of cold rolling finished product need further improve alloy property through timeliness thermal treatment, satisfies request for utilization.The timeliness thermal treatment of capillary tubes is carried out in reducing atmosphere or high vacuum, in case the capillary tubes surface oxidation,
Beneficial effect of the present invention is:
1, on the basis of existing 3J1 alloy (iron-nickel based highly elastic alloy, NiCrALTi are elastic alloy), add elements such as alloy strengthening, crystal grain thinning and reinforced alloys tissue, improved the machinery and the physicals of capillary tubes.
2, adopt the two vacuum metling technologies of vacuum melting+vacuum consumable to purify alloy structure; Adopt continuous oven annealed method and unique exclusive technology such as cold-drawing process, solve that resistance to deformation in the alloy cold working is big, be prone to crackle and cracking in the capillary tubes processing, the difficult technical barrier of cast control.
3, the kapillary lumber recovery of the present invention's making is high, reaches 15～20%; Cast capillaceous has obtained better controlled; Surface smoothness capillaceous is improved.
4, employing iron-nickel based highly elastic alloy of the present invention produces the high-performance kapillary of Φ 0.75 * 0.1 ± 0.01mm, its tensile strength sigma
b=1351～1542Mpa, ys σ
0.2=1105～1232Mpa, unit elongation δ
5=9.0～13.6%, elastic modulus E=203.5～210.6Gpa has satisfied the particular requirement of formability " B " value between 0.4～0.5mm simultaneously, satisfies the request for utilization of market special elastic element.
Embodiment
Below with embodiment the present invention is made more detailed description.These embodiment only are the descriptions to best mode for carrying out the invention, scope of the present invention are not had any restriction.
Embodiment 1
Press the chemical ingredients smelting molten steel shown in the table 2, the 30Kg vacuum oven is adopted in melting, after main composition melts fully; Under the Ar protection, add elements such as Si, Mn, Nb, Zr, Ce, refining is after 20 minutes; Steel tapping casting becomes the pole of 2 Φ 55mm; Go cap mouth peeling final vacuum consumable to become the steel ingot of Φ 100mm, steel ingot peeling after heat is swaged into Φ 75 * Lmm pipe, punches into Φ 60 * 6.5 * Lmm hollow forging after the peeling.Through thermal treatment, the capillary pipe material of cold rolling one-tenth Φ 8.2 * 0.8 * Lmm after the pickling.Then at continuous oven through 1100～1150 ℃ of solution heat treatment; Adopt little milling train through 17 cold rolling processing of cold rolling pass again; The cold deformation of preceding 7 cold rolling passes is 60～65%, and the cold deformation of back 10 cold rolling passes is 10～25%, is made into the kapillary of Φ 0.75 * 0.1 ± 0.01mm; At last in reducing atmosphere or high vacuum through 500～550 ℃, be incubated 3 hours timeliness thermal treatment.
Embodiment 2
Except adopting little milling train through 20 cold rolling processing of cold rolling pass; The cold deformation of preceding 7 cold rolling passes is 60～65%; The cold deformation of 13 cold rolling passes in back is 15～25%, is made into the kapillary of Φ 0.79 * 0.1 ± 0.01mm, and the aging heat treatment temperature is 550～600 ℃; Outside being incubated 4 hours, all the other embodiments are with embodiment 1.
Embodiment 3
Except adopting little milling train through 18 cold rolling processing of cold rolling pass; The cold deformation of preceding 7 cold rolling passes is 55～60%; The cold deformation of 11 cold rolling passes in back is 10～20%; The aging heat treatment temperature is 550～600 ℃, be incubated 3 hours outside, all the other embodiments are with embodiment 1.
Embodiment 4
Except adopting little milling train through 16 cold rolling processing of cold rolling pass; The cold deformation of preceding 6 cold rolling passes is 55～65%; The cold deformation of 10 cold rolling passes in back is 15～20%; The aging heat treatment temperature is 600～650 ℃, be incubated 3 hours outside, all the other embodiments are with embodiment 1.
The chemical ingredients (wt%) of table 2 embodiment of the invention 1-4 iron-nickel based highly elastic alloy
| Alloying element | C | Mn | Si | P | S | Ni | Cr | Ti | A1 | Mo | Nb | Zr | Ce | Fe |
| Embodiment 1 | 0.032 | 0.45 | 0.52 | 0.009 | 0.0068 | 34.58 | 11.62 | 2.82 | 1.15 | 3.61 | 0.28 | 0.15 | 0.08 | Surplus |
| Embodiment 2 | 0.038 | 0.52 | <0.61 | 0.01 | 0.0071 | 35.12 | 11.22 | 2.72 | 1.31 | 3.95 | 0.43 | 0.22 | 0.075 | Surplus |
| Embodiment 3 | 0.036 | 0.64 | <0.65 | 0.010 | 0.0080 | 35.68 | 12.45 | 2.83 | 1.52 | 5.42 | 0.75 | 0.24 | 0.067 | Surplus |
| Embodiment 4 | 0.040 | 0.55 | <0.01 | 0.069 | 0.0069 | 35.69 | 13.25 | 2.71 | 1.61 | 4.36 | 0.33 | 0.28 | 0.063 | Surplus |
Test Example 1
Adopt special high-strength capillary tubes test fixture that the kapillary that embodiment of the invention 1-2 makes is carried out Mechanics Performance Testing, test result is seen table 3.
Mechanical property capillaceous and physicals that table 3 embodiment of the invention 1-2 makes
Claims (4)
1. iron-nickel based highly elastic alloy; It is characterized in that; The chemical ingredients of said iron-nickel based highly elastic alloy comprises: C:0.02～0.05wt%, Mn:0.3～1.2wt%, Si＜0.8wt%, P＜0.02wt%, S＜0.008wt%, Ni:34.50～36.50wt%, Cr:11.00～13.50wt%, Ti:2.50～3.20wt%, Al:1.0～1.9wt%, Mo:3.5～5.5wt%, Nb:0.2～0.80wt%, Zr:0.15～0.3wt%, Ce:0.063～0.1wt%, surplus is Fe and unavoidable impurities.
2. kapillary; It is the iron-nickel based highly elastic alloy manufacturing; It is characterized in that; The chemical ingredients of said iron-nickel based highly elastic alloy comprises: C:0.02～0.05wt%, Mn:0.3～1.2wt%, Si＜0.8wt%, P＜0.02wt%, S＜0.008wt%, Ni:34.50～36.50wt%, Cr:11.00～13.50wt%, Ti:2.50～3.20wt%, Al:1.0～1.9wt%, Mo:3.5～5.5wt%, Nb:0.2～0.80wt%, Zr:0.15～0.3wt%, Ce:0.063～0.1wt%, surplus is Fe and unavoidable impurities.
3. make method capillaceous with iron-nickel based highly elastic alloy for one kind, it is characterized in that, said method comprising the steps of:
(1) adopts after the vacuum melting iron-nickel based highly elastic alloy of vacuum consumable smelting following compositions again;
The chemical ingredients of said iron-nickel based highly elastic alloy comprises: C:0.02～0.05wt%, Mn:0.3～1.2wt%, Si＜0.8wt%, P＜0.02wt%, S＜0.008wt%, Ni:34.50～36.50wt%, Cr:11.00～13.50wt%, Ti:2.50～3.20wt%, Al:1.0～1.9wt%, Mo:3.5～5.5wt%, Nb:0.2～0.80wt%, Zr:0.15～0.3wt%, Ce:0.063～0.1wt%, and surplus is Fe and unavoidable impurities;
(2) after the melting, at continuous oven through 1100～1150 ℃ of solution heat treatment;
(3) cold rolling through 17～20 cold rolling passes, wherein, the cold deformation of preceding 7 cold rolling passes is 55～65%, and the cold deformation of 10～13 cold rolling passes in back is 10～25%;
(4) in reducing atmosphere or high vacuum, carry out timeliness thermal treatment.
4. method according to claim 3 is characterized in that, in said step (4), the aging heat treatment temperature is 500～650 ℃, is incubated 2～5 hours.
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| CN102373382B (en) * | 2010-08-18 | 2013-06-05 | 宝山钢铁股份有限公司 | Standard sample for Young's modulus performance detection, and preparation method thereof |
| CN104805431B (en) * | 2014-01-23 | 2018-01-30 | 宝山钢铁股份有限公司 | A kind of manufacture method of cold spraying stainless steel and carbon steel composite plate |
| CN104324971B (en) * | 2014-09-01 | 2016-04-27 | 太原钢铁(集团)有限公司 | The cold rolling crack resistence processing method of a kind of nickel based tubular product made from high temperature alloy |
| CN104328325B (en) * | 2014-09-29 | 2017-05-17 | 钢铁研究总院 | Iron-nickel-based low-delaying constant-elastic alloy used in diaphragm capsule sensor and preparation method thereof |
| CN104947012B (en) * | 2015-07-08 | 2017-02-01 | 南昌航空大学 | Toughening method for novel temperature controller capillary material |
| CN104988423B (en) * | 2015-07-24 | 2017-04-26 | 南京东科西艺新材料有限公司 | Constant elasticity alloy for high-elasticity-modulus elastic component and manufacturing method of constant elasticity alloy |
| CN106702262A (en) * | 2016-12-09 | 2017-05-24 | 安徽银龙泵阀股份有限公司 | Alloy with high elasticity |
| CN113444970B (en) * | 2021-06-22 | 2022-08-23 | 上海神洲阳光特种钢管有限公司 | Stretch-resistant stainless steel capillary tube and preparation method thereof |
| CN113621890A (en) * | 2021-07-19 | 2021-11-09 | 哈尔滨工程大学 | Polycrystalline FeNiCoAlNb alloy with superelasticity and preparation method thereof |
| CN113500097B (en) * | 2021-07-30 | 2023-03-03 | 李新中 | Preparation method and application of alloy thin-wall capillary tube for hydrogen purification |
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