CN106636968A - Iron-cobalt-nickel alloy cold rolled strip and production method thereof - Google Patents

Abstract

The invention relates to an iron-cobalt-nickel alloy cold rolled strip and a production method thereof. The iron-cobalt-nickel alloy cold rolled strip consists of the following chemical components in percentage by mass: less than or equal to 0.03% of Na, less than or equal to 0.03% of C, less than or equal to 0.020% of P, less than or equal to 0.020% of S, less than or equal to 0.50% of Mn, less than or equal to 0.30% of Si, less than or equal to 0.20% of Cru, less than or equal to 0.20% of Cr, less than or equal to 0.20% of Mo, 28.5-29.5% of Ni, 16.8-17.8% of Co, and the balance iron. In a process of smelting an iron-cobalt-nickel alloy to prepare a steel ingot, when a smelting temperature is 1500 DEG C or higher, at least one of rare earth elements Ca and La is added as a catalyst before steel tapping during smelting, and weight of the added rare earth element accounts for 0.05-0.2% (in percentage by weight) of the total mass of ingredients; and a multi-pass rolling process is adopted during follow-up hot-rolling and cold-rolling, so that crystal degree of the rolled strip is more uniform, and crystalline grain difference is prevented from being too great.

Description

A kind of iron cobalt nickel alloy cold-strip and its production method

Technical field

The present invention relates to iron-cobalt-nickel glass sealing alloy technical field, a kind of particularly iron cobalt nickel alloy 4J29 Cold-strip and its production method.

Background technology

4J29 alloys are also known as can cut down (Kovar) alloy.The alloy has close with silicon boron Bohemian glass at 20～450 DEG C Linear expansion coefficient, curie point is higher, and has good cryo tissue stability.The alloy is international Typical Fe-Ni-Co Bohemian glass sealing alloys.Jing aviations factory Long-Time Service, stable performance.It is mainly used in Electrovacuum components and parts for example transmitting tube, oscillating tube, ignitron, magnetron, transistor, sealing plug, relay, The glass sealing of lead-out wire, chassis, shell, the support of integrated circuit etc..The glass of selection should be made in the application With the matched expansion coefficient of alloy.

In actual applications, 4J29 alloys make band Jing after the 960 DEG C of annealing of many cold rolling cold-strips for obtaining Cracking phenomenon during shape closure, Metallographic Analysis show the alloy grain degree for problem of Cracking occur be 3.5～ 6.5 grades, be abnormal coarse grain, and excessive with the grain size difference of batch products, if being not for grain size level The larger product of difference carries out differentiation process, and the properties of product for obtaining are inconsistent, directly affect material deep drawability And sealing property, it is related to quality and the life-span of electrovacuum components and parts.

4J29 expansion alloys cold-strip how is avoided to occur coarse grain in the fabrication process, obtain grain size Differential less cold-strip is those skilled in the art's technical issues that need to address.

The content of the invention

It is an object of the invention to provide a kind of iron cobalt nickel alloy cold-strip and its production method, iron-cobalt-nickel conjunction Golden cold-strip grain size is for 6～9 grades and differential within 1.5 grades.

The technical scheme is that, a kind of iron cobalt nickel alloy cold-strip, its each composition for including and its weight Percentage includes：

Na≤0.03%；

C≤0.03%；

P≤0.020%；

S≤0.020%；

Mn≤0.50%；

Si≤0.30%；

Cu≤0.20%；

Cr≤0.20%；

Mo≤0.20%；

Ni：28.5～29.5%；

Co：16.8～17.8%；Balance of iron；The iron cobalt nickel alloy cold-strip grain size be 6～9 grades and grade Difference is within 1.5 grades.

A kind of production method of above-mentioned iron cobalt nickel alloy cold-strip, including：

Dispensing → vacuumize → applying argon gas → energization → melting → plus rare earth element → power failure → cast, after cooling To steel ingot.

Then forged steel, repeatedly hot rolling, cold rolling and intermediate heat-treatment, finished product heat treatment are carried out：

A. forged steel：1280 DEG C of initial forging temperature, final forging temperature are not less than 1150 DEG C, subsequently carry out air cooling and obtain band Base.

B. hot rolling：Made-up belt is carried out into multistage hot deformation, finishing temperature is not less than 1050 DEG C, obtain half into base.

C. many cold rolling and intermediate heat-treatments：Many cold rolling and intermediate annealings of Jing meet into base finish rolling by half into thickness The band of requirement, intermediate anneal temperature is controlled at 1050～1100 DEG C.

D. finished product heat treatment：Band is carried out in the range of 940～960 DEG C bright annealing.

During iron cobalt nickel alloy is smelted and steel ingot is obtained, smelting temperature is controlled more than 1500 DEG C, molten At least one in rare earth element ce, La is added before tapping in refining as catalyst, the rare earth element of addition It is 0.05～0.20% that weight accounts for the percentage of its dispensing gross mass；Due to the equilibrium distribution coefficient very little of rare earth, In process of setting, rare-earth enrichment prevents growing for crystal in the liquid phase of crystallization front, makes high-temperature metal Liquid forms more cores in process of setting, so as to reach the purpose of crystal grain thinning, and the iron-cobalt-nickel is closed Golden cold-strip grain size is for 6～9 grades and differential within 1.5 grades.For same material, alloy As-cast grain is thinner, and the crystal grain of rolled products is also thinner.And add rare earth element, in smelting process with O, The oxysulfide of other element reaction rare earths such as S, its fusing point is very high and stable, and molten steel is dilute after calmness Native oxide, sulfide will be excluded from steel, and so as to purify molten steel, the alloy purity for obtaining is higher.

Further, temperature control is at 600～800 DEG C when hot-rolled billet enters stove, it is to avoid temperature is too high when entering stove makes Into product burning, while the waste heat after effectively utilizes forge hot processing, reduces energy waste.

Further, total deformation is controlled 70%～85% during multiple hot rolling, is effectively improved the uniformity of crystal grain.

Further, total deformation is controlled 50%～65% when repeatedly cold rolling, material can be avoided in critical Deformation state, causes to generate thick recrystal grain after annealing；Multi- pass rolling can effectively make rolled strip Grain size it is more uniform.

Further, it is cold rolling it is front carry out reconditioning process to surface, remove face crack.

The iron cobalt nickel alloy cold-strip production method operation of the present invention is simple, it is easy to control, uniformity is higher, Can avoid in follow-up processing because same batch of material grain size it is differential it is larger cause processing technology different, cause money The waste in source and the difficulty of production are increased；By the addition rare earth element in smelting process and in follow-up cooling Remove, the degree of purity of blank can be effectively increased, while blank as-cast grain is refined, during being following process Avoid the occurrence of coarse grain to lay the foundation, the band grain size for obtaining is generally at 6～9 grades；Using multi-pass, The hot rolling of aximal deformation value and cold rolling processing, can effectively make the grain size of rolled strip more uniform, it is to avoid brilliant Grade difference is excessive, with the differential band better adaptability within 1.5 grades, obtaining of a batch of product grains degree.

Specific embodiment

The present embodiment has manufactured experimently 3 batches of iron cobalt nickel alloy cold-strips, is separately added into the rare earth element of different proportion, And through dispensing → vacuumize → applying argon gas → energization → melting → plus rare earth element → powers failure → cast, cool down After obtain steel ingot；During comparative example is prepared, remaining is equal in addition to rare earth element is not added in fusion process Identical with the production technology of embodiment, the blank to obtaining carries out chemical element component detection using energy disperse spectroscopy, its As a result 1 is shown in Table with the rare earth elements content of addition in smelting process, wherein surplus Fe constituent content is not arranged Go out.

The embodiment steel ingot and comparative example steel ingot that smelting is obtained carries out forging, 1280 DEG C of initial forging temperature, finish-forging 1150 DEG C of temperature, obtains the made-up belt that thickness is 28mm or so.

Carry out hot rolling after made-up belt is reheated, charging temperature control at 600～800 DEG C, heating-up temperature 1180～1200 DEG C, 1160 DEG C of 30～40min of preheating time, temperature retention time ＜ 10min, start rolling temperature ＞, 1050 DEG C of finishing temperature ＞, air cooling after finish to gauge；Rolling mill practice is 28 → 23 → 18 → 14 → 11 → 8.5 → 7 → 6 → 5 → 4.2mm, total deformation 85.0%, 9 hot rolling passes, to obtain wall thickness be 4.2mm half into base.

Carry out intermediate heat-treatment into base by obtain half, then the leaching of Jing alkali, water quenching, three pickling, high pressure water washing, Neutralization removes hot-working oxide skin, then carries out half-and-half carrying out reconditioning into base surface using levigator；Half is every into base Face water mill number of times should >=4 times, until steel strip surface roughness reaches 2～3 μm, surface does not scratch, crackle, The defects such as peeling.

Partly carrying out into base after by reconditioning is cold rolling, and cold rolling passage is more, and strip surface roughness is less, table Face is brighter and cleaner；It is the embodiment 1,2,3 of 4.2mm and the band of comparative example by different cold rolling by thickness It is 1.5mm that passage is rolled down to thickness, and total deflection is 64.3%, and wherein embodiment 1 rolls 5 passages, Embodiment 2 rolls 6 passages, and embodiment 3 rolls 7 passages, and comparative example rolls 5 passages.Adjacent cold rolling pass Between carry out intermediate heat-treatment, temperature is 1080～1100 DEG C.

Band 350mm after the cold rolling 1.5mm for obtaining is carried out into respectively using protective atmosphere bright annealing unit Product are heat-treated, and temperature is 940～960 DEG C；Bright annealing work atmosphere is 75% hydrogen and the mixing of 25% nitrogen Gas, it is to avoid strip surface is aoxidized.

Finished product after heat treatment is sampled respectively, reference numerals, according to the rule of YBT5231-2005 standards It is fixed, sample is heated into 900 DEG C of 20 DEG C of scholars in vacuum or hydrogen atmosphere, lh is incubated, it is again heated to 1100 DEG C 20 DEG C of scholar, is incubated 15min, is come out of the stove with being not more than the speed of 5 DEG C/min and being cooled to less than 200 DEG C.To To sample carry out grain size detection, obtain the results are shown in Table 2.

The rare earth element content added in the embodiment of table 1 and comparative example chemical element component and smelting process

The each sample grain size testing result of table 2

As shown in Table 2, in the case of cold rolling same passage, the reality of rare earth element is added in smelting process The grain size of iron cobalt nickel alloy cold-strip obtained in example 1 is applied between 6.5 grades to 8 grades, and do not smelted In journey add rare earth element comparative example obtained in iron cobalt nickel alloy cold-strip grain size compare it is clearly finer, And it is differential less；And from comparative example 2 and comparative example 3, within the specific limits with the increase of rare earth element With the increase of cold rolling pass, the band grain size for obtaining is thinner and differential less；By adding in smelting process Rare earth element is simultaneously removed in follow-up cooling, can be effectively increased the degree of purity of blank, while refining blank casting State crystal grain, is to avoid the occurrence of coarse grain during following process to lay the foundation；Using multi-pass, aximal deformation value Hot rolling and cold rolling processing, can effectively make the grain size of rolled strip more uniform, it is to avoid the differential mistake of crystal grain Greatly, with the differential band better adaptability within 1.5 grades, obtaining of a batch of product grains degree.

Obviously, above-described embodiment is only intended to clearly illustrate example of the present invention, and is not to this The restriction of bright embodiment.For those of ordinary skill in the field, on the basis of the above description Can also make other changes in different forms.There is no need to give all of embodiment It is exhaustive.And these belong to the obvious change extended out of spirit or variation of the present invention still in the present invention Protection domain in.

Claims (10)

1. a kind of iron cobalt nickel alloy cold-strip, it is characterised in that its each chemical composition for including and its mass percent include：

Na≤0.03%；

C ≤0.03%；

P≤0.020%；

S≤0.020%；

Mn≤0.50%；

Si≤0.30%；

Cu≤0.20%；

Cr ≤0.20%；

Mo≤0.20%；

Ni： 28.5~29.5%；

Co ：16.8~17.8%；

Balance of iron；The iron cobalt nickel alloy cold-strip grain size is for 6～9 grades and differential within 1.5 grades.

2. the production method of iron cobalt nickel alloy cold-strip according to claim 1, it is characterised in that comprise the steps：

（1）Dispensing → vacuumize → applying argon gas → energization → melting → plus rare earth element → power failure → cast, obtain steel ingot after cooling；

（2）Forged steel, repeatedly hot rolling, cold rolling and intermediate heat-treatment, finished product heat treatment.

3. production method according to claim 2, it is characterized in that, smelting temperature is controlled more than 1500 DEG C, adds at least one in rare earth element ce, La as catalyst before tapping in melting, and the percentage by weight for accounting for its dispensing gross mass of the rare earth element of addition is 0.05 ~ 0.20%.

4. production method according to claim 2, it is characterised in that the forged steel includes：1280 DEG C of initial forging temperature, final forging temperature are not less than 1150 DEG C, subsequently carry out air cooling and obtain made-up belt.

5. the production method according to claim 2, it is characterised in that the hot rolling includes：Made-up belt is carried out into multistage hot deformation, finishing temperature is not less than 1050 DEG C, obtain half into base.

6. production method according to claim 2, it is characterised in that the repeatedly cold rolling and intermediate heat-treatment includes that many times of Jing is cold rolling and intermediate annealing will be half into base finish rolling into the satisfactory band of thickness, and intermediate anneal temperature is controlled at 1050～1100 DEG C.

7. production method according to claim 2, it is characterised in that the finished product heat treatment includes band carrying out bright annealing in the range of 940～960 DEG C.

8. production method according to claim 5, it is characterised in that temperature control is at 600～800 DEG C when hot-rolled billet enters stove.

9. production method according to claim 5, it is characterised in that repeatedly total deformation is controlled 70%～85% during hot rolling.

10. production method according to claim 6, it is characterised in that total deformation is controlled 50%～65% when repeatedly cold rolling.