CN106636968B - A kind of iron cobalt nickel alloy cold-strip and its production method - Google Patents

Abstract

The present invention relates to a kind of iron cobalt nickel alloy cold-strip and its production methods, and the iron cobalt nickel alloy cold-strip chemical component 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%；Surplus is iron；During iron cobalt nickel alloy is smelted and steel ingot is made, smelting temperature is at 1500 DEG C or more, at least one of rare earth element ce, La are added before tapping in melting and is used as catalyst, the percentage that the weight of the rare earth element of addition accounts for its ingredient gross mass is 0.05 ~ 0.2%, and multi- pass rolling technique is used in subsequent hot rolling and cold rolling, it can effectively make the grain size of rolled strip more uniform, avoid crystal grain differential excessive.

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-rolled strip Material and its production method.

Background technique

4J29 alloy can also known as cut down (Kovar) alloy.The alloy has and line similar in silicon boron Bohemian glass at 20~450 DEG C The coefficient of expansion, curie point is higher, and has good cryo tissue stability.The alloy is international typical Fe-Ni-Co Bohemian glass sealing alloy.Through aviation, factory is used for a long time, and performance is stablized.It is mainly used for electrovacuum component such as transmitting tube, oscillation The glass of pipe, ignitron, magnetron, transistor, sealing plug, relay, the lead-out wire of integrated circuit, chassis, shell, bracket etc. Glass sealing-in.The coefficient of expansion of the glass selected and alloy should be made to match in the application.

In practical applications, the cyclic annular envelope of production band after 960 DEG C of the cold-strip annealing that 4J29 alloy is obtained through multiple cold rolling Occurs cracking phenomena when fitting, Metallographic Analysis shows that the alloy grain degree for problem of Cracking occur is 3.5~6.5 grades, is abnormal thick Big crystal grain, and it is excessive with the grain size difference of batch products, if not carried out at differentiation for the differential biggish product of grain size Reason, obtained properties of product are inconsistent, directly affect material deep drawability and sealing property, are related to the matter of electrovacuum component Amount and service life.

How to avoid 4J29 expansion alloy cold-strip occur in the fabrication process coarse grain, obtain grain size it is differential compared with Small cold-strip is those skilled in the art's technical issues that need to address.

Summary of the invention

The purpose of the present invention is to provide a kind of iron cobalt nickel alloy cold-strip and its production method, the iron cobalt nickel alloy is 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 comprising each ingredient and its weight percent Than including:

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%；Surplus is iron；The iron cobalt nickel alloy cold-strip grain size be 6~9 grades and it is differential Within 1.5 grades.

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

Ingredient → vacuumize → applying argon gas → energization → melting → plus rare earth element → power failure → casting obtain steel after cooling Ingot.

Then forged steel, hot rolling, multiple 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, then carry out air-cooled obtaining made-up belt.

B. hot rolling: carrying out multistage hot deformation for made-up belt, and finishing temperature is not less than 1050 DEG C, obtains half into base.

C. it more cold rollings and intermediate heat-treatment: half will meet the requirements at base finish rolling at thickness through multiple cold rolling and intermediate annealing Band, intermediate anneal temperature control at 1050~1100 DEG C.

D. finished product is heat-treated: band is carried out bright annealing within the scope of 940~960 DEG C.

During iron cobalt nickel alloy is smelted and steel ingot is made, smelting temperature is controlled at 1500 DEG C or more, is gone out in melting At least one of rare earth element ce, La are added before steel and is used as catalyst, the weight of the rare earth element of addition accounts for the total matter of its ingredient The percentage of amount is 0.05~0.20%；Due to the equilibrium distribution coefficient very little of rare earth, in process of setting, rare-earth enrichment is in knot The liquid phase in brilliant forward position prevents growing for crystal, and high-temperature liquid metal is made to form more cores in process of setting, to reach To the purpose of refinement crystal grain, and make the iron cobalt nickel alloy cold-strip grain size for 6~9 grades and differential within 1.5 grades.It is right For same material, the as-cast grain of alloy is thinner, and the crystal grain of rolled products is also thinner.And the rare earth element being added, in smelting During refining with the oxysulfide of other element reaction rare earths such as O, S, fusing point it is very high and stablize, molten steel after calmness, Rare earth oxide, sulfide will be excluded from steel, to purify molten steel, obtained alloy purity is higher.

Further, temperature control is at 600~800 DEG C when hot-rolled billet is into furnace, and temperature is excessively high when avoiding into furnace causes product Burning, while the waste heat after hot forging processing is efficiently used, reduce energy waste.

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

Further, total deformation is controlled 50%~65% when multiple cold rolling, critical strain can be in avoid material State generates coarse recrystal grain after leading to annealing；Multi- pass rolling can effectively make the grain size of rolled strip more Uniformly.

Further, reconditioning processing is carried out to surface before cold rolling, removes face crack.

Iron cobalt nickel alloy cold-strip production method process of the invention is simple, and easily controllable, uniformity is higher, can keep away Exempt from during subsequent processing because same batch of material grain size it is differential it is larger caused by processing technology it is different, cause the waste and production of resource Difficulty increase；By the way that rare earth element is added in smelting process and removes in subsequent cooling, blank can be effectively increased Degree of purity, while refining blank as-cast grain, lay the foundation, obtain to avoid the occurrence of coarse grain during following process Band grain size is generally at 6~9 grades；It is processed using multi-pass, the hot rolling of aximal deformation value and cold rolling, can effectively make rolled bands The grain size of material is more uniform, avoids crystal grain differential excessive, differential within 1.5 grades with a batch of product grains degree, obtains Band better adaptability.

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 pass through Ingredient → vacuumize → applying argon gas → energization → melting → plus rare earth element → power failure → casting are crossed, obtains steel ingot after cooling；? During preparing comparative example, remaining equal and embodiment production technology phase in addition to rare earth element is not added in fusion process Together, chemical element component detection is carried out using energy disperse spectroscopy to obtained blank, the rare earth member added in result and smelting process Plain component content is shown in Table 1, and wherein surplus Fe constituent content is unlisted.

Obtained embodiment steel ingot will be smelted and comparative example steel ingot carries out forging, 1280 DEG C of initial forging temperature, final forging temperature 1150 DEG C, obtain the made-up belt with a thickness of 28mm or so.

Carry out hot rolling after made-up belt is reheated, charging temperature control at 600~800 DEG C, heating temperature 1180~ 1200 DEG C, 30~40min of preheating time, 1160 DEG C of soaking time < 10min, start rolling temperature >, 1050 DEG C of finishing temperature >, eventually It rolls rear air-cooled；Rolling mill practice be 28 → 23 → 18 → 14 → 11 → 8.5 → 7 → 6 → 5 → 4.2mm, total deformation 85.0%, 9 Hot rolling pass, obtaining wall thickness is 4.2mm partly at base.

Intermediate heat-treatment is carried out at base by obtain half, then rinsed through alkali leaching, water quenching, three pickling, high pressure water, neutralized and go Except hot-working oxide skin, then carry out half-and-half carrying out reconditioning at base surface using levigator；Half answers >=4 at the every face water mill number of base It is secondary, until steel strip surface roughness reaches 2~3 μm, the defects of surface do not scratch, crackle, peeling.

Half after reconditioning is subjected to cold rolling at base, cold rolling passage is more, and strip surface roughness is smaller, surface more light It is clean；By with a thickness of the band of the embodiment 1,2,3 of 4.2mm and comparative example by different cold rolling passes be rolled down to a thickness of 1.5mm, total deflection are 64.3%, and wherein embodiment 1 rolls 5 passages, and embodiment 2 rolls 6 passages, the rolling of embodiment 37 Passage, comparative example roll 5 passages.Intermediate heat-treatment is carried out between adjacent cold rolling pass, temperature is 1080~1100 DEG C.

Band 350mm after the 1.5mm that cold rolling is obtained carries out finished product heat using protective atmosphere bright annealing unit respectively Processing, temperature are 940~960 DEG C；The hydrogen and 25% nitrogen mixed gas that bright annealing work atmosphere is 75%, avoid band Surface oxidation.

Finished product after heat treatment is sampled respectively, reference numerals, according to the regulation of YBT5231-2005 standard, true Sample is heated to 20 DEG C of 900 DEG C of scholars in empty or hydrogen atmosphere, keeps the temperature lh, is again heated to 20 DEG C of 1100 DEG C of scholars, keeps the temperature 15min, It is cooled to 200 DEG C or less with the speed no more than 5 DEG C/min to come out of the stove.Grain size detection is carried out to obtained sample, result is obtained and sees Table 2.

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

Each sample grain size testing result of table 2

As shown in Table 2, in the case where cold rolling same passage, it joined the embodiment 1 of rare earth element in smelting process The grain size of iron cobalt nickel alloy cold-strip obtained and rare earth element is not added between 6.5 grades to 8 grades in smelting process Comparative example made from iron cobalt nickel alloy cold-strip grain size compared to clearly finer and differential smaller；And by 2 He of comparative example Comparative example 3 is it is found that in a certain range with the increase of the increase of rare earth element and cold rolling pass, and obtained band grain size is more It is thin and differential smaller；By the way that rare earth element is added in smelting process and removes in subsequent cooling, base can be effectively increased The degree of purity of material, while blank as-cast grain is refined, it lays the foundation to avoid the occurrence of coarse grain during following process；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, avoid crystal grain It is differential excessive, with the differential band better adaptability within 1.5 grades, obtained of a batch of product grains degree.

Obviously, the above embodiment is merely an example for clearly illustrating the present invention, and is not to of the invention The restriction of embodiment.For those of ordinary skill in the art, it can also be made on the basis of the above description Its various forms of variation or variation.There is no necessity and possibility to exhaust all the enbodiments.And these belong to this hair The obvious changes or variations that bright spirit is extended out are still in protection scope of the present invention.

Claims (1)

1. a kind of production method of iron cobalt nickel alloy cold-strip, each chemical component which includes and Its mass percent are as follows:

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%；

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

It is characterized by comprising the following steps:

(1) ingredient → vacuumize → applying argon gas → energization → melting → plus rare earth element → power failure → casting, obtain steel after cooling Ingot；

(2) forged steel, hot rolling, multiple cold rolling and intermediate heat-treatment, finished product heat treatment；

Smelting temperature is controlled at 1500 DEG C or more, and at least one of rare earth element ce, La conduct is added before tapping in melting Catalyst, the weight percent for accounting for its ingredient gross mass of the rare earth element of addition are 0.05 ~ 0.20%；

The rare earth element of addition, reacts the oxysulfide for generating rare earth in smelting process with O, S, and molten steel is dilute after calmness Native oxide, sulfide will be excluded from steel；

Made-up belt is subjected to multistage hot deformation, finishing temperature is not less than 1050 DEG C, obtains half into base；

Temperature control is at 600~800 DEG C when hot-rolled billet is into furnace；

Total deformation is controlled 70%~85% when multiple hot rolling.