CN113293317B - Preparation method of pure nickel plate with high cold formability - Google Patents

Preparation method of pure nickel plate with high cold formability Download PDF

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CN113293317B
CN113293317B CN202110501273.4A CN202110501273A CN113293317B CN 113293317 B CN113293317 B CN 113293317B CN 202110501273 A CN202110501273 A CN 202110501273A CN 113293317 B CN113293317 B CN 113293317B
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pure nickel
semi
finished
plate blank
nickel plate
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CN113293317A (en
Inventor
丁五洲
程伟
杨哲
杨芙蓉
符先石
强乃鹏
杨永石
丁清华
杨晓荣
孙宏伟
杨娟丽
刘鹏聪
郭盛详
王俭
和平志
尹胜利
李向东
郭建华
石卫民
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Baoti Group Ltd
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Baoti Group Ltd
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making alloys
    • C22C1/02Making alloys by melting
    • C22C1/023Alloys based on nickel
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B9/00General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
    • C22B9/16Remelting metals
    • C22B9/18Electroslag remelting
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making alloys
    • C22C1/02Making alloys by melting
    • C22C1/03Making alloys by melting using master alloys
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C19/00Alloys based on nickel or cobalt
    • C22C19/03Alloys based on nickel or cobalt based on nickel
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22FCHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/10Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of nickel or cobalt or alloys based thereon
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/25Process efficiency

Abstract

The invention discloses a preparation method of a pure nickel plate with high cold formability, which comprises the following steps: carrying out vacuum induction melting on the raw materials and the melting additive to obtain a first semi-finished product, namely a pure nickel cast ingot; then carrying out electroslag remelting to obtain a finished pure nickel ingot; forging the finished pure nickel cast ingot to obtain a first semi-finished pure nickel slab; hot rolling the first semi-finished product pure nickel plate blank to obtain a second semi-finished product pure nickel plate blank; carrying out rough rolling on the second semi-finished product pure nickel plate blank on a rough rolling mill to obtain a third semi-finished product pure nickel plate blank; carrying out finish rolling on the third semi-finished product pure nickel plate blank on a continuous rolling mill set to obtain a fourth semi-finished product pure nickel plate blank; annealing and pickling the fourth semi-finished product pure nickel plate blank, and curling to obtain a fifth semi-finished product pure nickel plate blank; rolling the fifth semi-finished pure nickel plate blank, and then carrying out online bright annealing to obtain a finished pure nickel plate blank; through the processes, the pure nickel plate meeting the use requirements of special industries such as cold stamping, cold bending and the like can be obtained.

Description

Preparation method of pure nickel plate with high cold formability
Technical Field
The invention belongs to the technical field of metal material processing, and particularly relates to a preparation method of a fine-grain and high-cold-formability wide-width nickel plate.
Background
The pure nickel plate has excellent corrosion resistance and is widely applied to equipment manufacturing industries such as chemical industry, composite plate preparation and the like. But the cold stamping has extremely high requirements on the properties of toughness, bending and the like of the pure nickel plate. At present, the pure nickel materials used in the industry at home basically depend on import, the nickel belt for the plate heat exchanger produced by the titanium Bao group at home can meet the requirements of the industry, and the pure nickel thin plates produced by other manufacturers have poor cold stamping forming effect and can not meet the use requirements of the cold stamping forming industry.
At present, the product has two production processes at home, the first is a pure nickel sheet produced by adopting the traditional process, and the heat treatment process of the finished product is further adjusted, so that the plasticity of the material is enhanced, and the strength of the material is reduced, but the produced product still has larger anisotropy, large crystal grains, poor bending property and toughness, and easy cracking in cold stamping forming, thereby seriously affecting the development of the industry; the second is the chip type production process route invented by Baotii group, which changes the microstructure of the blank by effectively controlling the technological parameters of primary induction smelting, greatly improves the processing performance of the material, and finally obtains the finished product chip sheet meeting the use requirements; however, because the blank produced by the method has inherent metallurgical defects of looseness, impurities, subcutaneous air holes, shrinkage cavities and the like, the surface treatment of the material in the processing process is complicated, the production cost is high, the process is tedious, the period is long, the overall efficiency is low, and the industrial batch production is difficult to realize.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a preparation method of a pure nickel plate with high cold formability. The technical problem to be solved by the invention is realized by the following technical scheme:
a method for preparing a pure nickel plate with high cold formability comprises the following steps:
step 1: adding a pure nickel raw material and a smelting additive into a vacuum induction furnace for vacuum induction smelting to obtain a first semi-finished product, namely a pure nickel ingot; wherein the smelting additive comprises: carbon, titanium and nickel-magnesium alloy, and the smelting additive is added according to the following weight ratio based on the total weight of the pure nickel raw material: carbon is 0.01-0.03%; 0.01 to 0.10 percent of titanium; 0.05-0.1% of nickel-magnesium alloy;
step 2: sawing the head of the first semi-finished product pure nickel ingot, and then placing the head into a resistance furnace for baking to obtain a second semi-finished product pure nickel ingot; wherein the baking temperature is 400-450 ℃, and the baking time is 6.5-7.5 h;
and step 3: carrying out electroslag remelting on the second semi-finished product pure nickel ingot, and cutting off a riser and the bottom after cooling to obtain a finished product pure nickel ingot;
and 4, step 4: heating the finished pure nickel cast ingot to 980-1000 ℃, preserving heat for 5.5-6.5 h, and forging to obtain a first semi-finished pure nickel slab with the thickness of 210-230 mm; wherein the final forging temperature is not lower than 800 ℃;
and 5: heating the first semi-finished product pure nickel plate blank to 930-970 ℃, preserving heat for 3-4 hours, and carrying out hot rolling to obtain a second semi-finished product pure nickel plate blank with the thickness of 95-100 mm; wherein the finishing temperature is not lower than 750 ℃;
step 6: heating the second semi-finished pure nickel plate blank to 950-1000 ℃, preserving heat for 140-160 min, and then carrying out rough rolling on a rough rolling mill to obtain a third semi-finished pure nickel plate blank with the thickness of 30-35 mm;
and 7: heating the third semi-finished pure nickel plate blank to 950-1000 ℃, and then performing finish rolling on a continuous rolling mill set to obtain a fourth semi-finished pure nickel plate blank with the thickness of 2.0-5.0 mm;
and 8: carrying out online continuous annealing and online continuous acid washing on the fourth semi-finished pure nickel plate blank, and curling to obtain a fifth semi-finished pure nickel plate blank; wherein the annealing temperature is 680-700 ℃, and the annealing speed is 3-4 m/min;
and step 9: rolling the fifth semi-finished product pure nickel plate blank in a cold rolling unit to obtain a sixth semi-finished product pure nickel plate blank with the thickness of 0.3-2.0 mm;
step 10: carrying out online bright annealing on the sixth semi-finished pure nickel plate blank to obtain a finished pure nickel plate blank; wherein the heat treatment temperature is 690-710 ℃, and the annealing speed is 3-6 m/min.
Further, the step 1 comprises:
step 1.1: sequentially adding the pure nickel raw material, carbon and pure titanium into a vacuum induction furnace for smelting, and obtaining first liquid metal after all the pure nickel raw material, the carbon and the pure titanium are completely molten; wherein the vacuum degree in the vacuum induction furnace is less than or equal to 10 Pa; the smelting power is increased to 600kw according to a system of 50-150 kw/30 min;
step 1.2: refining the first liquid metal, then adding a nickel-magnesium alloy into the refined first liquid metal in an argon atmosphere, and melting to obtain a second liquid metal; wherein the refining time is 55-65 min, and the vacuum degree is less than 0.5Pa after the refining is finished;
step 1.3: and heating the vacuum induction furnace, pouring the second liquid metal when the temperature reaches 1520-1540 ℃, and opening the mold to cool to obtain the first semi-finished pure nickel ingot.
Further, the step 3 comprises:
step 3.1: taking the second semi-finished product of the pure nickel cast ingot as a remelting electrode, and using TiO with the weight ratio of 0.9-1: 1-1.1 2 And CaF 2 Preparing an arc striking agent and paving the arc striking agent at the bottom of the crystallizer;
step 3.2: arcing and slagging; wherein, slag charge is prepared according to the following weight ratio: CaF 2 :0.45~0.53%;Al 2 O 3 :0.21~0.25%;CaO:0.13~0.17%;MgO:0.08~0.13%;
Step 3.3: remelting the remelting electrode after the slag is completely melted, wherein TiAl alloy blocks are added into the crystallizer every 10-20 min during remelting, and the total amount of the added TiAl alloy blocks is 0.05-0.08% of the weight of the remelting electrode;
step 3.4: and after remelting, cooling the obtained cast ingot in a crystallizer, discharging, and cutting off a riser and the bottom to obtain the finished pure nickel cast ingot.
Further, the TiAl alloy block comprises the following chemical components in percentage by weight: 30 to 40 percent of Al, and the balance of Ti and inevitable impurities.
The invention has the beneficial effects that:
1. by adopting a two-step smelting process of vacuum induction smelting and electroslag remelting and by improving parameters and an operation method, the content of a key element Mg is controlled within the range of 0.005-0.05 percent, and an electroslag remelting ingot with single heavy element, low content of interstitial elements and impurity elements, fine crystal grains and excellent processing performance is obtained; and then controlling the series of process routes, methods and process parameters of forging, blank making, rough rolling, finish rolling, online processing, cold rolling, finished product heat treatment and the like to obtain a fine-grained high-cold-formability wide-width nickel plate with the unit weight of not less than 3.5t, the thickness of delta 0.3-5.0mm and the width of not less than 1350mm of the rolled finished product plate; the processing process is stable, inherent metallurgical defects such as looseness, impurities, subcutaneous air holes and shrinkage cavities and defects such as peeling and cracks do not exist, the average grain size of the finished plate is 9.5-10 grade, the anisotropy is small, the bending, plasticity and cold stamping properties are excellent, and the comprehensive properties meet various requirements in the cold stamping forming aspect;
2. compared with a sheet type production mode with long production period, high cost and low yield, the method has the advantages that the problems of peeling, leaking, edge cracking and the like of the product surface finally caused by one-time smelting defects are solved through roll type operation, the production period is shortened by 30-50 days, the yield is improved by 10-15%, and the production cost is reduced by 3.5-5%.
The present invention will be described in further detail with reference to the accompanying drawings and examples.
Drawings
FIG. 1 is a photograph of a first semi-finished pure nickel slab after trimming;
FIG. 2 is a photograph of a second semi-finished pure nickel slab;
FIG. 3 is a soft whitened delta 3.2X 1350mm nickel plate;
FIG. 4 is a gold phase diagram of a soft whitened delta 3.2X 1350mm nickel plate;
FIG. 5 is a report of the performance of a finished pure nickel plate of 3.2 mm;
FIG. 6 is a nickel plate of δ 0.6 × 1300 mm;
FIG. 7 is a gold phase diagram of a nickel plate of δ 0.6X 1300 mm;
FIG. 8 is a report of the performance of a finished pure nickel plate of 0.6 mm.
Detailed Description
The present invention will be described in further detail with reference to specific examples, but the embodiments of the present invention are not limited thereto.
Example 1
The embodiment of the invention provides a preparation method of a pure nickel plate with high cold formability, which comprises the following steps:
step 1: adding a pure nickel raw material and a smelting additive into a vacuum induction furnace for vacuum induction smelting to obtain a first semi-finished product, namely a pure nickel ingot; wherein, the pure nickel raw material is electrolytic nickel and pure nickel edges and corners; the smelting additive comprises: carbon, titanium, nickel-magnesium alloys; wherein the proportion of each component is shown in table 1, the smelting additive is added by taking the total weight of pure nickel raw materials as a base number, the carbon is 0.02 percent, the titanium is 0.02 percent, and the nickel-magnesium alloy is 0.1 percent; the proportion is beneficial to accurately controlling the content of each element and impurity elements; wherein the magnesium content in the nickel-magnesium alloy is 30 percent, the nickel content is 70 percent,
TABLE 1 addition amounts of raw materials and smelting additives
The adding proportion of the pure nickel corner is less than or equal to 30 percent, so that the influence of impurities contained in the pure nickel corner on the quality of the obtained cast ingot is prevented.
The embodiment of the invention adopts 2T vacuum induction melting, three furnaces are melted in total, and the used mold is a graphite mold with phi 480 mm; all materials need to be cleaned, then the materials are charged into a furnace and smelted, and 3 first semi-finished pure nickel ingots with the unit weights of 1763kg, 1752kg and 1780kg are prepared.
The composition of the 3 first semi-finished pure nickel ingots is shown in table 2:
TABLE 2 chemical composition testing of first semi-finished pure nickel ingots
Specifically, step 1 can be performed as follows:
step 1.1: sequentially adding electrolytic nickel, pure nickel corners, carbon and pure titanium into a vacuum induction furnace; and then, vacuumizing, slowly feeding power after the vacuum degree is less than or equal to 10Pa, heating according to a system of 50-150 kw/30min, increasing the power to 600kw, and obtaining the first liquid metal after the materials in the vacuum induction furnace are completely melted.
Step 1.2: refining the first liquid metal for 60min, wherein the vacuum degree is less than 0.5Pa after the refining is finished; and then closing the big valve, reducing the power to 350kw, filling argon into the vacuum induction furnace to 0.85-0.9 atmospheric pressure, then adding the nickel-magnesium alloy into the refined first liquid metal in the argon atmosphere, transmitting power, stirring and melting to obtain a second liquid metal.
Step 1.3: heating the vacuum induction furnace, pouring the second liquid metal when the temperature reaches 1520-1540 ℃, wherein the pouring time is 3-5 min, opening the ingot to an ingot mold chamber after pouring, cooling for 30-40 min, and discharging to obtain a first semi-finished pure nickel ingot; the power of the process is 300-400 kw.
Through the step, the first semi-finished product pure nickel cast ingot can obtain a uniform fine crystal structure under the alloying action of the additive, and the content of interstitial elements is controlled at a lower level.
Step 2: respectively sawing the heads of 3 first semi-finished pure nickel ingots, and then placing the sawed heads into a resistance furnace for baking to obtain 3 second semi-finished pure nickel ingots; wherein the baking temperature is 400-450 ℃, and the baking time is 7 h.
And step 3: and carrying out electroslag remelting on the second semi-finished product pure nickel ingot, and cutting off a dead head and the bottom after cooling to obtain the finished product pure nickel ingot.
The step 3 specifically comprises the following steps:
step 3.1: assembling and welding the three second semi-finished pure nickel ingots obtained in the step 2 end to serve as a remelting electrode, and then using TiO with the weight ratio of 0.9-1: 1-1.1 2 And CaF 2 Preparing an arc striking agent and paving the arc striking agent at the bottom of the crystallizer.
Before the remelting electrode is used, preheating is firstly carried out; the preheating temperature is 400-500 ℃, the preheating time is 6 hours, and the liquid adhered to the electrode is fully baked.
Electroslag remelting adopts a 5T electroslag furnace, and the specification of a crystallizer is phi 580/phi 620 multiplied by 2200 mm; the dummy electrode is phi 200 × 1000mm, the auxiliary electrode is phi 300 × 1300mm, and the remelting electrode is phi 480 × Lmm; checking the welding quality and concentricity between the electrodes before charging to ensure that the electrodes are centered during charging; when charging, firstly, polishing the surface of the bottom water tank and the surface of the steel ring, and then, filling the bottom water tank and the steel ring into a bottom pad, wherein the bottom pad is made of N6; filling a little slag between the bottom pad and the steel ring, and putting 200-400 g of arc striking agent on the bottom pad; finally, the crystallizer is hung on the steel ring, and the dislocation between the crystallizer and the steel ring is required to be less than 2 mm; then the remelting electrode is put into the crystallizer and is arranged on the holder, the electrode is centered on the crystallizer by adjusting the positions of the large arm and the trolley,
step 3.2: arcing and slagging;wherein, slag charge is prepared according to the following weight ratio: CaF 2 :0.45~0.53%;Al 2 O 3 :0.21~0.25%;CaO:0.13~0.17%;MgO:0.08~0.13%。
And (3) rapidly descending the remelting electrode, sending high voltage when the electrode is 100mm away from the arc striking agent, slowly descending, rapidly adding slag after arcing, manually controlling the current and the voltage to be in a stable state, finishing slag addition within 30min and finishing slag melting within 1 h.
Step 3.3: remelting the remelted electrode after the slag is completely melted, wherein TiAl alloy blocks are added into the crystallizer every 10min during remelting, the total addition amount of the TiAl alloy blocks is 4000g, and the total addition amount of the TiAl alloy blocks is 60 times during remelting; meanwhile, the amount of the TiAl alloy blocks added each time is adjusted according to the change of the smelting rate in the electroslag remelting process, the faster the smelting rate is, the more the amount of the TiAl alloy blocks is added, and in the embodiment of the invention, when the TiAl alloy blocks are added for the first 20 times in the remelting process, the amount added each time is 102 g; when the TiAl alloy block is added in the middle 20 times, the addition amount is 62g each time; when the TiAl alloy blocks are added for the last 20 times, the addition amount is 36g each time; the TiAl alloy block comprises the following chemical components in percentage by weight: 34% of Al, and the balance of Ti and inevitable impurities.
TiAl alloy is added in the electroslag remelting process, the replacement effect of active element Al is utilized, the content of Mg element is controlled within the range of 0.005-0.05%, and the defects of ingot casting peeling and cracking caused by excessive Mg element loss are avoided; meanwhile, Ti element and Al element preferentially react with oxygen element, so that oxygen enrichment of the cast ingot is effectively prevented.
The remelting process is automatic, the water temperature needs to be observed, and feeding is carried out when remelting is carried out until the electrode is about 150mm, so that pores are prevented from being formed.
Step 3.4: and after remelting, cooling the obtained cast ingot in a crystallizer for 1h, discharging, and cutting off a dead head and the bottom to obtain a finished pure nickel cast ingot.
Through the step, the cast ingot with the single weight not less than 5 tons, no metallurgical defects such as looseness, slag inclusion, shrinkage cavity, subcutaneous pores and the like can be obtained, the internal structure is purer, and a large columnar structure can be eliminated.
The chemical composition of the finished pure nickel ingot is shown in table 3:
TABLE 3 chemical composition of finished pure nickel ingots
And 4, step 4: heating the finished pure nickel cast ingot to 980-1000 ℃, preserving heat for 6 hours, and forging on an oil press to obtain a first semi-finished pure nickel plate blank with the thickness of 230 mm; wherein the final forging temperature is not lower than 800 ℃.
Heating the finished pure nickel ingot, discharging, forging the finished pure nickel ingot to delta 400 multiplied by 1000-1050 multiplied by Lmm on an oil press by adopting the operation of upsetting → rounding → flattening, then tempering for 1.5h at the temperature of 980 ℃, and finally forging the finished pure nickel ingot to delta 230 multiplied by 1050 multiplied by Lmm on the oil press; where δ represents the thickness and L represents the length.
The forging technological parameters in the step ensure that the as-cast structure of the first semi-finished pure nickel slab is fully crushed, and ensure good subsequent processing performance.
And 5: heating the first semi-finished product pure nickel plate blank to 930-970 ℃, preserving heat for 3.5 hours, and carrying out hot rolling to obtain a second semi-finished product pure nickel plate blank with the thickness of 98 mm; wherein the finishing temperature is not lower than 750 ℃.
Before cogging, the first semi-finished pure nickel slab obtained in the step 4 is planed, milled and polished, as shown in fig. 1, the slab surface is ensured to be flat and free of oxide skin, defects such as indentation, folding and cracks are avoided, the slab is manufactured in a 3300mm hot rolling unit, a roller electric furnace is used for heating, after heat preservation is carried out for 3.5 hours at the temperature of 930-970 ℃, the pure nickel slab is rolled to be delta 100 multiplied by 1350 multiplied by Lmm by one fire, then the heat is relatively flat, the slab shape is ensured to be flat, and the finish rolling temperature is ensured to be not lower than 750 ℃.
And then cutting off two ends and two side drums of the blank, and peeling off the surface, as shown in figure 2, to ensure that the head, the tail and the side edges of the strip blank are flat, the surface is smooth and flat, and no defects such as pressed objects, cracks, folding and the like can be seen by naked eyes, and finally the second semi-finished pure nickel plate blank of delta 98 multiplied by 1350 multiplied by Lmm is obtained.
The blank with excellent surface and meeting the requirements of the subsequent plate processing process can be obtained by the step.
Step 6: and heating the second semi-finished product pure nickel plate blank to 1000 ℃, preserving heat for 150min, and then carrying out rough rolling on a rough rolling mill to obtain a third semi-finished product pure nickel plate blank with the thickness of 35 mm.
Rough rolling is carried out on a four-roller rough rolling mill, and the blanks discharged from the furnace are rolled in a forward direction from delta 98mm to delta 35mm under the combined action of a vertical rolling mill; the rough rolling process is beneficial to obtaining the plate blank with good forming effect and certain processing performance.
And 7: and heating the third semi-finished pure nickel plate blank to 1000 ℃, and then performing finish rolling on a continuous rolling unit to obtain a fourth semi-finished pure nickel plate blank with the thickness of 3.2 mm.
And (3) finish rolling is carried out on a continuous rolling unit, pass deformation is reasonably distributed, and a third semi-finished pure nickel plate is rolled to delta 3.2 multiplied by 1350 multiplied by L mm through continuous rolling of a plurality of rolling mills.
The finish rolling process is favorable for obtaining the nickel plate with good plate shape, small same plate difference and excellent surface quality, and avoids the problems of cracking, breaking and the like caused by work hardening.
And step 8: carrying out online continuous annealing and online continuous acid washing on the fourth semi-finished product pure nickel plate blank, and curling to obtain a fifth semi-finished product pure nickel plate blank; wherein the annealing temperature is 680-700 ℃, and the annealing speed is 3-4 m/min.
And finishing the heat treatment and surface treatment of a fourth semi-finished pure nickel plate blank on a continuous annealing and pickling line, as shown in figure 3, then coiling the finally obtained fifth semi-finished pure nickel plate blank into a coil, bundling, sampling and detecting, as shown in figures 4 and 5, wherein the grain size of the nickel plate with the thickness of 3.2mm prepared in the step reaches 10 grades, and all mechanical properties of the nickel plate meet the use requirements.
According to the requirement of a user, if the thickness of 3.2mm is the thickness required by the user, the whole preparation process can be finished after the step is finished, and if the thickness required by the user is thinner, the preparation process is continued.
The continuous annealing and pickling process system combines the procedures of coiling and bundling, can obtain soft whitened surface finished products or semi-finished product plate strips, and simultaneously completes recrystallization, thereby obtaining good shaping improvement guarantee for subsequent processing.
And step 9: rolling the fifth semi-finished product pure nickel plate blank in a cold rolling unit to obtain a sixth semi-finished product pure nickel plate blank with the thickness of 0.6 mm;
and (3) rolling the fifth semi-finished product pure nickel plate blank in the soft state on a twenty-roller reversible cold rolling unit for 4-7 passes, and finally rolling to the thickness of 0.6mm required by the finished product, wherein the pass deformation, the rolling force and the tension are strictly controlled in the cold rolling process.
Step 10: carrying out online bright annealing on the sixth semi-finished pure nickel plate blank to obtain a finished pure nickel plate blank; as shown in FIG. 6, the heat treatment temperature is 690 to 710 ℃ and the annealing speed is 4.5 m/min.
As shown in fig. 7 and 8, the heat treatment process described in this step can obtain a finished nickel plate with a grain size of greater than or equal to 9.5 grade, satisfactory mechanical properties, high toughness and excellent cold stamping performance.
Example 2
The embodiment of the invention provides a preparation method of a pure nickel plate with high cold formability, which comprises the following steps:
step 1: adding a pure nickel raw material and a smelting additive into a vacuum induction furnace for vacuum induction smelting to obtain a first semi-finished product, namely a pure nickel ingot; wherein, the pure nickel raw material is electrolytic nickel and pure nickel corners; the smelting additive comprises: carbon, titanium, nickel-magnesium alloys; wherein the proportion of each component is shown in Table 4, the smelting additive is added by taking the total weight ratio of pure nickel raw materials as a base number, the carbon is 0.015 percent, the titanium is 0.025 percent, and the nickel-magnesium alloy is 0.08 percent; the proportion is beneficial to accurately controlling the content of each element and impurity elements; wherein, the magnesium content in the nickel-magnesium alloy is 30 percent, and the nickel content is 70 percent.
TABLE 4 addition amounts of raw materials and smelting additives
The adding proportion of the pure nickel corner is less than or equal to 30 percent, so that the influence of impurities contained in the pure nickel corner on the quality of the obtained cast ingot is prevented.
The embodiment of the invention adopts 2T vacuum induction melting, three furnaces are melted in total, and the used mold is a graphite mold with phi 480 mm; all materials must be cleaned, then the materials are charged into a furnace and smelted, and 3 first semi-finished pure nickel ingots with the single weights of 1760kg, 1752kg and 1779kg are prepared.
The composition of the 3 first semi-finished pure nickel ingots is shown in table 5:
TABLE 5 chemical composition testing of first semi-finished pure nickel ingots
Specifically, step 1 can be performed as follows:
step 1.1: sequentially adding electrolytic nickel, pure nickel corners, carbon and pure titanium into a vacuum induction furnace; and then, vacuumizing, slowly feeding power after the vacuum degree is less than or equal to 10Pa, heating according to a system of 50-150 kw/30min, increasing the power to 600kw, and obtaining the first liquid metal after the materials in the vacuum induction furnace are completely melted.
Step 1.2: refining the first liquid metal for 63min, wherein the vacuum degree is less than 0.5Pa after the refining is finished; and then closing the big valve, reducing the power to 400kw, filling argon into the vacuum induction furnace to 0.85-0.9 atmospheric pressure, then adding the nickel-magnesium alloy into the refined first liquid metal in the argon atmosphere, transmitting power, stirring and melting to obtain a second liquid metal.
Step 1.3: heating the vacuum induction furnace, pouring the second liquid metal when the temperature reaches 1520-1540 ℃, wherein the pouring time is 3-5 min, opening the ingot to an ingot mold chamber after pouring, cooling for 30-40 min, and discharging to obtain a first semi-finished pure nickel ingot; the power of the process is 300-400 kw.
Through the step, the first semi-finished product pure nickel cast ingot can obtain a uniform fine crystal structure under the alloying action of the additive, and the content of interstitial elements is controlled at a lower level.
Step 2: respectively sawing the heads of 3 first semi-finished pure nickel ingots, and then placing the sawed heads into a resistance furnace for baking to obtain 3 second semi-finished pure nickel ingots; wherein the baking temperature is 400-450 ℃, and the baking time is 7.5 h.
And 3, step 3: and carrying out electroslag remelting on the second semi-finished product pure nickel ingot, and cutting off a dead head and the bottom after cooling to obtain the finished product pure nickel ingot.
The step 3 specifically comprises the following steps:
step 3.1: assembling and welding the three second semi-finished pure nickel ingots obtained in the step 2 end to serve as a remelting electrode, and then using TiO with the weight ratio of 0.9-1: 1-1.1 2 And CaF 2 Preparing an arc striking agent and paving the arc striking agent at the bottom of the crystallizer.
Before the remelting electrode is used, preheating is firstly carried out; the preheating temperature is 400-500 ℃, the preheating time is 5.5 hours, and the liquid adhered to the electrode is fully baked.
Electroslag remelting adopts a 5T electroslag furnace, and the specification of a crystallizer is phi 580/phi 620 multiplied by 2200 mm; the dummy electrode is phi 200 multiplied by 1000mm, the auxiliary electrode is phi 300 multiplied by 1300mm, and the remelting electrode is phi 480 multiplied by Lmm; checking the welding quality and concentricity between the electrodes before charging to ensure that the electrodes are centered during charging; during charging, the surface of the bottom water tank and the surface of the steel ring are polished clean and then are loaded into a bottom pad, and the bottom pad is made of N6; filling a little slag between the bottom pad and the steel ring, and putting 200-400 g of arc striking agent on the bottom pad; finally, hoisting the crystallizer on the steel ring, wherein the dislocation between the crystallizer and the steel ring is required to be less than 2 mm; then the remelting electrode is put into the crystallizer and is arranged on the holder, the electrode is centered on the crystallizer by adjusting the positions of the large arm and the trolley,
step 3.2: arcing and slagging; wherein, slag charge is prepared according to the following weight ratio: CaF 2 :0.45~0.53%;Al 2 O 3 :0.21~0.25%;CaO:0.13~0.17%;MgO:0.08~0.13%。
And (3) rapidly descending the remelting electrode, sending high voltage when the electrode is 100mm away from the arc striking agent, slowly descending, rapidly adding slag after arcing, manually controlling the current and the voltage to be in a stable state, finishing slag addition within 30min and finishing slag melting within 1 h.
Step 3.3: remelting the remelting electrode after the slag is completely melted, wherein TiAl alloy blocks are added into the crystallizer every 20min during remelting, the total addition amount of the TiAl alloy blocks is 3740g, and the total addition amount of the TiAl alloy blocks is 30 times during remelting; meanwhile, the amount of the TiAl alloy blocks added each time is adjusted according to the change of the smelting rate in the electroslag remelting process, the faster the smelting rate is, the more the amount of the TiAl alloy blocks are added, and in the embodiment of the invention, when the TiAl alloy blocks are added for the first 10 times in the remelting process, the amount added each time is 192 g; when the TiAl alloy block is added in the middle 10 times, the addition amount is 116g each time; when the TiAl alloy blocks are added for the last 10 times, the addition amount is 66g each time; the TiAl alloy block comprises the following chemical components in percentage by weight: 38% of Al, and the balance of Ti and inevitable impurities.
TiAl alloy is added in the electroslag remelting process, the replacement effect of active element Al is utilized, the content of Mg element is controlled within the range of 0.005-0.05%, and the defects of ingot casting peeling and cracking caused by excessive Mg element loss are avoided; meanwhile, Ti element and Al element preferentially react with oxygen element, so that oxygen enrichment of the cast ingot is effectively prevented.
The remelting process is automatic, the water temperature needs to be observed, and feeding is carried out when remelting is carried out until the electrode is about 150mm, so that pores are prevented from being formed.
Step 3.4: and after remelting, cooling the obtained cast ingot in a crystallizer for 1h, discharging, and cutting off a dead head and the bottom to obtain a finished pure nickel cast ingot.
Through the step, the cast ingot with the single weight not less than 5 tons, no metallurgical defects such as looseness, slag inclusion, shrinkage cavity, subcutaneous pores and the like can be obtained, the internal structure is purer, and a large columnar structure can be eliminated.
And 4, step 4: heating the finished pure nickel cast ingot to 980-1000 ℃, preserving heat for 6.5 hours, and forging on an oil press to obtain a first semi-finished pure nickel plate blank with the thickness of 220 mm; wherein the final forging temperature is not lower than 800 ℃.
Heating the finished pure nickel ingot, discharging, forging the finished pure nickel ingot to delta 400 multiplied by 1000-1050 multiplied by Lmm on an oil press by adopting the operation of upsetting → rounding → flattening, then tempering for 1.5h at 980 ℃, and finally forging the finished pure nickel ingot to delta 220 multiplied by 1050 multiplied by Lmm on the oil press; where δ represents the thickness and L represents the length.
The forging technological parameters in the step ensure that the as-cast structure of the first semi-finished pure nickel slab is fully crushed, and ensure good subsequent processing performance.
And 5: heating the first semi-finished product pure nickel plate blank to 930-970 ℃, preserving heat for 4 hours, and carrying out hot rolling to obtain a second semi-finished product pure nickel plate blank with the thickness of 95 mm; wherein the finishing temperature is not lower than 750 ℃.
Before cogging, the first semi-finished pure nickel plate blank obtained in the step 4 is planed, milled and polished to ensure that the surface of the plate blank is smooth and has no oxide skin, no defects such as indentation, folding, cracks and the like, the plate blank is manufactured in a 3300mm hot rolling unit, a roller electric furnace is used for heating, heat preservation is carried out for 3.5 hours at the temperature of 930-970 ℃, then the pure nickel plate blank is rolled to be delta 98 multiplied by 1350 multiplied by Lmm by one fire, and then the plate blank is heated to be flat to ensure that the plate shape is smooth and the finish rolling temperature is not lower than 750 ℃.
And then cutting off two ends and two side drums of the blank, and peeling the surface to ensure that the head, the tail and the side edges of the strip blank are smooth and flat, the surface is smooth and flat, and the defects of pressed objects, cracks, folding and the like which can be seen by naked eyes are avoided, and finally the second semi-finished pure nickel plate blank of delta 95 multiplied by 1350 multiplied by Lmm is obtained.
The blank with excellent surface and meeting the requirement of the subsequent plate processing technology can be obtained by the step.
Step 6: and heating the second semi-finished product pure nickel plate blank to 1000 ℃, preserving the heat for 160min, and then carrying out rough rolling on a rough rolling machine to obtain a third semi-finished product pure nickel plate blank with the thickness of 30 mm.
Rough rolling is carried out on a four-roller rough rolling mill, and the blanks discharged from the furnace are rolled in a forward direction from delta 95mm to delta 30mm under the combined action of a vertical rolling mill; the rough rolling process is beneficial to obtaining the plate blank with good forming effect and certain processing performance.
And 7: and heating the third semi-finished product pure nickel plate blank to 1000 ℃, and then performing finish rolling on a continuous rolling unit to obtain a fourth semi-finished product pure nickel plate blank with the thickness of 3.2 mm.
And (3) finish rolling is carried out on a continuous rolling unit, pass deformation is reasonably distributed, and a third semi-finished pure nickel plate is rolled to delta 3.2 multiplied by 1350 multiplied by L mm through continuous rolling of a plurality of rolling mills.
The finish rolling process is beneficial to obtaining the nickel plate with good plate shape, small same plate difference and good surface quality, and avoids the problems of cracking, breaking and the like caused by work hardening.
And 8: carrying out online continuous annealing and online continuous acid washing on the fourth semi-finished product pure nickel plate blank, and curling to obtain a fifth semi-finished product pure nickel plate blank; wherein the annealing temperature is 680-700 ℃, and the annealing speed is 3-4 m/min.
And finishing the heat treatment and surface treatment of the fourth semi-finished pure nickel plate blank on a continuous annealing and pickling line, then coiling the finally obtained fifth semi-finished pure nickel plate blank into a coil, bundling, sampling and detecting.
According to the requirement of a user, if the thickness of 3.2mm is the thickness required by the user, the whole preparation process can be finished after the step is finished, and if the thickness required by the user is thinner, the preparation process is continued.
The continuous annealing and pickling process system combines the procedures of coiling and bundling, can obtain soft whitened surface finished products or semi-finished product plate strips, and simultaneously completes recrystallization, thereby obtaining good shaping improvement guarantee for subsequent processing.
And step 9: rolling the fifth semi-finished product pure nickel plate blank in a cold rolling unit to obtain a sixth semi-finished product pure nickel plate blank with the thickness of 0.6 mm;
and (3) rolling the fifth semi-finished product pure nickel plate blank in the soft state on a twenty-roller reversible cold rolling unit for 4-7 passes, and finally rolling to the thickness of 0.6mm required by the finished product, wherein the pass deformation, the rolling force and the tension are strictly controlled in the cold rolling process.
Step 10: carrying out online bright annealing on the sixth semi-finished pure nickel plate blank to obtain a finished pure nickel plate blank; wherein the heat treatment temperature is 690-710 ℃, and the annealing speed is 4.5 m/min.
The pure nickel slab with delta 3.2mm obtained in step 9 of example 1 and example 2 and the nickel slab with delta 0.6mm finally obtained were sampled and analyzed, and the detection results are shown in table 6:
TABLE 6 test results of nickel plate
The non-metallic inclusion of the finished pure nickel plate is analyzed, and the result shows that: the sulfide and the carbide both meet the first-grade requirement of B.1; the chemical analysis results show that the content control of the interstitial element, S, P and the like has good effects, and the detection results are shown in table 7:
TABLE 7 composition analysis of finished pure nickel plate
Element(s) O N H S P C
Content/% ≤0.0019 <0.0005 <0.001 <0.001 <0.001 <0.01
The results show that the nickel plate with high cold formability prepared by the invention has lower production cost, short period and much higher comprehensive yield than sheet type operation; through finished product detection and actual stamping tests, various properties of the plate can meet dual requirements of use and related standards, the plate has excellent comprehensive performance and good cold stamping forming effect, and the success rate of one-time stamping exceeds 99.7 percent and exceeds 97 percent of the success rate required by imported materials.
By the method, the invention can achieve the following beneficial effects:
1. by improving the melting process parameters and the operation method of the two-step vacuum induction melting and electroslag remelting, an electroslag remelting ingot with single weight and high metallurgical quality is obtained, the content of a key element Mg is controlled within the range of 0.005-0.05%, so that a pure nickel plate with high surface quality is obtained, the processing process is stable, inherent metallurgical defects such as looseness, inclusion, subcutaneous air holes and shrinkage cavities and the like and defects such as peeling, cracks and the like are avoided, the average grain size of a finished plate is 9.5-10 grades, the anisotropy is small, and the bending, plasticity and cold stamping performance are excellent;
2. compared with a sheet type production mode with long production period, high cost and low yield, the roll type operation not only solves the problems of peeling, leaking, edge cracking and the like of the product surface finally caused by the defect of one-time smelting, but also shortens the production period by 30-50 days, improves the yield by 10-15% and reduces the production cost by 3.5-5%.
In the description of the present invention, the terms "first", "second", "third", "fourth", "fifth", "sixth" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implying any number of technical features indicated. Thus, features defined as "first", "second", "third", "fourth", "fifth", "sixth" may explicitly or implicitly include one or more of the features. In the description of the present invention, "a number" means two or more unless specifically limited otherwise.
The foregoing is a further detailed description of the invention in connection with specific preferred embodiments and it is not intended to limit the invention to the specific embodiments described. For those skilled in the art to which the invention pertains, several simple deductions or substitutions can be made without departing from the spirit of the invention, and all shall be considered as belonging to the protection scope of the invention.

Claims (1)

1. A method for preparing a pure nickel plate with high cold formability is characterized by comprising the following steps:
step 1: adding a pure nickel raw material and a smelting additive into a vacuum induction furnace for vacuum induction smelting to obtain a first semi-finished product, namely a pure nickel ingot; the smelting additive is composed of carbon, titanium and nickel-magnesium alloy, and is added according to the following weight ratio by taking the total weight of the pure nickel raw material as a base: 0.01-0.03% of carbon; 0.01 to 0.10 percent of titanium; 0.05-0.1% of nickel-magnesium alloy;
the step 1 comprises the following steps:
step 1.1: sequentially adding the pure nickel raw material, carbon and titanium into a vacuum induction furnace for smelting, and obtaining first liquid metal after the pure nickel raw material, the carbon and the titanium are completely molten; wherein the vacuum degree in the vacuum induction furnace is less than or equal to 10 Pa; the smelting power is increased to 600k W according to a rule of 50-150 k W/30 min;
step 1.2: refining the first liquid metal, then adding a nickel-magnesium alloy into the refined first liquid metal in an argon atmosphere, and melting to obtain a second liquid metal; wherein the refining time is 55-65 min, and the vacuum degree is less than 0.5Pa after the refining is finished;
step 1.3: heating the vacuum induction furnace, pouring the second liquid metal when the temperature reaches 1520-1540 ℃, and opening the mold to cool to obtain the first semi-finished pure nickel ingot;
step 2: sawing the head of the first semi-finished product pure nickel ingot, and then placing the head into a resistance furnace for baking to obtain a second semi-finished product pure nickel ingot; wherein the baking temperature is 400-450 ℃, and the baking time is 6.5-7.5 h;
and step 3: carrying out electroslag remelting on the second semi-finished product pure nickel ingot, and cutting off a riser and the bottom after cooling to obtain a finished product pure nickel ingot;
the step 3 comprises the following steps:
step 3.1: taking the second semi-finished product of the pure nickel cast ingot as a remelting electrode, and using TiO with the weight ratio of 0.9-1: 1-1.1 2 And CaF 2 Preparing an arc striking agent and paving the arc striking agent at the bottom of the crystallizer;
step 3.2: arcing and slagging;
step 3.3: remelting the remelted electrode after the slag is completely melted, wherein a TiAl alloy block is added into the crystallizer every 10-20 min during remelting, and the content of Mg is controlled within the range of 0.005-0.05% by mass percent; the total addition amount of the TiAl alloy blocks is 0.05-0.08% of the weight of the remelting electrode; the TiAl alloy block comprises the following chemical components in percentage by weight: 30-40% of Al, and the balance of Ti and inevitable impurities;
step 3.4: after remelting, cooling the obtained cast ingot in a crystallizer, discharging, and cutting off a riser and the bottom to obtain the finished pure nickel cast ingot;
and 4, step 4: heating the finished pure nickel cast ingot to 980-1000 ℃, preserving heat for 5.5-6.5 h, and then forging to obtain a first semi-finished pure nickel slab with the thickness of 210-230 mm; wherein the final forging temperature is not lower than 800 ℃;
and 5: heating the first semi-finished pure nickel plate blank to 930-970 ℃, preserving heat for 3-4 h, and carrying out hot rolling to obtain a second semi-finished pure nickel plate blank with the thickness of 95-100 mm; wherein the finishing temperature is not lower than 750 ℃;
and 6: heating the second semi-finished pure nickel plate blank to 950-1000 ℃, preserving heat for 140-160 min, and then carrying out rough rolling on a rough rolling mill to obtain a third semi-finished pure nickel plate blank with the thickness of 30-35 mm;
and 7: heating the third semi-finished pure nickel plate blank to 950-1000 ℃, and then performing finish rolling on a continuous rolling mill set to obtain a fourth semi-finished pure nickel plate blank with the thickness of 2.0-5.0 mm;
and 8: carrying out on-line continuous annealing and on-line continuous acid washing on the fourth semi-finished pure nickel plate blank, and coiling to obtain a fifth semi-finished pure nickel plate blank; wherein the annealing temperature is 680-700 ℃, and the annealing speed is 3-4 m/min;
and step 9: rolling the fifth semi-finished product pure nickel plate blank in a cold rolling unit to obtain a sixth semi-finished product pure nickel plate blank with the thickness of 0.3-2.0 mm;
step 10: carrying out online bright annealing on the sixth semi-finished pure nickel plate blank to obtain a finished pure nickel plate blank; wherein the heat treatment temperature is 690-710 ℃, and the annealing speed is 3-6 m/min.
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