CN117821850A - Hard glass seals and uses resistantEtching Ni 29 Co 17 Cr 2 Cu 3 Alloy strip and method for producing same - Google Patents
Hard glass seals and uses resistantEtching Ni 29 Co 17 Cr 2 Cu 3 Alloy strip and method for producing same Download PDFInfo
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- 238000005275 alloying Methods 0.000 claims description 12
- 229910052799 carbon Inorganic materials 0.000 claims description 12
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- UGKDIUIOSMUOAW-UHFFFAOYSA-N iron nickel Chemical compound [Fe].[Ni] UGKDIUIOSMUOAW-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/25—Process efficiency
Abstract
The invention provides a corrosion-resistant Ni for hard glass sealing 29 Co 17 Cr 2 Cu 3 Alloy strip and method of producing the same. According to the requirement of the material on the fixed expansion characteristic, corrosion resistance and high reliability, the alloy is prepared from the original iron-based Ni 29 Co 17 Based on the design of copper and chromium control, and reasonably optimizing the proportion of nickel, cobalt, manganese, chromium, copper and silicon, the corrosion-resistant Ni for sealing high-quality hard glass is ensured 29 Co 17 Cr 2 Cu 3 The alloy strip has excellent performance, improves corrosion resistance and thermal expansion stability, strictly controls raw materials and auxiliary materials, reduces the increase of residual and harmful element contents, and aims to ensure low gas content, high cleanliness and high structural uniformity of the strip.
Description
Technical Field
The invention belongs to the technical field of metal functional materials, and particularly relates to corrosion-resistant Ni for hard glass sealing 29 Co 17 Cr 2 Cu 3 Alloy strip and method of producing the same.
Background
Iron-based Ni 29 Co 17 The alloy belongs to a hard glass sealing alloy, the expansion coefficient of the alloy is close to that of silicon-boron hard glass, and an oxide film formed by glass and alloy sealing can be well infiltrated. Iron-based Ni 29 Co 17 The alloy is mainly used for leading out electric vacuum components such as a transmitting tube, an oscillating tube, a igniting tube, a magnetron, a transistor, a sealing plug, a relay and an integrated circuitGlass seals for wires, chassis, housing, brackets, etc. With the development of large-scale integrated circuits and very large-scale integrated circuits, the iron-based Ni29Co17 alloy product is required to be applied in the severe natural environment with high temperature, high humidity and high salt mist, and development of high-quality corrosion-resistant iron-based Ni is urgently needed 29 Co 17 The alloy strip meets the market demand.
In the prior art, the iron-based Ni is widely used for manufacturing electric vacuum components 29 Co 17 The alloy strip has extremely stable thermal expansion characteristics under the condition of extreme temperature change, and can maintain equipment stability, reliability and instrument control precision, but the alloy strip needs to have extremely strong corrosion resistance and high uniformity of tissues as the material is required to have conventional stability when applied under the severe natural environment of high temperature, high humidity and high salt mist.
Disclosure of Invention
The invention aims to solve the problems of insufficient corrosion resistance and fluctuation of tissue uniformity of the existing material, and needs to design, develop and produce the high-quality corrosion-resistant Ni for hard glass sealing 29 Co 17 Cr 2 Cu 3 The alloy strip and the production method thereof realize the situations of stable product performance, good corrosion resistance and alleviation of the shortage of market application.
The invention adopts the following technical scheme: corrosion-resistant Ni for hard glass sealing 29 Co 17 Cr 2 Cu 3 The alloy strip comprises the following components in percentage by weight: less than or equal to 0.05 percent of C, 0.01 to 0.20 percent of Si, 0.10 to 0.50 percent of Mn, 28.5 to 29.5 percent of Ni, 17 to 17.5 percent of Co, 2.0 to 3.0 percent of Cu, 1.0 to 2.0 percent of Cr, less than or equal to 0.20 percent of Mo, less than or equal to 0.015 percent of P, less than or equal to 0.008 percent of S, less than or equal to 0.0020 percent of O, less than or equal to 0.0030 percent of N, less than or equal to 0.0005 percent of H, and the balance of Fe.
In a further embodiment, the composition comprises the following components in weight percent:
less than or equal to 0.03 percent of C, 0.05 to 0.15 percent of Si, 0.20 to 0.35 percent of Mn, 28.5 to 29.0 percent of Ni, 15.5 to 17.5 percent of Co, 2.5 to 3.0 percent of Cu, 1.5 to 2.0 percent of Cr, less than or equal to 0.15 percent of Mo, less than or equal to 0.010 percent of P, less than or equal to 0.005 percent of S, less than or equal to 0.0015 percent of O, less than or equal to 0.0025 percent of N, less than or equal to 0.0003 percent of H, and the balance of Fe.
In a further embodiment, the Ni 29 Co 17 Cr 2 Cu 3 The pitting corrosion resistance equivalent PREN of the alloy strip is more than or equal to 1.5;
wherein pren=cr (%) +3×mo (%) +30×n (%).
In a further embodiment, the Ni 29 Co 17 Cr 2 Cu 3 The reheat crack sensitivity coefficient of the alloy strip is less than or equal to 3.0;
wherein psr=cr (%) +cu (%) +2mo (%) +10v (%) +7nb (%) +5ti (%) -2.
In a further embodiment, the Ni 29 Co 17 Cr 2 Cu 3 The cold crack sensitivity coefficient PCM of the alloy strip is less than or equal to 0.95; wherein,
PCM＝C(％)+Si(％)/30+[Mn(％)+Cr(％)+Cu]/20+Ni(％)/60+Mo(％)/15+V(％)/10+5B(％)
preparation of corrosion-resistant Ni for sealing of hard glass as described above 29 Co 17 Cr 2 Cu 3 The preparation method of the alloy strip comprises the following steps:
smelting in a vacuum induction furnace: the raw materials are prepared according to the following steps: the method comprises the steps of electrolyzing nickel, cobalt, low-sulfur pure iron, carbon spectrum electrodes in high-purity graphite and crystalline silicon, and sequentially carrying out the following treatment on the raw materials to obtain premelted slag; charging, melting, refining, alloying and casting;
step two, electroslag remelting: pretreating an electrode rod and premelting slag, remelting the electrode rod by using an argon protective atmosphere electroslag furnace, wherein the premelting slag is remelted by adopting a quaternary slag system and four-stage control;
step three, forging: the steel ingot charging temperature is less than or equal to 800 ℃, the temperature rising rate of a cold furnace is less than or equal to 200 ℃/h, when the temperature in the furnace is more than 800 ℃, the temperature rising rate is less than or equal to 300 ℃/h, the heat preservation temperature is 1160+/-30 ℃, the heat preservation time is 3-4 h, the forging opening temperature is more than or equal to 1120 ℃, and the final forging temperature is more than or equal to 880 ℃;
step four, hot rolling: the steel ingot charging temperature is less than or equal to 700 ℃, the temperature rising rate of a cold furnace is less than or equal to 100 ℃/h, when the temperature in the furnace is more than 700 ℃, the temperature rising rate is less than or equal to 300 ℃/h, the heat preservation temperature is 1150+/-30 ℃, the heat preservation time is 30-40 min, the initial rolling temperature is more than or equal to 1150 ℃, and the final rolling temperature is more than or equal to 900 ℃;
step five, cold rolling: the maximum total deformation degree of a single rolling process is less than or equal to 70 percent; the maximum pass deformation degree is less than or equal to 25%, the first pass deformation degree is less than or equal to 15%, the intermediate pass deformation degree is less than or equal to 20%, and the final 1 st to 2 nd pass deformation degree is less than or equal to 10%;
step six, annealing: and annealing the blank and the semi-finished product in the strip process by adopting a three-zone temperature-control pure hydrogen protective atmosphere continuous annealing furnace, and annealing the intermediate cold-rolled strip: 980 ℃ and annealing the semi-finished cold-rolled strip: 950 DEG C
Seventhly, 23 roller withdrawal and straightening: controlling the strip shape, correcting the strip shape of the finished strip by adopting a 23-roller straightening and withdrawal machine, wherein the deformation of the straightening and withdrawal machine is less than or equal to 0.2 percent.
In a further embodiment, the step one specifically includes the steps of:
step 101, charging: high-purity carbon and low-sulfur pure iron are sequentially filled in the middle position of the bottom of the crucible, and cobalt and chromium are electrolyzed; the middle and upper parts of the crucible are filled with nickel plates, and crystalline silicon, electrolytic manganese, electrolytic copper and Ni-Mg are filled into a feeder.
Step 102, melting: vacuum pumping is carried out in a furnace, when the vacuum degree is less than or equal to 20Pa, power transmission melting is carried out, low-power transmission is carried out with the power less than or equal to 200KW, and the temperature is gradually raised by slow heating;
step 103, refining: after the furnace burden is cleared, the power is transmitted to 300-480 KW for 5min, the power is adjusted to 200-300 KW after the temperature reaches 1625+ -25 ℃, and the temperature of molten steel is adjusted to 1600+ -15 ℃ to enter the refining period; refining time is 45-60 min;
step 104, alloying: charging argon gas of 2-4Kpa, adding Si and Mn, melting, tilting the crucible for at least 5 times, wherein the power is 400kW, stirring for 3 minutes by UDS, controlling the alloying temperature at 1530+/-15 ℃, and maintaining for 10-15 minutes; stirring, controlling the temperature, charging Ar gas at 1510+/-10 ℃ and 2-4kPa, adding Ni-Mg, and mechanically stirring in a shaking furnace or carrying out UDS electromagnetic stirring;
step 105, casting: controlling the power transmission, and tilting the crucible to perform casting after the temperature reaches the requirement of the casting superheat degree, wherein the power of charged casting is less than or equal to 100KW; after casting, standing for 10 min in vacuum state, and then breaking and hanging out the casting mould.
In a further embodiment, the quaternary slag system in the second step is: caF (CaF) 2 、Al 2 O 3 、CaO、MgO；
The four-stage control is represented by: the arcing slag melting current is 2000-5000A, and the voltage is 38-51V; current 6500-7500A and voltage 45-52V in current lifting stage; the current in the remelting stage is 6500-7000A, and the voltage is 46-52V; the current in the feeding stage is 6500-4000A, and the voltage is 52-43V.
The invention has the beneficial effects that: in the original iron-based Ni 29 Co 17 Copper and chromium are controlled on the basis, and the proportion of nickel, cobalt, manganese, chromium, copper and silicon is reasonably optimized, and pitting corrosion resistance equivalent, reheat crack sensitivity coefficient and cold crack sensitivity coefficient are introduced; improving Ni by introducing pitting corrosion resistance equivalent, reheat crack sensitivity coefficient and cold crack sensitivity coefficient three-control optimal solution 29 Co 17 Cr 2 Cu 3 Alloy strip combination property. Pitting resistance equivalent for an austenite single-phase structure, the higher the pitting resistance equivalent, the better. The reheat crack sensitivity coefficient (PSR) and the cold crack sensitivity coefficient (PCM) reflect the relation between chemical components and the sensitivity of hot and cold cracks, and the smaller the heat and cold crack sensitivity coefficient is, the better the sealability of the alloy is, the design PREN is more than or equal to 1.5, the PSR is less than or equal to 3.0, and the PCM is less than or equal to 0.95.
Corrosion resistant Ni for high quality hard glass sealing of the present invention 29 Co 17 Cr 2 Cu 3 The alloy strip and the production method thereof have the advantages that the effects of vacuum induction furnace smelting, electroslag remelting, forging, hot rolling, cold rolling, annealing and 23-roller withdrawal and straightening are obvious, the surface quality of the strip is effectively improved, the yield is improved, and the effective cost is little.
Corrosion resistant Ni for high quality hard glass sealing of the present invention 29 Co 17 Cr 2 Cu 3 Alloy strip and production method thereof, copper and chromium control and low gas content control are adopted, and thermodynamic stability elements copper and chromium are added into nickel-iron-based alloy to form solid solution and improve Ni 29 Co 17 Cr 2 Cu 3 The alloy electrode potential improves the corrosion resistance of the alloy strip. The lower gas content control can reduce the impurity atoms in crystal defectsThe displacement and rearrangement of atoms in the crystal affect the influence of the change of the crystal size on the thermal expansion coefficient, so that the alloy strip with good sealing performance is obtained.
Corrosion resistant Ni for high quality hard glass sealing of the present invention 29 Co 17 Cr 2 Cu 3 The alloy strip has obvious effect of improving the material structure property and corrosion resistance, and the corrosion weight is increased from 3 to 4.5.10 in the prior weather atmosphere exposure test of high temperature, high humidity and high salt fog for 180 days -4 g/mm 2 Reduced to less than or equal to 2.5.10 -4 g/mm 2 The corrosion resistance can completely meet the use requirement in island environments.
Drawings
FIG. 1 is a microstructure of a corrosion resistant Ni29Co17Cr2Cu3 alloy strip for high quality hard glass sealing according to the invention.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to fig. 1 of the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention. In order to solve the problems of insufficient corrosion resistance and fluctuation of tissue uniformity of materials in the prior art, the invention provides a corrosion-resistant Ni for sealing high-quality hard glass 29 Co 17 Cr 2 Cu 3 A method for producing an alloy strip. According to the requirement of the material on the fixed expansion characteristic, corrosion resistance and high reliability, the alloy is prepared from the original iron-based Ni 29 Co 17 Based on the design of copper and chromium control, and reasonably optimizing the proportion of nickel, cobalt, manganese, chromium, copper and silicon, the corrosion-resistant Ni for sealing high-quality hard glass is ensured 29 Co 17 Cr 2 Cu 3 The alloy strip has excellent performance, improves corrosion resistance and thermal expansion stability, controls the original and auxiliary materials strictly, reduces the increase of residual and harmful element contents, ensures the low gas content, high cleanliness and high tissue uniformity of the strip, and prolongs the process in the initial stage of vacuum meltingLong melting time, increased refining time, optimized alloying time, heat preservation and continuous slow casting, and obtaining the high-purity fine-grain original steel ingot.
Ni is improved by adopting pure hydrogen continuous annealing furnace process production through hot forging, hot rolling heating time, final forging and final rolling temperature control and cold rolling cold deformation pass optimization 29 Co 17 Cr 2 Cu 3 The alloy strip has a structural shape to meet the requirement of constant expansion and corrosion resistance.
In order to achieve the above object, the present embodiment provides a high-quality corrosion-resistant Ni for sealing hard glass 29 Co 17 Cr 2 Cu 3 The alloy strip comprises the following components in percentage by weight: less than or equal to 0.05 percent of C, 0.01 to 0.20 percent of Si, 0.10 to 0.50 percent of Mn, 28.5 to 29.5 percent of Ni, 15.5 to 17.5 percent of Co, 2.0 to 3.0 percent of Cu, 1.0 to 2.0 percent of Cr, less than or equal to 0.20 percent of Mo, less than or equal to 0.015 percent of P, less than or equal to 0.008 percent of S, less than or equal to 0.0020 percent of O, less than or equal to 0.0030 percent of N, less than or equal to 0.0005 percent of H, and the balance of Fe.
Further, the composition comprises the following components in percentage by weight:
less than or equal to 0.03 percent of C, 0.05 to 0.15 percent of Si, 0.20 to 0.35 percent of Mn, 28.5 to 29.0 percent of Ni, 17 to 17.5 percent of Co, 2.5 to 3.0 percent of Cu, 1.5 to 2.0 percent of Cr, less than or equal to 0.15 percent of Mo, less than or equal to 0.010 percent of P, less than or equal to 0.005 percent of S, less than or equal to 0.0015 percent of O, less than or equal to 0.0025 percent of N, less than or equal to 0.0003 percent of H, and the balance of Fe.
It should be noted that the number of the substrates, ni (Ni) 29 Co 17 Cr 2 Cu 3 The pitting corrosion resistance equivalent PREN of the alloy strip is more than or equal to 1.5; wherein pren=cr (%) +3×mo (%) +30×n (%).
Ni 29 Co 17 Cr 2 Cu 3 The reheat crack sensitivity coefficient of the alloy strip is less than or equal to 3.0; wherein psr=cr (%) +cu (%) +2mo (%) +10v (%) +7nb (%) +5ti (%) -2.
The Ni is 29 Co 17 Cr 2 Cu 3 The cold crack sensitivity coefficient PCM of the alloy strip is less than or equal to 0.95; wherein pcm=c (%) +si (%)/30+ [ Mn (%) +cr (%) +cu ]]/20+Ni(％)/60+Mo(％)/15+V(％)/10+5B(％)。
To prepare Ni with the above properties 29 Co 17 Cr 2 Cu 3 Alloy strip, this example also provides corrosion resistant Ni for high quality hard glass sealing 29 Co 17 Cr 2 Cu 3 The main preparation principle of the alloy strip production method comprises two aspects:
chemical component optimization, copper and chromium alloying and low gas content control are adopted: the melting period is rapidly pumped by a carbon-oxygen reaction vacuum pump in a vacuum environment, the power and vacuum parameters in the melting period are optimized to achieve an effective degassing effect, alloying time is controlled to achieve the purpose of uniform molten steel, continuous slow steady casting control is adopted in the casting process, and electroslag remelting with gas-retaining constant melting speed is matched to secondarily purify the primary smelting steel ingot and improve the as-cast structure, so that the steel ingot with high cleanliness and uniform structure is obtained.
Cold rolling cogging and rolling: the rolling deformation of the cold rolling cogging is controlled according to a parabolic curve, the deformation of single pass and single rolling pass is produced by considering the work hardening index, and the deformation resistance of each pass tends to be consistent, so that the effect of uniform deformation of the cold-rolled strip is obtained, and the maximum total deformation of the single rolling pass is less than or equal to 70%; the maximum pass deformation degree is generally less than or equal to 25%, the first pass deformation degree is generally less than or equal to 15%, the intermediate pass deformation degree is generally less than or equal to 20%, and the final 1 st to 2 nd pass deformation degree is as small as possible and is generally less than or equal to 10%.
Based on the principle, the corrosion-resistant Ni for high-quality hard glass sealing 29 Co 17 Cr 2 Cu 3 The alloy strip production method comprises seven steps of vacuum induction furnace smelting, electroslag remelting, forging, hot rolling, cold rolling, annealing and 23-roller withdrawal and straightening, and specifically comprises the following steps:
smelting in a vacuum induction furnace: the raw materials are prepared according to the following steps: the method comprises the steps of electrolyzing nickel, cobalt, low-sulfur pure iron, carbon spectrum electrodes in high-purity graphite and crystalline silicon, and sequentially carrying out the following treatment on the raw materials to obtain premelted slag; charging, melting, refining, alloying and casting;
step two, electroslag remelting: and (3) carrying out surface finishing treatment on the electrode rod, wherein the removal amount of surface oxide skin is more than or equal to 95%, and carrying out preheating treatment on the electrode rod and premelting slag before electroslag remelting so as to avoid bringing in of moisture. Pretreating an electrode rod and premelting slag, remelting the electrode rod by using an argon protective atmosphere electroslag furnace, wherein the premelting slag is remelted by adopting a quaternary slag system and four-stage control; and cooling the fed-back end along with the furnace for 60min, and discharging the cooled end.
Step three, forging: the steel ingot charging temperature is less than or equal to 800 ℃, the temperature rising rate of a cold furnace is less than or equal to 200 ℃/h, when the temperature in the furnace is more than 800 ℃, the temperature rising rate is less than or equal to 300 ℃/h, the heat preservation temperature is 1160+/-30 ℃, the heat preservation time is 3-4 h, the forging opening temperature is more than or equal to 1120 ℃, and the final forging temperature is more than or equal to 880 ℃; the forging is light, heavy and light and quick, and the forging is frequently rotated, and the forging should be carefully operated when approaching the size. The surface is flat and the size is uniform. And when the temperature is lower than the final forging temperature requirement, returning to the furnace for heating.
Step four, hot rolling: the steel ingot charging temperature is less than or equal to 700 ℃, the temperature rising rate of a cold furnace is less than or equal to 100 ℃/h, when the temperature in the furnace is more than 700 ℃, the temperature rising rate is less than or equal to 300 ℃/h, the heat preservation temperature is 1150+/-30 ℃, the heat preservation time is 30-40 min, the initial rolling temperature is more than or equal to 1150 ℃, and the final rolling temperature is more than or equal to 900 ℃; and calculating the reduction of the hot rolling pass according to the rheological stress change trend in the JMPRO simulation software, and designing steady rolling to achieve the purpose of uniform plastic deformation.
Step five, cold rolling: the maximum total deformation degree of a single rolling process is less than or equal to 70 percent; the maximum pass deformation degree is less than or equal to 25%, the first pass deformation degree is less than or equal to 15%, the intermediate pass deformation degree is less than or equal to 20%, and the final 1 st to 2 nd pass deformation degree is less than or equal to 10%;
step six, annealing: and annealing the blank and the semi-finished product in the strip process by adopting a three-zone temperature-control pure hydrogen protective atmosphere continuous annealing furnace, and annealing the intermediate cold-rolled strip: 980 ℃ and annealing the semi-finished cold-rolled strip: 950 DEG C
Seventhly, 23 roller withdrawal and straightening: controlling the strip shape, correcting the strip shape of the finished strip by adopting a 23-roller straightening and withdrawal machine, wherein the deformation of the straightening and withdrawal machine is less than or equal to 0.2 percent.
Wherein, the first step specifically comprises the following steps:
step 101, charging: high-purity carbon and low-sulfur pure iron are sequentially filled in the middle position of the bottom of the crucible, and cobalt and chromium are electrolyzed; the middle and upper parts of the crucible are filled with nickel plates, and crystalline silicon, electrolytic manganese, electrolytic copper and Ni-Mg are filled into a feeder. All raw materials need to be cleaned and dried, and dust, dirt and the like which influence the cleanliness of the materials can be removed for use.
Step 102, melting: vacuum pumping is carried out in a furnace, when the vacuum degree is less than or equal to 20Pa, power transmission melting is carried out, low-power transmission is carried out with the power less than or equal to 200KW, and the temperature is gradually raised by slow heating; so as to ensure higher vacuum degree in the melting period and be beneficial to the full removal of gas and harmful impurities.
Step 103, refining: after the furnace burden is cleared, the power is transmitted to 300-480 KW for 5min, the power is adjusted to 200-300 KW after the temperature reaches 1625+ -25 ℃, and the temperature of molten steel is adjusted to 1600+ -15 ℃ to enter the refining period; refining time is 45-60 min;
step 104, alloying: charging argon gas of 2-4Kpa, adding Si and Mn, melting, tilting the crucible for at least 5 times, wherein the power is 400kW, stirring for 3 minutes by UDS, controlling the alloying temperature at 1530+/-15 ℃, and maintaining for 10-15 minutes; stirring, controlling the temperature, charging Ar gas at 1510+/-10 ℃ and 2-4kPa, adding Ni-Mg, and mechanically stirring in a shaking furnace or carrying out UDS electromagnetic stirring;
step 105, casting: controlling the power transmission, and tilting the crucible to perform casting after the temperature reaches the requirement of the casting superheat degree, wherein the power of charged casting is less than or equal to 100KW; after casting, standing for 10 min in vacuum state, and then breaking and hanging out the casting mould.
In a further embodiment, the quaternary slag system in the second step is: caF (CaF) 2 、Al 2 O 3 、CaO、MgO；
The four-stage control is represented by: the arcing slag melting current is 2000-5000A, and the voltage is 38-51V; current 6500-7500A and voltage 45-52V in current lifting stage; the current in the remelting stage is 6500-7000A, and the voltage is 46-52V; the current in the feeding stage is 6500-4000A, and the voltage is 46-43V.
In conclusion, the corrosion-resistant Ni for high-quality hard glass sealing 29 Co 17 Cr 2 Cu 3 The alloy strip mainly comprises the following steps: smelting in a vacuum induction furnace, grinding an electrode rod, remelting protective electroslag, forging, flaw detection, forging blank finishing, hot rolling, water grinding, cold rolling, hydrogen annealing, edge shearing, grinding, cold rolling, cleaning, hydrogen annealing, finished product withdrawal and straightening, shearing and finished product.
By using a solidExample A corrosion resistant Ni for sealing high quality hard glass 29 Co 17 Cr 2 Cu 3 Four groups of materials are prepared by the production method of the alloy strip, test pieces are obtained, and the test pieces have the following numbers: b1, B2, B3, B4;
the characteristic detection is carried out on the four groups of test pieces and the four groups of control test pieces, and specific detection items comprise: gas content, nonmetallic inclusion, austenite grain grade of cold-rolled strip, mechanical property and microstructure.
(1) Gas content detection
The gas content testing method comprises the following steps: respectively taking Ni smelted by different furnace numbers 29 Co 17 Cr 2 Cu 3 And (3) detecting the oxygen and nitrogen contents in the molten alloy steel.
Specific test data are shown in table 1:
TABLE 1Ni 29 Co 17 Cr 2 Cu 3 Gas content in alloy
Corrosion-resistant Ni for high-quality hard glass sealing prepared by adopting example 29 Co 17 Cr 2 Cu 3 The average value of the oxygen content obtained by the alloy strip technology is 13.275ppm, the average value of the nitrogen content is 14.5ppm, and the average value of the oxygen content in the comparative example is 17.4ppm, and the average value of the nitrogen content is 16.75ppm. Oxide inclusions in the alloy strip are reduced after the oxygen content is reduced, the nitrogen content is reduced, massive nitride inclusions are reduced, and after the cold-rolled strip is sealed, the electrochemical corrosion performance is greatly improved, so that the corrosion resistance of the sealing material is improved, and the technical advantage is obvious.
(2) Nonmetallic inclusion detection
The nonmetallic inclusion test method comprises the following steps: respectively taking Ni smelted by different furnace numbers 29 Co 17 Cr 2 Cu 3 Alloy samples were examined for nonmetallic inclusions A, B, C, D and DS in molten steel. Specific test data are shown in table 2:
TABLE 2Ni 29 Co 17 Cr 2 Cu 3 Nonmetallic inclusion in alloysDetection data of object
(3) Austenitic grain grade detection for cold-rolled strip
Testing annealed Ni 29 Co 17 Cr 2 Cu 3 The austenitic grain grade of the alloy cold-rolled material is detected, and the high-quality Ni obtained by the invention 29 Co 17 Cr 2 Cu 3 Austenite structure grains of the alloy cold rolled material are uniform: the austenite grain is more than or equal to 7.5 grade, the extremely poor austenite grain of the cross section is less than or equal to 1.0 grade, and specific detection data are shown in table 3.
Table 3 Ni 29 Co 17 Cr 2 Cu 3 Detection data of austenite grains of alloy annealed cold rolled material
| Category(s) | Test piece number | Furnace number | Steel grade | Specification of specification | Austenite grain size |
| Comparative 1 | A1 | K220267 | Ni 29 Co 17 | 0.15*210 | 7.0 |
| Comparative example 2 | A2 | K220295 | Ni 29 Co 17 | 0.15*210 | 7.5 |
| Comparative example 3 | A3 | K220301 | Ni 29 Co 17 | 0.30*210 | 7.0 |
| Comparative example 4 | A4 | K220455 | Ni 29 Co 17 | 0.11*210 | 7.0 |
| Example 1 | B1 | K230108 | Ni 29 Co 17 Cr 2 Cu 3 | 0.15*210 | 7.5 |
| Example 2 | B2 | K230196 | Ni 29 Co 17 Cr 2 Cu 3 | 0.15*210 | 8.0 |
| EXAMPLE 3 | B3 | K230288 | Ni 29 Co 17 Cr 2 Cu 3 | 0.30*210 | 8.0 |
| EXAMPLE 4 | B4 | K230289 | Ni 29 Co 17 Cr 2 Cu 3 | 0.11*210 | 7.5 |
(4) Mechanical property detection
For Ni 29 Co 17 Cr 2 Cu 3 The mechanical properties of the alloy are tested, and the detection shows that the high-quality Ni obtained by the invention 29 Co 17 Cr 2 Cu 3 The elongation A after fracture of the alloy is more than or equal to 8.57%, the tensile strength Rm is more than or equal to 610MPa (average Rm= 623.84 MPa), the average hardness is 195.18HV, and specific detection data are shown in Table 4.
TABLE 4 high quality Ni 29 Co 17 Cr 2 Cu 3 Mechanical properties of alloy strips
(5) Thermal expansion Property
For Ni 29 Co 17 Cr 2 Cu 3 The alloy was tested for thermal expansion properties, the test results are shown in Table 5, and the high-quality Ni obtained by the present invention was found by the test 29 Co 17 Cr 2 Cu 3 The thermal expansion stability of the alloy is better.
TABLE 5 high quality Ni 29 Co 17 Cr 2 Cu 3 Thermal expansion properties of alloy strips
(6) Microscopic tissue detection
For the high-quality Ni prepared by the invention 29 Co 17 Cr 2 Cu 3 The microstructure of the annealed alloy strip is observed, and the result is shown in figure 1, and the high-quality Ni obtained by the invention 29 Co 17 Cr 2 Cu 3 Alloy strip austenite structure, carbide is uniformly dispersed and distributed in austenite grain boundary, and toughness is optimally combined, so that Ni 29 Co 17 Cr 2 Cu 3 The corrosion resistance of the alloy strip is greatly improved. Therefore, the high-quality Ni prepared by the invention 29 Co 17 Cr 2 Cu 3 The alloy strip has obvious effect of improving the material structure performance and corrosion resistance, and the corrosion weight gain is 3 to 4.5 x 10 from the previous weather atmosphere exposure test for 180 days at high temperature, high humidity and high salt fog -4 g/mm 2 Reduced to less than or equal to 2.5 x 10 -4 g/mm 2 The corrosion resistance can completely meet the use requirement in island environments.
It should be understood that the above-described specific embodiments are only for explaining the present invention and are not intended to limit the present invention. Obvious variations or modifications which extend from the spirit of the present invention are within the scope of the present invention.
Claims (8)
1. Corrosion-resistant Ni for hard glass sealing 29 Co 17 Cr 2 Cu 3 The alloy strip is characterized by comprising the following components in percentage by weight: less than or equal to 0.05 percent of C, 0.01 to 0.20 percent of Si, 0.10 to 0.50 percent of Mn, 28.5 to 29.5 percent of Ni, 15 to 18 percent of Co, 2.0 to 3.0 percent of Cu, 1.0 to 2.0 percent of Cr, less than or equal to 0.20 percent of Mo, less than or equal to 0.015 percent of P, less than or equal to 0.008 percent of S, less than or equal to 0.0020 percent of O, less than or equal to 0.0030 percent of N, less than or equal to 0.0005 percent of H, and the balance of Fe.
2. The corrosion resistant Ni for sealing a hard glass according to claim 1 29 Co 17 Cr 2 Cu 3 The alloy strip is characterized by comprising the following components in percentage by weight:
less than or equal to 0.03 percent of C, 0.05 to 0.15 percent of Si, 0.20 to 0.35 percent of Mn, 28.5 to 29.0 percent of Ni, 15.5 to 17.5 percent of Co, 2.5 to 3.0 percent of Cu, 1.5 to 2.0 percent of Cr, less than or equal to 0.15 percent of Mo, less than or equal to 0.010 percent of P, less than or equal to 0.005 percent of S, less than or equal to 0.0015 percent of O, less than or equal to 0.0025 percent of N, less than or equal to 0.0003 percent of H, and the balance of Fe.
3. The corrosion resistant Ni for sealing a hard glass according to claim 1 29 Co 17 Cr 2 Cu 3 Alloy strip, characterized in that the Ni 29 Co 17 Cr 2 Cu 3 The pitting corrosion resistance equivalent PREN of the alloy strip is more than or equal to 1.5;
wherein pren=cr (%) +3×mo (%) +30×n (%).
4. The corrosion resistant Ni for sealing a hard glass according to claim 1 29 Co 17 Cr 2 Cu 3 Alloy strip, characterized in that the Ni 29 Co 17 Cr 2 Cu 3 The reheat crack sensitivity coefficient of the alloy strip is less than or equal to 3.0;
wherein psr=cr (%) +cu (%) +2mo (%) +10v (%) +7nb (%) +5ti (%) -2.
5. A hard glass according to claim 1Corrosion-resistant Ni for sealing 29 Co 17 Cr 2 Cu 3 Alloy strip, characterized in that the Ni 29 Co 17 Cr 2 Cu 3 The cold crack sensitivity coefficient PCM of the alloy strip is less than or equal to 0.95; wherein,
PCM＝C(％)+Si(％)/30+[Mn(％)+Cr(％)+Cu]/20+Ni(％)/60+Mo(％)/15+V(％)/10+5B(％)。
6. preparation of corrosion-resistant Ni for sealing hard glass according to any one of claims 1 to 5 29 Co 17 Cr 2 Cu 3 The preparation method of the alloy strip is characterized by comprising the following steps:
smelting in a vacuum induction furnace: the raw materials are prepared according to the following steps: the method comprises the steps of electrolyzing nickel, cobalt, low-sulfur pure iron, carbon spectrum electrodes in high-purity graphite and crystalline silicon, and sequentially carrying out the following treatment on the raw materials to obtain premelted slag; charging, melting, refining, alloying and casting;
step two, electroslag remelting: pretreating an electrode rod and premelting slag, remelting the electrode rod by using an argon protective atmosphere electroslag furnace, wherein the premelting slag is remelted by adopting a quaternary slag system and four-stage control;
step three, forging: the steel ingot charging temperature is less than or equal to 800 ℃, the temperature rising rate of a cold furnace is less than or equal to 200 ℃/h, when the temperature in the furnace is more than 800 ℃, the temperature rising rate is less than or equal to 300 ℃/h, the heat preservation temperature is 1160+/-30 ℃, the heat preservation time is 3-4 h, the forging opening temperature is more than or equal to 1120 ℃, and the final forging temperature is more than or equal to 880 ℃;
step four, hot rolling: the steel ingot charging temperature is less than or equal to 700 ℃, the temperature rising rate of a cold furnace is less than or equal to 100 ℃/h, when the temperature in the furnace is more than 700 ℃, the temperature rising rate is less than or equal to 300 ℃/h, the heat preservation temperature is 1150+/-30 ℃, the heat preservation time is 30-40 min, the initial rolling temperature is more than or equal to 1150 ℃, and the final rolling temperature is more than or equal to 900 ℃;
step five, cold rolling: the maximum total deformation degree of a single rolling process is less than or equal to 70 percent; the maximum pass deformation degree is less than or equal to 25%, the first pass deformation degree is less than or equal to 15%, the intermediate pass deformation degree is less than or equal to 20%, and the final 1 st to 2 nd pass deformation degree is less than or equal to 10%;
step six, annealing: and annealing the blank and the semi-finished product in the strip process by adopting a three-zone temperature-control pure hydrogen protective atmosphere continuous annealing furnace, and annealing the intermediate cold-rolled strip: 980 ℃ and annealing the semi-finished cold-rolled strip: 950 DEG C
Seventhly, 23 roller withdrawal and straightening: controlling the strip shape, correcting the strip shape of the finished strip by adopting a 23-roller straightening and withdrawal machine, wherein the deformation of the straightening and withdrawal machine is less than or equal to 0.2 percent.
7. The corrosion resistant Ni for sealing hard glass according to claim 5 29 Co 17 Cr 2 Cu 3 The preparation method of the alloy strip is characterized by comprising the following steps:
step 101, charging: high-purity carbon and low-sulfur pure iron are sequentially filled in the middle position of the bottom of the crucible, and cobalt and chromium are electrolyzed; the middle and upper parts of the crucible are filled with nickel plates, and crystalline silicon, electrolytic manganese, electrolytic copper and Ni-Mg are filled into a feeder.
Step 102, melting: vacuum pumping is carried out in a furnace, when the vacuum degree is less than or equal to 20Pa, power transmission melting is carried out, low-power transmission is carried out with the power less than or equal to 200KW, and the temperature is gradually raised by slow heating;
step 103, refining: after the furnace burden is cleared, the power is transmitted to 300-480 KW for 5min, the power is adjusted to 200-300 KW after the temperature reaches 1625+ -25 ℃, and the temperature of molten steel is adjusted to 1600+ -15 ℃ to enter the refining period; refining time is 45-60 min;
step 104, alloying: charging argon gas of 2-4Kpa, adding Si and Mn, melting, tilting the crucible for at least 5 times, wherein the power is 400kW, stirring for 3 minutes by UDS, controlling the alloying temperature at 1530+/-15 ℃, and maintaining for 10-15 minutes; stirring, controlling the temperature, charging Ar gas at 1510+/-10 ℃ and 2-4kPa, adding Ni-Mg, and mechanically stirring in a shaking furnace or carrying out UDS electromagnetic stirring;
step 105, casting: controlling the power transmission, and tilting the crucible to perform casting after the temperature reaches the requirement of the casting superheat degree, wherein the power of charged casting is less than or equal to 100KW; after casting, standing for 10 min in vacuum state, and then breaking and hanging out the casting mould.
8. The corrosion resistant Ni for sealing hard glass according to claim 5 29 Co 17 Cr 2 Cu 3 Method for producing alloy stripThe method is characterized in that the quaternary slag system in the second step is as follows: caF (CaF) 2 、Al 2 O 3 、CaO、MgO；
The four-stage control is represented by: the arcing slag melting current is 2000-5000A, and the voltage is 38-51V; current 6500-7500A and voltage 45-52V in current lifting stage; the current in the remelting stage is 6500-7000A, and the voltage is 46-52V; the current in the feeding stage is 6500-4000A, and the voltage is 52-43V.
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