CN117512402A - Iron-nickel electrothermal alloy and preparation method thereof - Google Patents
Iron-nickel electrothermal alloy and preparation method thereof Download PDFInfo
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- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 106
- 239000000956 alloy Substances 0.000 title claims abstract description 106
- UGKDIUIOSMUOAW-UHFFFAOYSA-N iron nickel Chemical compound [Fe].[Ni] UGKDIUIOSMUOAW-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title abstract description 11
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 31
- 229910001030 Iron–nickel alloy Inorganic materials 0.000 claims abstract description 13
- 239000000126 substance Substances 0.000 claims abstract description 13
- 229910052727 yttrium Inorganic materials 0.000 claims abstract description 8
- 229910052735 hafnium Inorganic materials 0.000 claims abstract description 7
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 6
- 238000000137 annealing Methods 0.000 claims description 28
- 238000010438 heat treatment Methods 0.000 claims description 25
- 238000000034 method Methods 0.000 claims description 23
- 238000005096 rolling process Methods 0.000 claims description 23
- 238000007670 refining Methods 0.000 claims description 21
- 238000005266 casting Methods 0.000 claims description 19
- 229910000831 Steel Inorganic materials 0.000 claims description 18
- 239000010959 steel Substances 0.000 claims description 18
- 239000002893 slag Substances 0.000 claims description 16
- 229910021419 crystalline silicon Inorganic materials 0.000 claims description 12
- 238000002844 melting Methods 0.000 claims description 12
- 230000008018 melting Effects 0.000 claims description 12
- 229910004261 CaF 2 Inorganic materials 0.000 claims description 10
- 238000003723 Smelting Methods 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 10
- 238000000746 purification Methods 0.000 claims description 4
- 238000004381 surface treatment Methods 0.000 claims description 4
- 238000010309 melting process Methods 0.000 claims description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 21
- 230000003647 oxidation Effects 0.000 abstract description 12
- 238000007254 oxidation reaction Methods 0.000 abstract description 12
- 238000012937 correction Methods 0.000 abstract description 4
- 238000002474 experimental method Methods 0.000 abstract description 4
- 230000002035 prolonged effect Effects 0.000 abstract description 2
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- 230000008092 positive effect Effects 0.000 description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 12
- 239000000463 material Substances 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 9
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 8
- 238000002791 soaking Methods 0.000 description 8
- 229910052759 nickel Inorganic materials 0.000 description 7
- 229910052761 rare earth metal Inorganic materials 0.000 description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 229910052799 carbon Inorganic materials 0.000 description 6
- 239000002245 particle Substances 0.000 description 6
- 238000005406 washing Methods 0.000 description 6
- 229910000863 Ferronickel Inorganic materials 0.000 description 5
- 230000009286 beneficial effect Effects 0.000 description 4
- 238000007599 discharging Methods 0.000 description 4
- 229910052742 iron Inorganic materials 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 229910000851 Alloy steel Inorganic materials 0.000 description 3
- 229910018487 Ni—Cr Inorganic materials 0.000 description 3
- 230000009471 action Effects 0.000 description 3
- VNNRSPGTAMTISX-UHFFFAOYSA-N chromium nickel Chemical compound [Cr].[Ni] VNNRSPGTAMTISX-UHFFFAOYSA-N 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- 229910052681 coesite Inorganic materials 0.000 description 3
- 229910052906 cristobalite Inorganic materials 0.000 description 3
- 230000006698 induction Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- 235000012239 silicon dioxide Nutrition 0.000 description 3
- 229910052682 stishovite Inorganic materials 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 229910052905 tridymite Inorganic materials 0.000 description 3
- 229910000640 Fe alloy Inorganic materials 0.000 description 2
- 229910001566 austenite Inorganic materials 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000011010 flushing procedure Methods 0.000 description 2
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 description 2
- MTRJKZUDDJZTLA-UHFFFAOYSA-N iron yttrium Chemical compound [Fe].[Y] MTRJKZUDDJZTLA-UHFFFAOYSA-N 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 150000002910 rare earth metals Chemical class 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 238000010079 rubber tapping Methods 0.000 description 2
- 229910003271 Ni-Fe Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000003064 anti-oxidating effect Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
- 235000000396 iron Nutrition 0.000 description 1
- 229910000734 martensite Inorganic materials 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 238000005121 nitriding Methods 0.000 description 1
- 238000013021 overheating Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- -1 rare earth compounds Chemical class 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 235000014347 soups Nutrition 0.000 description 1
- 238000005482 strain hardening Methods 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 238000010301 surface-oxidation reaction Methods 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 230000004584 weight gain Effects 0.000 description 1
- 235000019786 weight gain Nutrition 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C19/00—Alloys based on nickel or cobalt
- C22C19/03—Alloys based on nickel or cobalt based on nickel
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21C—MANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
- B21C37/00—Manufacture of metal sheets, bars, wire, tubes or like semi-manufactured products, not otherwise provided for; Manufacture of tubes of special shape
- B21C37/04—Manufacture of metal sheets, bars, wire, tubes or like semi-manufactured products, not otherwise provided for; Manufacture of tubes of special shape of bars or wire
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D18/00—Pressure casting; Vacuum casting
- B22D18/06—Vacuum casting, i.e. making use of vacuum to fill the mould
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
- C21D9/52—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for wires; for strips ; for rods of unlimited length
- C21D9/525—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for wires; for strips ; for rods of unlimited length for wire, for rods
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B23/00—Obtaining nickel or cobalt
- C22B23/06—Refining
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
- C22B9/16—Remelting metals
- C22B9/18—Electroslag remelting
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/023—Alloys based on nickel
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/02—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working in inert or controlled atmosphere or vacuum
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/10—Changing 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention provides an iron-nickel electrothermal alloy and a preparation method thereof, belonging to the field of alloy preparation. The iron-nickel electrothermal alloy comprises the following chemical components: C. si, S, P, ni, Y and Hf, the balance being Fe; the weight percentage of the alloy is 0.01 to 0.03 percent, the weight percentage of Si is 0.1 to 0.5 percent, the weight percentage of S is less than or equal to 0.003 percent, the weight percentage of P is less than or equal to 0.020 percent, the weight percentage of Ni is 51 to 53 percent, the weight percentage of Y is 0.04 to 0.2 percent, and the weight percentage of Hf is 0.02 to 0.07 percent. By adding Y, hf element, the high-temperature oxidation resistance of the nickel-iron alloy is improved, the service life of the nickel-iron alloy in a medium-temperature environment is prolonged, the quick service life reaches more than 100 hours in a 900 ℃ quick service life experiment, the resistivity of the nickel-iron alloy wire at 20 ℃ is 0.30uΩ & m to 0.37uΩ & m, and the resistance correction coefficient meets the PTC performance requirement.
Description
Technical Field
The application relates to the technical field of alloy preparation, in particular to an iron-nickel electrothermal alloy and a preparation method thereof.
Background
The Fe-Ni thermistor alloy has medium resistivity, large and positive resistance temperature coefficient, the resistance value and the temperature are in linear relation, and the stability of the resistance is good. The electric heating device is mainly used for elevators, water pumps, continuously-operated electrical equipment, ovens and the like to prevent overheat and overtemperature, and can also be used for household appliances such as electric blankets, electric irons, electric cookers and the like.
At present, the service temperature of the iron-nickel thermistor alloy wire is mostly 0-150 ℃, the iron-nickel thermistor alloy wire can be only used for low-temperature control, the heating temperature requirement is difficult to meet, and in order to simultaneously utilize the automatic constant temperature and the heating performance of materials, it is necessary to develop an iron-nickel alloy with longer service life in a medium-temperature environment.
Disclosure of Invention
The application provides an iron-nickel electrothermal alloy and a preparation method thereof, which solve the technical problem that the service life of the existing iron-nickel electrothermal alloy in a medium temperature environment is shorter by improving the oxidation resistance of the iron-nickel electrothermal alloy.
In a first aspect, the present application provides an iron-nickel electrothermal alloy comprising the chemical components: C. si, S, P, ni, Y and Hf, the balance being Fe; in terms of mass fraction, the total mass fraction,
the content of C is 0.01 to 0.03 percent, the content of Si is 0.1 to 0.5 percent, the content of S is less than or equal to 0.003 percent, the content of P is less than or equal to 0.020 percent, the content of Ni is 51 to 53 percent, the content of Y is 0.04 to 0.2 percent, and the content of Hf is 0.02 to 0.07 percent.
Optionally, the iron-nickel electrothermal alloy comprises the following chemical components in percentage by mass: 0.02% of C, 0.28% of Si, 0.001% of S, 0.007% of P, 52.1% of Ni, 0.2% of Y, 0.02% of Hf and the balance of Fe.
Optionally, the iron-nickel electrothermal alloy satisfies at least one of the following properties: the resistivity at 20 ℃ is 0.31uΩ.m-0.37 uΩ.m, the quick life value at 900 ℃ is >100h, and the class D of the inclusion is 0.5 class.
In a second aspect, the present application provides a method for preparing an iron-nickel electrothermal alloy, which is characterized in that the method is used for preparing the iron-nickel electrothermal alloy according to any one of the embodiments of the first aspect, and the method includes:
vacuum smelting to obtain an alloy rod containing the chemical components;
purifying the alloy rod to obtain an alloy ingot;
heating and rolling the alloy ingot to obtain an alloy wire rod;
performing first annealing, cooling, surface treatment and drawing on the alloy wire rod to obtain a drawn cold state finished product;
and (3) carrying out second annealing on the drawn cold finished product to obtain the Fe-Ni electrothermal alloy.
Optionally, the vacuum smelting process specifically includes: adding a Ni source, a Fe source and a C source into a crucible of a vacuum melting furnace, adding crystalline silicon, a Y source and a Hf source through a vacuum charging bin after the crystalline silicon, the Y source and the Hf source are completely melted, refining after charging, and carrying out electrified vacuum casting.
Optionally, the refining temperature is 1550-1650 ℃, and the charged vacuum casting temperature is 1500-1550 ℃.
Optionally, the purification mode comprises electroslag remelting and vacuum consumable, and the purified slag comprises Y 2 O 3 CaO and CaF 2 The mass ratio of the purified slag satisfies Y 2 O 3 :CaO:CaF 2 (10-20): (3-5): (70-80), wherein the use amount of the purified slag is 3 Kg/t.steel-5 Kg/t.steel.
Optionally, the heating temperature is 1120-1180 ℃, the heating time is 90-400 min, and the initial rolling temperature of the rolling is 1120-1180 ℃.
Optionally, the temperature of the first annealing is 950-1050 ℃, and the time of the first annealing is 120-240 min.
Optionally, the temperature of the second annealing is 1000 ℃ to 1150 ℃.
Compared with the prior art, the technical scheme provided by the embodiment of the application has the following advantages:
according to the method, the Y, hf element is added, so that the high-temperature oxidation resistance of the nickel-iron alloy is improved, the service life of the nickel-iron alloy in a medium-temperature environment is prolonged, the rapid service life reaches more than 100h in a rapid service life experiment at 900 ℃, the resistivity of the nickel-iron alloy wire at 20 ℃ is 0.30uΩ & m-0.37 uΩ & m, and the resistance correction coefficient meets the PTC performance requirement.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments consistent with the application and together with the description, serve to explain the principles of the application.
In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings that are required to be used in the description of the embodiments or the prior art will be briefly described below, and it will be obvious to those skilled in the art that other drawings can be obtained from these drawings without inventive effort.
Fig. 1 is a schematic flow chart of a method for preparing an iron-nickel electrothermal alloy according to an embodiment of the present application;
fig. 2 is a graph showing the oxidation weight gain at 600 ℃ of the ferronickel electrothermal alloy obtained in example 1 and comparative examples 1 and 2 of the present application.
Detailed Description
For the purposes of making the objects, technical solutions and advantages of the embodiments of the present application more clear, the technical solutions of the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application, and it is apparent that the described embodiments are some embodiments of the present application, but not all embodiments. All other embodiments, which can be made by one of ordinary skill in the art without undue burden from the present disclosure, are within the scope of the present application based on the embodiments herein.
Various embodiments of the present application may exist in a range format; it should be understood that the description in a range format is merely for convenience and brevity and should not be interpreted as a rigid limitation on the scope of the application. It is therefore to be understood that the range description has specifically disclosed all possible sub-ranges and individual values within that range. For example, it should be considered that a description of a range from 1 to 6 has specifically disclosed sub-ranges, such as from 1 to 3, from 1 to 4, from 1 to 5, from 2 to 4, from 2 to 6, from 3 to 6, etc., as well as single numbers within the range, such as 1, 2, 3, 4, 5, and 6, wherever applicable. In addition, whenever a numerical range is referred to herein, it is meant to include any reference number (fractional or integer) within the indicated range.
In addition, in the description of the present application, the terms "include", "comprise", "comprising" and the like mean "including but not limited to". Relational terms such as "first" and "second", and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Herein, "and/or" describing an association relationship of an association object means that there may be three relationships, for example, a and/or B, may mean: a alone, a and B together, and B alone. Wherein A, B may be singular or plural. Herein, "at least one" means one or more, and "a plurality" means two or more. "at least one", "at least one" or the like refer to any combination of these items, including any combination of single item(s) or plural items(s). For example, "at least one (individual) of a, b, or c," or "at least one (individual) of a, b, and c," may each represent: a, b, c, a-b (i.e., a and b), a-c, b-c, or a-b-c, wherein a, b, c may be single or multiple, respectively.
Unless specifically indicated otherwise, the various raw materials, reagents, instruments, equipment, and the like used in this application are commercially available or may be prepared by existing methods.
In a first aspect, the present application provides an iron-nickel electrothermal alloy comprising the chemical components: C. si, S, P, ni, Y and Hf, the balance being Fe; in terms of mass fraction, the total mass fraction,
the content of C is 0.01 to 0.03 percent, the content of Si is 0.1 to 0.5 percent, the content of S is less than or equal to 0.003 percent, the content of P is less than or equal to 0.020 percent, the content of Ni is 51 to 53 percent, the content of Y is 0.04 to 0.2 percent, and the content of Hf is 0.02 to 0.07 percent.
The positive effect of controlling the content of Si to be 0.1-0.5 percent: si can react with air to generate SiO2, the SiO2 is positioned between the alloy matrix and the oxide film, and can also play a role in isolating oxygen, so that the SiO2 is an important ring in an anti-oxidation mechanism, and can reduce the oxidation rate of the alloy, thereby prolonging the service time. Meanwhile, the resistivity of Si can be improved, and the stability of the content of Si is maintained, so that the stability of the alloy resistance is facilitated. However, when the Si content is too high, segregation tends to occur during use, which affects the structural stability of the material, affects the creep properties, and combines oxidation resistance, resistivity and high temperature structural stability. The Si content may be 0.1%, 0.2%, 0.3%, 0.4%, 0.5%, etc.
The positive effects of controlling the content of C to be 0.01-0.03%, the content of S to be less than or equal to 0.003% and the content of P to be less than or equal to 0.020%) are that: C. the S, P element is harmful to the high-temperature oxidation resistance of the material, and adopts low-limit control. The content of C may be 0.01%, 0.02%, 0.03%, etc., the content of S may be 0.001%, 0.002%, 0.003%, etc., and the content of P may be 0.005%, 0.010%, 0.015%, 0.020%, etc.
The positive effect of controlling the Ni content to be 51% -53%: the Ni element has the effect of expanding austenite in the alloy, so that the increase of the Ni content in the alloy can stabilize the austenite, the transformation temperature of the martensite can be reduced to be lower than the room temperature, the high-temperature strength of the material can be ensured, and meanwhile, the stability of the temperature correction coefficient of the resistance of the material can be ensured by controlling the proportion of nickel and iron. The Ni content may be 51%, 51.5%, 52%, 52.5%, 53%, etc.
The positive effect of controlling the content of Hf to be 0.01% -0.2%: hf can inhibit nitriding precipitation at high temperature, and Y and Hf are matched to generate stable nano composite phase, so that the grain boundary strengthening effect is achieved, and the material use temperature is improved. Specifically, the content of Hf may be 0.01%, 0.05%, 0.10%, 0.15%, 0.20%, etc.
The positive effect of controlling the content of Y to be 0.04% -0.20%: the rare earth element Y can form rare earth compounds with N, O, S and other elements in the alloy, so that the content of inclusions is effectively reduced, and the inclusions are uniformly dispersed in the alloy. Meanwhile, the rare earth elements are added, so that the growth of alloy grains can be inhibited, the grains tend to be refined, the occurrence of cracks is reduced, and the plasticity and the strength of the alloy at high temperature and room temperature are improved. The rare earth is also beneficial to improving the adhesiveness of the oxide film and improving the compactness of the oxide film, thereby improving the high-temperature oxidation resistance of the alloy. The rare earth element content may be 0.04%, 0.08%, 0.12%, 0.16%, 0.18%, 0.20%, etc.
In some embodiments, the iron-nickel electrothermal alloy comprises the following chemical components in percentage by mass: 0.02% of C, 0.28% of Si, 0.001% of S, 0.007% of P, 52.1% of Ni, 0.2% of Y, 0.02% of Hf and the balance of Fe.
In some embodiments, the iron-nickel electrothermal alloy satisfies at least one of the following properties: the resistivity at 20 ℃ is 0.31uΩ.m-0.37 uΩ.m, the quick life value at 900 ℃ is >100h, and the class D of the inclusion is 0.5 class.
The Fe-Ni electrothermal alloy obtained by the application has longer service life in a medium-temperature environment, lower inclusion content, stable resistivity of the Ni-Fe alloy wire and resistance correction coefficient meeting PTC performance requirements. The resistivity at 20℃may be 0.31uΩ·m, 0.33uΩ·m, 0.35uΩ·m, 0.37uΩ·m, etc., and the rapid lifetime values at 900℃may be 101h, 105h, 110h, 115h, 120h, etc.
In a second aspect, the present application provides a method for preparing an iron-nickel electrothermal alloy, which is characterized in that the method is used for preparing an iron-nickel electrothermal alloy according to any one of the embodiments of the first aspect, referring to fig. 1, and the method includes:
s1, carrying out vacuum melting to obtain an alloy rod containing the chemical components;
in some embodiments, the vacuum melting process is specifically: adding a Ni source, a Fe source and a C source into a crucible of a vacuum melting furnace, adding crystalline silicon, a Y source and a Hf source through a vacuum charging bin after the crystalline silicon, the Y source and the Hf source are completely melted, refining after charging, and carrying out electrified vacuum casting. Cooling along with the furnace after casting, discharging from the furnace after breaking vacuum, and demoulding to form an alloy rod.
In some embodiments, the temperature of the refining is 1550 ℃ to 1650 ℃ and the temperature of the charged vacuum casting is 1500 ℃ to 1550 ℃.
The refining temperature may be 1550 ℃, 1570 ℃, 1590 ℃, 1610 ℃, 1630 ℃, 1650 ℃ and the like.
The positive effect of controlling the temperature of the charged vacuum casting of molten steel to 1500-1550℃ is that: and the alloy burning loss is reduced while the smooth casting is ensured. If the tapping temperature is too high, the oxidation burning loss of alloy elements can be accelerated to a certain extent; if the tapping temperature is too low, molten steel is solidified in the pouring process to a certain extent, a soup channel is blocked, and the quality of the steel bar is affected. The temperature of the charged vacuum casting of the molten steel may be 1500 ℃, 1510 ℃, 1520 ℃, 1530 ℃, 1540 ℃, 1550 ℃ and the like.
S2, purifying the alloy rod to obtain an alloy ingot;
in some embodiments, the means of purification includes electroslag remelting and vacuum consumable, and the purified slag includes Y 2 O 3 CaO and CaF 2 The mass ratio of the purified slag satisfies Y 2 O 3 :CaO:CaF 2 (10-20): (3-5): (70-80), wherein the use amount of the purified slag is 3 Kg/t.steel-5 Kg/t.steel.
In the embodiment of the application, control Y 2 O 3 :CaO:CaF 2 Positive effects of = (10-20): (3-5): (70-80): in order to ensure the recovery rate of rare earth in the purified alloy, Y is added into the purified slag 2 O 3 . On the basis of ensuring that the resistance, melting point and adsorption inclusion capacity of the refining slag are not reduced, the burning loss of rare earth elements is reduced, and the recovery rate is improved. The Y is 2 O 3 CaO and CaF 2 The mass ratio of (c) may be 20:3:77, 15:5:80, 20:4:76, 20:5:75, 15:3:72, 15:4:71, 15:5:70, etc. The amount of the purified slag can be 3 Kg/t.steel, 3.5 Kg/t.steel, 4 Kg/t.steel, 4.5 Kg/t.steel and 5 Kg/t.steel.
S3, heating and rolling the alloy ingot to obtain an alloy wire rod;
in some embodiments, the heating temperature is 1120 ℃ to 1180 ℃, the heating time is 90min to 400min, and the initial rolling temperature of the rolling is 1120 ℃ to 1180 ℃.
The positive effect of controlling the heating temperature to 1120-1180℃: ensuring that the inner and outer parts of the steel ingot reach the initial rolling temperature. If the temperature is too high, the surface of the steel ingot is oxidized and the structure is seriously roughened to a certain extent, and the steel ingot is cracked in rolling after overheating; if the temperature is too low, the steel ingot can not reach the initial rolling temperature to a certain extent, the thermoplastic property of the material is poor, and cracking is caused in the deformation process. The heating temperature may be 1120 ℃, 1130 ℃, 1140 ℃, 1160 ℃, 1170 ℃, 1180 ℃, etc.
The positive effect of controlling the heating time to be 90-400 min is that: and the uniform heating of the inner part and the outer part of the steel ingot is ensured. The time is too long, so that the steel ingot tissue grows up to a certain extent, and the surface is oxidized; if the time is too short, the internal temperature of the ingot may not reach the set temperature to some extent, and the core may crack during rolling. The heating time can be 90min, 100min, 150min, 200min, 250min, 300min, 400min, etc.
The positive effect of controlling the initial rolling temperature to 1120-1180℃ is that: the temperature section has better thermoplasticity and is beneficial to thermal processing deformation. If the starting rolling temperature is too high, the surface oxidation and the serious coarsening of the structure of the alloy can be caused to a certain extent, and the rolling is cracked; if the start rolling temperature is too low, the alloy will have poor thermoplasticity to some extent, and will cause cracking during deformation. Specifically, the start rolling temperature may be 1120 ℃, 1140 ℃, 1160 ℃, 1180 ℃, or the like.
S4, performing first annealing, cooling, surface treatment and drawing on the alloy wire rod to obtain a drawn cold-state finished product;
in some embodiments, the temperature of the first anneal is 950 ℃ to 1050 ℃ and the time of the first anneal is 120min to 240min.
The positive effects of controlling the temperature of the first annealing to 950-1050 ℃ and the first annealing time to 120-240 min are that: the control temperature and time range is solid solution treatment, so that the tissue composition of the wire rod is uniform, and the work hardening is eliminated. If the annealing temperature is too high, the coil rod tissue is coarse and the surface is oxidized to a certain extent; if the annealing temperature is too low, the solution treatment cannot be performed to some extent. Specifically, the first annealing temperature may be 950 ℃, 970 ℃, 990 ℃, 1010 ℃, 1030 ℃, 1050 ℃, or the like. The first annealing time may be 120min, 150min, 180min, 210min, 240min, etc.
In some embodiments, the means for surface treatment comprises: laser cleaning, mechanical polishing, plasma method, wire rod peeling, acid cleaning and melting alkali cleaning.
In the embodiment of the present application, the manner of removing the surface oxide film: soaking the alloy wire rod in molten sodium hydroxide at 700 ℃ for 3-5 minutes, then flushing with water, then soaking in sulfuric acid with the concentration of more than 180g/L for 30-40 minutes, flushing with water to remove surface residues, and airing.
S5, carrying out second annealing on the drawn cold finished product to obtain the Fe-Ni electrothermal alloy.
In some embodiments, the temperature of the second anneal is 1000 ℃ to 1150 ℃.
The positive effect of controlling the temperature of the second annealing to be 1000-1150℃: the control within the temperature range is beneficial to eliminating processing stress and dislocation and improving the mechanical property of the finished product. If the annealing temperature is too high, the internal structure of the alloy is coarse to a certain extent; if the temperature of the annealing is too low, the strength of the material is too high to some extent, and the processability of the material is deteriorated. The annealing temperature may be 1000 ℃, 1050 ℃, 1100 ℃, 1150 ℃, etc.
The preparation process is beneficial to improving the purity of the material and reducing the inclusion.
The present application is further illustrated below in conjunction with specific examples. It should be understood that these examples are illustrative only of the present application and are not intended to limit the scope of the present application. The experimental procedures, which are not specified in the following examples, are generally determined according to national standards. If the corresponding national standard does not exist, the method is carried out according to the general international standard, the conventional condition or the condition recommended by the manufacturer.
Example 1
The iron-nickel electrothermal alloy comprises the following chemical components in percentage by mass: 0.02% of C, 0.28% of Si, 0.001% of S, 0.007% of P, 52.1% of Ni, 0.2% of Y, 0.02% of Hf and the balance of Fe.
The preparation method of the iron-nickel electrothermal alloy comprises the following steps:
s11, smelting alloy steel bars by using pure iron, electrolytic nickel, crystalline silicon, yttrium iron, metal hafnium and carbon particles as raw materials and adopting a vacuum induction furnace, adding nickel plates, pure iron and carbon particles into a crucible of the vacuum smelting furnace, and vacuumizing, wherein the vacuum degree in the furnace is not higher than 30Pa. And (3) electric melting is carried out, furnace burden is completely melted, crystalline silicon, yttrium iron and metal hafnium are added through a vacuum charging bin after a molten pool is leveled, refining is carried out after charging is finished, the refining temperature is 1600 ℃, and electrified vacuum casting is carried out after temperature adjustment is carried out after refining. Casting temperature is 1500 ℃; cooling along with the furnace after casting, discharging from the furnace after breaking vacuum, and demoulding to form an alloy rod.
S21, purifying the alloy rod serving as a consumable electrode by adopting a single-phase electroslag remelting furnace to obtain an alloy ingot. Refining slag and mass ratio of Y 2 O 3 :CaO:CaF 2 =15:5:80, 5Kg per furnace refining slag.
S31, heating the obtained alloy ingot in a heating furnace at 1180 ℃ for 400Min; and then rolling is carried out, the initial rolling temperature is 1150 ℃, and the alloy wire rod is obtained.
S41, annealing the alloy Jin Pantiao, carrying out heat preservation for 180min at a temperature of 1050 ℃, carrying out water cooling, removing a surface oxide film, soaking in molten sodium hydroxide at 700 ℃ for 5 min, then washing with water, soaking with sulfuric acid with the concentration of 180g/L for 40min, washing with water to remove surface residues, and airing. And finally, drawing the cleaned wire rod to obtain a drawn cold-state finished product.
S51, annealing the drawn cold finished product in an atmosphere protection continuous annealing furnace at 1100 ℃ to obtain a nickel-chromium electrothermal alloy finished product, which can be used for heating element production.
Comparative example 1
The iron-nickel electrothermal alloy comprises the following chemical components in percentage by mass: 0.02% of C, 0.28% of Si, 0.001% of S, 0.007% of P, 52.1% of Ni and the balance of Fe.
The preparation method of the iron-nickel electrothermal alloy comprises the following steps:
s11, smelting alloy steel bars by using pure iron, electrolytic nickel, crystalline silicon and carbon particles as raw materials and adopting a vacuum induction furnace, adding nickel plates, pure iron and carbon particles into a crucible of the vacuum smelting furnace, and vacuumizing, wherein the vacuum degree in the furnace is not higher than 30Pa. And (3) electric melting is carried out, furnace materials are all melted, crystalline silicon is added through a vacuum charging bin after a molten pool is leveled, refining is carried out after charging is finished, the refining temperature is 1600 ℃, and electrified vacuum casting is carried out after temperature adjustment is carried out after refining. The casting temperature is 1550 ℃; cooling along with the furnace after casting, discharging from the furnace after breaking vacuum, and demoulding to form an alloy rod.
S21, purifying the alloy rod serving as a consumable electrode by adopting a single-phase electroslag remelting furnace to obtain an alloy ingot. Refining slag and mass ratio of Y 2 O 3 :CaO:CaF 2 =15:5:80, 5Kg per furnace refining slag.
S31, heating the obtained alloy ingot in a heating furnace at 1180 ℃ for 400Min; and then rolling is carried out, the initial rolling temperature is 1150 ℃, and the alloy wire rod is obtained.
S41, annealing the alloy Jin Pantiao, carrying out heat preservation for 180min at a temperature of 1050 ℃, carrying out water cooling, removing a surface oxide film, soaking in molten sodium hydroxide at 700 ℃ for 5 min, then washing with water, soaking with sulfuric acid with the concentration of 180g/L for 40min, washing with water to remove surface residues, and airing. And finally, drawing the cleaned wire rod to obtain a drawn cold-state finished product.
S51, annealing the drawn cold finished product in an atmosphere protection continuous annealing furnace at 1100 ℃ to obtain a nickel-chromium electrothermal alloy finished product, which can be used for heating element production.
Comparative example 2
The iron-nickel electrothermal alloy comprises the following chemical components in percentage by mass: 0.02% of C, 0.28% of Si, 0.001% of S, 0.007% of P, 52.1% of Ni and the balance of Fe.
The preparation method of the iron-nickel electrothermal alloy comprises the following steps:
s11, smelting alloy steel bars by using pure iron, electrolytic nickel, crystalline silicon and carbon particles as raw materials and adopting a vacuum induction furnace, adding nickel plates, pure iron and carbon particles into a crucible of the vacuum smelting furnace, and vacuumizing, wherein the vacuum degree in the furnace is not higher than 30Pa. And (3) feeding electric melting, namely melting all the furnace burden, feeding electric melting, melting all the furnace burden, leveling a molten pool, adding crystalline silicon through a vacuum charging bin, refining after charging, wherein the refining temperature is 1600 ℃, and carrying out electrified vacuum casting after temperature adjustment after refining. Casting temperature 1520 ℃; cooling along with the furnace after casting, discharging from the furnace after breaking vacuum, and demoulding to form an alloy rod.
S21, after peeling and finishing the obtained alloy rod, heating the alloy rod in a heating furnace at 1160 ℃ for 400Min; and then rolling is carried out, the initial rolling temperature is 1150 ℃, and the alloy wire rod is obtained.
S31, annealing the alloy Jin Pantiao, preserving heat for 180min at a temperature of 1050 ℃, performing water cooling, removing a surface oxide film, soaking in molten sodium hydroxide at 700 ℃ for 5 min, then washing with water, soaking in sulfuric acid with a concentration of 180g/L for 40min, washing with water to remove surface residues, and airing. And finally, drawing the cleaned wire rod to obtain a drawn cold-state finished product.
S41, annealing the drawn cold finished product in an atmosphere protection continuous annealing furnace at 1100 ℃ to obtain a nickel-chromium electrothermal alloy finished product, which can be used for heating element production.
The nickel-iron alloys (bright state alloy wire having a gauge of 0.8 mm) prepared in the above examples and comparative examples were subjected to a rapid life test and inclusion grade detection, and the results are shown in table 1.
Table 1 results of the rapid life test and inclusion grade test of the nickel-iron alloys prepared in examples and comparative examples
| Group of | Fast life value (h) at 900 ℃ | Inclusion grade |
| Example 1 | 125 | Class D lineage 0.5 |
| Comparative example 1 | 63 | Class D lineage 0.7 |
| Comparative example 2 | 42 | Class D lineage 2.5 |
As can be obtained from Table 1, the quick life value of the ferronickel electrothermal alloy provided by the invention can reach 125 hours at 900 ℃. The Fe-Ni electrothermal alloy has longer service life in medium temperature environment and lower inclusion content.
Detailed description of fig. 2:
as shown in fig. 2, the results of the oxidation weight increase experiments performed on the ferronickel electrothermal alloy obtained in example 1 and comparative examples 1 and 2 at 600 ℃ show that the high-temperature oxidation resistance of the ferronickel electrothermal alloy obtained in example 1 is better due to the addition of Y, hf element during smelting. In comparative example 2, the alloy rod is not purified by adopting an electroslag remelting process, the inclusion content is high, and the obtained ferronickel electrothermal alloy has poor high-temperature oxidation resistance.
The foregoing is merely a specific embodiment of the application to enable one skilled in the art to understand or practice the application. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the application. Thus, the present application is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. The iron-nickel electrothermal alloy is characterized by comprising the following chemical components: C. si, S, P, ni, Y and Hf, the balance being Fe; in terms of mass fraction, the total mass fraction,
the content of C is 0.01 to 0.03 percent, the content of Si is 0.1 to 0.5 percent, the content of S is less than or equal to 0.003 percent, the content of P is less than or equal to 0.020 percent, the content of Ni is 51 to 53 percent, the content of Y is 0.04 to 0.2 percent, and the content of Hf is 0.02 to 0.07 percent.
2. The iron-nickel electrothermal alloy of claim 1, wherein the iron-nickel electrothermal alloy comprises the following chemical components in mass percent: 0.02% of C, 0.28% of Si, 0.001% of S, 0.007% of P, 52.1% of Ni, 0.2% of Y, 0.02% of Hf and the balance of Fe.
3. The iron-nickel electrothermal alloy of claim 1, wherein the iron-nickel electrothermal alloy meets at least one of the following properties: the resistivity at 20 ℃ is 0.31uΩ.m-0.37 uΩ.m, the quick life value at 900 ℃ is >100h, and the class D of the inclusion is 0.5 class.
4. A method for preparing an iron-nickel electrothermal alloy according to any one of claims 1-3, the method comprising:
vacuum smelting to obtain an alloy rod containing the chemical components;
purifying the alloy rod to obtain an alloy ingot;
heating and rolling the alloy ingot to obtain an alloy wire rod;
performing first annealing, cooling, surface treatment and drawing on the alloy wire rod to obtain a drawn cold state finished product;
and (3) carrying out second annealing on the drawn cold finished product to obtain the Fe-Ni electrothermal alloy.
5. The method according to claim 4, characterized in that the vacuum melting process is specifically: adding a Ni source, a Fe source and a C source into a crucible of a vacuum melting furnace, adding crystalline silicon, a Y source and a Hf source through a vacuum charging bin after the crystalline silicon, the Y source and the Hf source are completely melted, refining after charging, and carrying out electrified vacuum casting.
6. The method of claim 5, wherein the refining temperature is 1550 ℃ to 1650 ℃ and the charged vacuum casting temperature is 1500 ℃ to 1550 ℃.
7. The method of claim 4, wherein the purification comprises electroslag remelting and vacuum consumable, and wherein the purified purification slag comprises Y 2 O 3 CaO and CaF 2 The mass ratio of the purified slag satisfies Y 2 O 3 :CaO:CaF 2 (10-20): (3-5): (70-80), wherein the use amount of the purified slag is 3 Kg/t.steel-5 Kg/t.steel.
8. The method according to claim 4, wherein the heating temperature is 1120-1180 ℃, the heating time is 90-400 min, and the initial rolling temperature is 1120-1180 ℃.
9. The method of claim 4, wherein the temperature of the first anneal is 950 ℃ to 1050 ℃ and the time of the first anneal is 120min to 240min.
10. The method of claim 4, wherein the second anneal is at a temperature of 1000 ℃ to 1150 ℃.
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