Heating method for improving high-temperature oxidation resistance and crack resistance of 9Ni steel billet

By optimizing the heating process, controlling the heating atmosphere, heating rate and insulation temperature, the problems of burning and crystal cracks in the high-temperature heating process of 9Ni billets are solved, and the high-temperature oxidation resistance and crack resistance are improved, reducing production costs and environmental pollution.

CN119506768AActive Publication Date: 2025-02-25新余钢铁股份有限公司
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Patent Information

Application Number
CN202411693395.8
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-11-25
Publication Date
2025-02-25
Estimated Expiration
2044-11-25

AI Technical Summary

Technical Problem

9Ni steel billets are prone to severe burning and crystal cracks during high-temperature heating, resulting in a decrease in metal yield and cracking of the steel plate surface during subsequent rolling, affecting product quality and toughness. The prior art solves this problem by adding antioxidant elements or spraying antioxidant coatings, but there are problems of high production costs and environmental pollution.

Method used

By optimizing the heating process, controlling the heating atmosphere, heating rate and insulation temperature, the rapid generation of dense Fe3O4 on the surface of 9Ni steel billets is achieved, reducing the formation of holes in the outer oxide layer, reducing the inward diffusion of oxygen, and suppressing the formation of along-crystal cracks.

Benefits of technology

It effectively improves the high-temperature oxidation resistance and crack resistance of 9Ni steel billets, reduces production costs, reduces environmental pollution, and ensures the surface quality of the rolled plate.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention discloses a heating method for improving high-temperature oxidation resistance and crack resistance of a 9Ni steel billet, which comprises the following steps of: controlling the temperature of a preheating section and the O2 content in mixed gas, and adjusting the O2 content, the heating rate and the heat preservation temperature in the mixed gas of a first soaking section, a second soaking section and a third soaking section, so as to promote the rapid generation of compact Fe3O4 on the surface of the 9Ni steel billet in the preheating process, thereby improving the high-temperature oxidation resistance and crack resistance of the 9Ni steel billet. The formation of holes and hot cracks in an outer oxide layer is effectively controlled, so that the diffusion effect of oxygen from the surface of the 9Ni steel billet to the interior of the 9Ni steel billet in the preheating and high-temperature soaking processes is obviously inhibited, and the stable control of weak oxidation and shallow crystal cracks on the surface of the 9Ni steel billet in the high-temperature heating process is realized; by means of the method, the problem that the production cost is high due to the fact that the metal yield is low under the high-nickel condition in the 9Ni steel billet hot rolling process can be effectively solved, the surface quality of a rolled plate can be fully guaranteed, and meanwhile environment-friendly and cost-reducing production of 9Ni steel billet non-oxidation coating heating is achieved.
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Description

Technical Field

[0001] The invention belongs to the technical field of steel plate surface quality control, and in particular relates to a heating method for improving high-temperature oxidation resistance and crack resistance of a 9Ni steel billet. Background Art

[0002] By the end of 2023, 28 liquefied natural gas (LNG) receiving stations have been built in China, with an annual receiving capacity of more than 116 million tons, ranking among the top in the world. At present, the materials that can safely store LNG below -162°C mainly include 9Ni steel, aluminum alloy, austenitic stainless steel and nickel alloy. Compared with other materials, 9Ni steel has become the preferred material for LNG storage and transportation and has been widely used due to its excellent low-temperature toughness, cold workability, weldability and crack propagation resistance, as well as lower ductile-brittle transition temperature and production cost.

[0003] The production process of 9Ni steel plate mainly includes smelting-continuous casting-ingot heating-controlled rolling and controlled cooling-heat treatment, and its final structure is low-carbon martensite + a small amount of reversed austenite. Before hot rolling production, 9Ni steel billets must be heated to 1150-1200℃ in a heating furnace and kept warm for a certain period of time. The fuel of the heating furnace is mainly coal gas (blast furnace gas / converter gas / coke oven gas) + combustion air. Due to the lack of antioxidant elements such as Cr and Al in the steel and the long-term heating in a high-temperature oxidizing environment, the 9Ni steel billet is severely burned after leaving the heating furnace and its surface is prone to obvious intergranular cracks, which will not only cause a significant reduction in the metal yield in the subsequent rolling process, but also easily lead to obvious cracking on the surface of the steel plate during subsequent thermal deformation and quenching, seriously affecting the surface quality and toughness of the product.

[0004] In order to effectively inhibit the high-temperature oxidation of steel billets, domestic and foreign steel companies mainly use the two methods of "adding antioxidant elements" and "spraying antioxidant coatings".

[0005] For example, the Chinese patents with publication numbers CN 114540712A and CN116219294A, which were published on May 27, 2022 and June 6, 2023, respectively, disclose "a kind of uncoated reinforced high-temperature oxidation-resistant hot stamping steel with added Ce element" and "a kind of uncoated high-temperature oxidation-resistant hot stamping steel with added Y element". The technical scheme mainly adds Ce and Y elements to form Ce and Y oxides on the surface of the steel plate, thereby reducing the growth rate of the oxide scale and increasing its adhesion to the matrix, thereby improving the high-temperature oxidation resistance of the steel. However, the high-content addition of Ce and Y not only significantly increases the production cost, but also easily leads to nodules in the continuous casting nozzle, which is not conducive to the continuous casting of 9Ni steel.

[0006] For example, the Chinese patents with publication numbers CN114438393B, CN 115047000A and CN 110229949A, which were published on March 21, 2023, September 13, 2022 and September 13, 2019, respectively, disclosed "a method for preventing intergranular oxidation cracks on the surface of high-nickel steel plates", "a method for evaluating the protective effect of high-temperature anti-oxidation coatings for nickel-based steels" and "a high-temperature anti-oxidation descaling isolation agent based on nickel-containing steel and a preparation method thereof". The technical solutions disclosed therein mainly inhibit the growth of iron oxide scale on the steel surface and the formation of intergranular cracks by grinding the ingot and spraying MgO-based or SiC-Al2O3-based high-temperature anti-oxidation coatings. However, grinding the ingot and spraying anti-oxidation coatings will not only significantly increase production costs, but may also cause significant environmental pollution.

[0007] The above-mentioned prior art mainly improves the high-temperature oxidation resistance and crack resistance of 9Ni steel by adding antioxidant Ce and Y elements, grinding the ingot and spraying antioxidant coatings. However, it has the disadvantages of being unfavorable for continuous casting, high production cost and being unfriendly to the environment, and is not suitable for the economical and environmentally friendly industrial production of 9Ni steel. Summary of the invention

[0008] In order to solve the above technical problems, the present invention provides a heating method for improving the high-temperature oxidation resistance and crack resistance of 9Ni steel billets. By controlling the heating atmosphere, heating rate and insulation temperature of the four-stage heating process, the reduction and harmless control of iron oxide scale and intergranular cracks on the surface of 9Ni steel billets at high temperatures are achieved. This can effectively improve the low metal yield and high production cost problems of the hot rolling process of 9Ni steel billets under high nickel conditions, and fully guarantee the surface quality of the rolled plates. At the same time, the environmentally friendly and cost-reducing production of 9Ni steel billets without oxidation coating can be achieved.

[0009] The specific technical solutions of the present invention are as follows:

[0010] The present invention provides a heating method for improving the high-temperature oxidation resistance and crack resistance of a 9Ni steel billet, the heating method comprising: heating the 9Ni steel billet in a mixed atmosphere of CO2, O2 and N2 through a preheating section, a soaking section, a soaking section 2 and a soaking section 3 in a heating furnace;

[0011] Preheating section: Control the volume fraction of O2 in the mixed atmosphere to 0.5-1.0%, and the temperature of the preheating section to 880-920°C;

[0012] Soaking stage: Control the volume fraction of O2 in the mixed atmosphere to be 0.5-1.5%, the temperature of the soaking stage to be 1030-1060°C; the heating rate from the preheating stage temperature to the soaking stage temperature is 1.4-1.6°C / min;

[0013] Soaking stage 2: Control the volume fraction of O2 in the mixed atmosphere to be 0.5-1.0%, the temperature of the soaking stage 2 to be 1120-1150°C; the heating rate from the temperature of the soaking stage 1 to the temperature of the soaking stage 2 is 1.8-2.1°C / min;

[0014] Three aquaponics stages: the volume fraction of O2 in the mixed atmosphere is controlled to be 0.5-1.0%, the temperature of the three aquaponics stages is 1190-1220°C; the heating rate from the temperature of the two aquaponics stages to the temperature of the three aquaponics stages is 2.2-2.5°C / min.

[0015] Furthermore, the insulation time of the preheating section is 20 to 25 minutes.

[0016] The soaking and heat preservation time of the soaking section is 3 to 5 minutes.

[0017] The second heat-isolating stage has a heat-isolating and heat-keeping time of 3 to 5 minutes.

[0018] The heat-maintaining time of the three heat-maintaining stages is 2 to 4 minutes.

[0019] In the mixed atmosphere, the volume fractions of CO2 and N2 are 15% to 35% and 67% to 85% respectively.

[0020] The residence time of the 9Ni steel billet in the heating furnace is 180 to 240 minutes.

[0021] After leaving the heating furnace, the 9Ni steel billet is air-cooled to room temperature.

[0022] After the 9Ni steel billet is heated in a heating furnace, the thickness of its inner oxide layer is ≤520μm; the thickness of its outer oxide layer is ≤620μm; the thickness of its total oxide layer is ≤1150μm; no intergranular cracks appear in the inner oxide layer; and no cracks occur in the outer oxide layer.

[0023] Since 9Ni steel lacks antioxidant elements such as Cr and Al and needs to be heated for a long time in a high-temperature oxidation environment, the 9Ni steel billet is severely burned after leaving the heating furnace and has many intergranular cracks on its surface, which can easily lead to a decrease in metal yield in the subsequent rolling process and obvious cracking on the surface of the steel plate, seriously affecting the surface quality and toughness of the product. If anti-oxidation coating is sprayed before entering the heating furnace, the production cost of 9Ni steel will increase significantly and the environmental pollution in the production process will increase.

[0024] The present invention is based on the heating system and flue gas composition of the heating furnace of the hot rolling mill. By optimizing and controlling the oxidizing atmosphere, heating rate and preheating (averaging) temperature of the preheating section, the first soaking section, the second soaking section and the third soaking section, the rapid generation of dense Fe3O4 on the surface of the 9Ni steel billet during the high-temperature heating process is promoted, the formation of holes in the outer oxide layer is reduced, and the thickness of the inner and outer oxide layers of the 9Ni steel is simultaneously thinned and the surface intergranular cracks are reduced without the protection of an anti-oxidation coating, thereby relaxing the requirement for coating the 9Ni steel billet with an anti-oxidation coating before entering the heating furnace, and realizing cost-reducing and environmentally friendly production of 9Ni steel.

[0025] Compared with the prior art, the present invention has the following beneficial effects:

[0026] (1) The present invention optimizes the preheating temperature and the O2 content in the heating atmosphere, thereby promoting the rapid formation of dense Fe3O4 on the surface of the 9Ni steel billet during the preheating process and avoiding the formation of loose Fe2O3, thereby significantly hindering the inward diffusion of oxygen and improving the problem of thick outer oxide scale formed during the long-term heating process in the heating furnace, resulting in a low hot rolling metal yield.

[0027] (2) The present invention controls the O2 content in the mixed gas in the first, second and third stages of the soaking process, thereby further reducing the diffusion rate of oxygen atoms in the outer oxide layer of 9Ni steel and their reaction with iron atoms during the high-temperature soaking process, and effectively inhibits the formation of pores in the outer oxide layer, thereby blocking the inward diffusion channel of oxygen atoms and reducing the depth of intergranular cracks on the surface of the 9Ni steel billet.

[0028] (3) The present invention effectively avoids the concentration of thermal stress generated by the temperature difference between the inner and outer oxide layers on the outer oxide layer, causing thermal cracks in the outer oxide layer, by controlling the heating rate and the absorptive temperature of the first, second and third absorptive stages, thereby reducing the risk of sudden oxidation on the surface of the 9Ni steel billet and further achieving stable control of weak oxidation and shallow intergranular cracks on the surface of the 9Ni steel billet during high-temperature heating. BRIEF DESCRIPTION OF THE DRAWINGS

[0029] Figure 1 This is the SEM morphology of the oxide layer cross section of Example 1;

[0030] Figure 2 The cross-sectional SEM morphology of the oxide layer of Comparative Example 1;

[0031] Figure 3 The energy spectrum analysis result of the surface phase (Fe3O4) of the oxide layer of Example 1;

[0032] Figure 4 This is the energy spectrum analysis result of the oxide layer surface phase (Fe2O3) of Comparative Example 1. DETAILED DESCRIPTION

[0033] In order to make the purpose, technical solution and advantages of the embodiments of the present invention clearer, the technical solution in the embodiments of the present invention will be clearly and completely described below in combination with the embodiments of the present invention. Obviously, the described embodiments are part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0034] If no specific techniques or conditions are specified in the examples, they can be carried out according to the techniques or conditions described in the literature in the art or according to the product instructions.

[0035] The chemical composition and weight percentage of the 9Ni steel billet in each embodiment and comparative example are: 0.043% C, 0.254% Si, 0.652% Mn, 0.0041% P, 0.0012% S, 9.12% Ni, 0.032% Al, and the rest is Fe and unavoidable impurities.

[0036] Example 1

[0037] A heating method for improving the high temperature oxidation resistance and crack resistance of a 9Ni steel billet comprises the following steps:

[0038] 1) 9Ni steel billet was processed into several 10mm×10mm×10mm cubic specimens by wire cutting. The specimens were ground with water sandpaper to 2000#, then polished, cleaned with alcohol and dried for later use.

[0039] 2) The horizontal molybdenum wire furnace is heated to a preheating temperature of 880°C and kept warm. Subsequently, a mixed gas of CO2, O2 and N2 with volume fractions of 15%, 1% and 84% respectively is introduced into the furnace. The sum of the flow rates of CO2, O2 and N2 is fixed at 1 L / min. After the mixed gas is introduced for 15 minutes, the 9Ni billet sample is pushed into the molybdenum wire furnace and the temperature is raised to 880°C with the furnace and kept warm for 25 minutes.

[0040] 3) The temperature of the molybdenum wire furnace was continuously raised at a rate of 1.5°C / min to a uniform heating temperature of 1043°C and kept at that temperature for 4 minutes. During the heating process, the volume fractions of the mixed gases CO2, O2 and N2 were adjusted to 15%, 1.5% and 83.5%, respectively.

[0041] 4) The heating furnace is heated at a rate of 1.85°C / min to a second-stage uniform heating temperature of 1124°C and kept at this temperature for 4 minutes. During the heating process, the volume fractions of the mixed gases CO2, O2 and N2 are adjusted to 15%, 0.9% and 84.1%, respectively.

[0042] 5) Continue to heat the heating furnace at 2.3℃ / min to the third-stage absorpting temperature of 1195℃ and keep it at this temperature for 3 minutes. Do not change the volume fraction of the mixed gas CO2, O2 and N2 during the heating and absorpting process. After the sample is kept at this temperature for 3 minutes, take it out and air cool it to room temperature.

[0043] Example 2

[0044] A high temperature anti-oxidation and anti-cracking heating atmosphere and heating method for a 9Ni steel billet (whose chemical composition is the same as that of Example 1), comprising the following steps:

[0045] 1) Sample processing: The sample processing method is the same as that in Example 1.

[0046] 2) The horizontal molybdenum wire furnace is heated to a preheating temperature of 891°C and kept warm. Subsequently, a mixed gas of CO2, O2 and N2 with volume fractions of 23%, 0.8% and 76.2% respectively is introduced into the furnace (the sum of the flow rates of CO2, O2 and N2 is fixed at 1 L / min). After the mixed gas is introduced for 15 minutes, the 9Ni billet sample is pushed into the molybdenum wire furnace and the temperature is raised to 891°C with the furnace and kept warm for 23 minutes.

[0047] 3) The temperature of the molybdenum wire furnace was continuously raised at a rate of 1.4°C / min to a uniform heating temperature of 1030°C and kept at that temperature for 4.5 minutes. During the heating process, the volume fractions of the mixed gases CO2, O2 and N2 were adjusted to 23%, 1.3% and 75.7%, respectively.

[0048] 4) The heating furnace is heated at a rate of 1.93°C / min to a second-stage uniform heating temperature of 1132°C and kept at this temperature for 3.5 minutes. During the heating process, the volume fractions of the mixed gases CO2, O2 and N2 are adjusted to 23%, 0.8% and 76.2%, respectively.

[0049] 5) Continue to heat the heating furnace at 2.2℃ / min to the third-stage absorpting temperature of 1201℃ and keep it warm for 3.5 minutes. The volume fractions of the mixed gases CO2, O2 and N2 do not change during the heating process. The volume fractions of the mixed gases CO2, O2 and N2 do not change during the heating and absorpting process. After the sample has been kept warm for 3.5 minutes, take it out and air cool it to room temperature.

[0050] Example 3

[0051] A high temperature anti-oxidation and anti-cracking heating atmosphere and heating method for a 9Ni steel billet (whose chemical composition is the same as that of Example 1), comprising the following steps:

[0052] 1) Sample processing: The sample processing method is the same as that in Example 1.

[0053] 2) The horizontal molybdenum wire furnace is heated to a preheating temperature of 905°C and kept warm. Subsequently, a mixed gas of CO2, O2 and N2 with volume fractions of 29%, 0.6% and 70.4% respectively is introduced into the furnace (the sum of the flow rates of CO2, O2 and N2 is fixed at 1 L / min). After the mixed gas is introduced for 15 minutes, the 9Ni billet sample is pushed into the molybdenum wire furnace and the temperature is raised to 905°C with the furnace and kept warm for 21 minutes.

[0054] 3) The molybdenum wire furnace is heated at a rate of 1.45°C / min to a uniform heating temperature of 1050°C and kept at this temperature for 5 minutes. During the heating process, the volume fractions of the mixed gases CO2, O2 and N2 are adjusted to 29%, 0.95% and 70.05%, respectively.

[0055] 4) The heating furnace is heated at a rate of 1.99°C / min to a second-stage uniform heating temperature of 1140°C and kept at this temperature for 4.5 minutes. During the heating process, the volume fractions of the mixed gases CO2, O2 and N2 are adjusted to 29%, 0.7% and 70.3%, respectively.

[0056] 5) Continue to heat the heating furnace at 2.4℃ / min to the third-stage absorpting temperature of 1212℃ and keep it warm for 2.5min. The volume fractions of the mixed gas CO2, O2 and N2 do not change during the heating process. The volume fractions of the mixed gas CO2, O2 and N2 do not change during the heating and absorpting process. After the sample is kept warm for 2.5min, take it out and air cool it to room temperature.

[0057] Example 4

[0058] A high temperature anti-oxidation and anti-cracking heating atmosphere and heating method for a 9Ni steel billet (whose chemical composition is the same as that of Example 1), comprising the following steps:

[0059] 1) Sample processing: The sample processing method is the same as that in Example 1.

[0060] 2) The horizontal molybdenum wire furnace is heated to a preheating temperature of 918°C and kept warm. Subsequently, a mixed gas of CO2, O2 and N2 with volume fractions of 34%, 0.5% and 65.5% respectively is introduced into the furnace (the sum of the flow rates of CO2, O2 and N2 is fixed at 1 L / min). After the mixed gas is introduced for 15 minutes, the 9Ni billet sample is pushed into the molybdenum wire furnace and the temperature is raised to 918°C with the furnace and kept warm for 22 minutes.

[0061] 3) The temperature of the molybdenum wire furnace was continuously raised at a rate of 1.55°C / min to a uniform heating temperature of 1058°C and kept at that temperature for 3.5 minutes. During the heating process, the volume fractions of the mixed gases CO2, O2 and N2 were adjusted to 34%, 0.55% and 65.45%, respectively.

[0062] 4) The heating furnace is heated at a rate of 2.08°C / min to a second-stage uniform heating temperature of 1148°C and maintained at this temperature for 3 minutes. During the heating process, the volume fractions of the mixed gases CO2, O2 and N2 are adjusted to 34%, 0.55% and 65.45%, respectively.

[0063] 5) Continue to heat the heating furnace at 2.35℃ / min to the third-stage absorpting temperature of 1219℃ and keep it at this temperature for 2 minutes. Do not change the volume fraction of the mixed gas CO2, O2 and N2 during the heating and absorpting process. After the sample has been kept at this temperature for 2 minutes, take it out and air cool it to room temperature.

[0064] Comparative Example 1

[0065] A method for heating a 9Ni steel billet comprises the following steps:

[0066] 1) Sample processing: The sample processing method is the same as that in Example 1.

[0067] 2) The horizontal molybdenum wire furnace is heated to a preheating temperature of 840°C and kept warm. Subsequently, a mixed gas of CO2, O2 and N2 with volume fractions of 18%, 1.5% and 80.5% respectively is introduced into the furnace (the sum of the flow rates of CO2, O2 and N2 is fixed at 1 L / min). After the mixed gas is introduced for 15 minutes, the 9Ni billet sample is pushed into the molybdenum wire furnace and the temperature is raised to 840°C with the furnace and kept warm for 24 minutes.

[0068] 3) The temperature of the molybdenum wire furnace was continuously raised at a rate of 1.6°C / min to a uniform heating temperature of 1036°C and kept at that temperature for 5 minutes. During the heating process, the volume fractions of the mixed gases CO2, O2 and N2 were adjusted to 18%, 1.5% and 80.5%, respectively.

[0069] 4) The heating furnace is heated at a rate of 1.88°C / min to a second-stage temperature of 1126°C and kept at this temperature for 4 minutes. During the heating process, the volume fractions of the mixed gases CO2, O2 and N2 are adjusted to 18%, 0.5% and 81.5%, respectively.

[0070] 5) The heating furnace is heated at a rate of 2.3°C / min to a temperature of 1194°C in the third stage of uniform heating and kept at this temperature for 3 minutes. The volume fractions of the mixed gases CO2, O2 and N2 are not changed during the heating process.

[0071] 6) After keeping the sample warm for 3 minutes, take it out and air cool it to room temperature.

[0072] Comparative Example 2

[0073] A method for heating a 9Ni steel billet comprises the following steps:

[0074] 1) Sample processing: The sample processing method is the same as that in Example 1.

[0075] 2) The horizontal molybdenum wire furnace is heated to a preheating temperature of 895°C and kept warm. Subsequently, a mixed gas of CO2, O2 and N2 with volume fractions of 27%, 1% and 72% respectively is introduced into the furnace (the sum of the flow rates of CO2, O2 and N2 is fixed at 1 L / min). After the mixed gas is introduced for 15 minutes, the 9Ni billet sample is pushed into the molybdenum wire furnace and the temperature is raised to 895°C with the furnace and kept warm for 23 minutes.

[0076] 3) The temperature of the molybdenum wire furnace was continuously raised at a rate of 1.75°C / min to a uniform heating temperature of 1051°C and kept at that temperature for 4.5 minutes. During the heating process, the volume fractions of the mixed gases CO2, O2 and N2 were adjusted to 27%, 2% and 71% respectively.

[0077] 4) The heating furnace is heated at a rate of 2.2°C / min to a second-stage temperature of 1130°C and kept at this temperature for 5 minutes. During the heating process, the volume fractions of the mixed gases CO2, O2 and N2 are adjusted to 27%, 1.5% and 71.5%, respectively.

[0078] 5) The heating furnace is heated at a rate of 2.6°C / min to a temperature of 1200°C in the third stage of uniform heating and kept at that temperature for 4 minutes. The volume fractions of the mixed gas CO2, O2 and N2 are not changed during the heating process.

[0079] 6) After keeping the sample warm for 4 minutes, take it out and air cool it to room temperature.

[0080] The cross-sectional morphology of the oxidized samples of Examples 1 to 4, Comparative Example 1, and Comparative Example 2 was observed and photographed using a scanning electron microscope (SEM), the holes and cracks in the outer oxide layer were observed, and the diameter of the holes in the outer oxide layer of each sample, the thickness of the inner and outer oxide layers, and the depth of the intergranular cracks in the inner oxide layer were measured. The results are shown in Table 1.

[0081] Table 1 Oxide layer thickness and holes and cracks of various embodiments of the present invention and comparative examples

[0082]

[0083] It can be seen from the above table that the total oxide layer thickness of the samples of Examples 1 to 4, which adopt high preheating temperature, low mixed gas O2 content and low heating rate, after high-temperature oxidation is 947 to 1134 μm, the outer oxide layer thickness is 526 to 617 μm, the inner oxide layer thickness is 421 to 517 μm, and the outer oxide layer has no obvious holes or cracks. The outer oxide layer phase is mainly Fe3O4, and there is basically no intergranular crack in the inner oxide layer.

[0084] Compared with Examples 1 to 4, the preheating temperature of Comparative Example 1 is lower, the volume fraction of O2 in the mixed gas is higher, the thickness of the inner and outer oxide layers increases to 725 and 1031 μm, respectively, and obvious large holes appear in the outer oxide layer, such as Figure 2As shown, and its outermost phase is Fe2O3, as Figure 4 As shown in the figure, there are obvious intergranular cracks in the inner oxide layer, and the depth reaches 755μm.

[0085] Compared with Examples 1 to 4, the heating rates of the first, second and third equalizing stages of Comparative Example 2 are faster and the volume fraction of O2 in the mixed gas is higher. The thicknesses of the inner and outer oxide layers are increased to 834 and 1109 μm, respectively. Obvious large holes and cracks appear in the outer oxide layer, and the intergranular cracks in the inner oxide layer are further deepened, with a depth of 823 μm.

[0086] The above-mentioned detailed description of a heating method for improving the high-temperature oxidation resistance and crack resistance of 9Ni steel billet with reference to the embodiment is illustrative rather than restrictive, and several embodiments can be listed according to the limited scope. Therefore, changes and modifications without departing from the overall concept of the present invention should fall within the scope of protection of the present invention.

Claims

1. A heating method for improving the high temperature oxidation resistance and crack resistance of 9Ni steel billet, characterized in that: The heating method comprises: heating the 9Ni steel billet in a mixed atmosphere of CO2, O2 and N2 through a preheating section, a soaking section, a soaking section, and a soaking section in a heating furnace; Preheating section: Control the volume fraction of O2 in the mixed atmosphere to 0.5-1.0%, and the temperature of the preheating section to 880-920°C; Soaking stage: Control the volume fraction of O2 in the mixed atmosphere to be 0.5-1.5%, the temperature of the soaking stage to be 1030-1060°C; the heating rate from the preheating stage temperature to the soaking stage temperature is 1.4-1.6°C / min; Soaking stage 2: Control the volume fraction of O2 in the mixed atmosphere to be 0.5-1.0%, the temperature of the soaking stage 2 to be 1120-1150°C; the heating rate from the temperature of the soaking stage 1 to the temperature of the soaking stage 2 is 1.8-2.1°C / min; Three aquaponics stages: the volume fraction of O2 in the mixed atmosphere is controlled to be 0.5-1.0%, the temperature of the three aquaponics stages is 1190-1220°C; the heating rate from the temperature of the two aquaponics stages to the temperature of the three aquaponics stages is 2.2-2.5°C / min.

2. The heating method according to claim 1, characterized in that: The holding time of the preheating section is 20 to 25 minutes.

3. The heating method according to claim 1, characterized in that: The soaking and heat preservation time of the soaking section is 3 to 5 minutes.

4. The heating method according to claim 1, characterized in that: The second heat-isolating stage has a heat-isolating and heat-keeping time of 3 to 5 minutes.

5. The heating method according to claim 1, characterized in that: The heat-maintaining time of the three heat-maintaining stages is 2 to 4 minutes.

6. The heating method according to any one of claims 1 to 5, characterized in that: In the mixed atmosphere, the volume fractions of CO2 and N2 are 15% to 35% and 67% to 85% respectively.

7. The heating method according to any one of claims 1 to 5, characterized in that: The residence time of the 9Ni steel billet in the heating furnace is 180 to 240 minutes.

8. The heating method according to any one of claims 1 to 5, characterized in that: After leaving the heating furnace, the 9Ni steel billet is air-cooled to room temperature.

9. The heating method according to any one of claims 1 to 5, characterized in that: After the 9Ni steel billet is heated in a heating furnace, the thickness of its inner oxide layer is ≤520μm; the thickness of its outer oxide layer is ≤620μm; the thickness of its total oxide layer is ≤1150μm; no intergranular cracks appear in the inner oxide layer; and no cracks occur in the outer oxide layer.

Citation Information

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