Smelting process of high-temperature-resistant alloy

Abstract

The invention relates to a smelting process of a high-temperature-resistant alloy, and belongs to the technical field of alloy smelting. The preparation method comprises the following steps: adding 0.06 to 0.08 part of C, 0.3 to 0.5 part of Si, 0.8 to 1.0 part of Mn, 0.008 to 0.01 part of S, 14 to 17 parts of Cr, 70 to 75 parts of Ni, 0.4 to 1.0 part of Al, 2.25 to 2.75 parts of Ti, 0.35 to 0.6 part of Nb, 0.35 to 0.6 part of Ta, 5 to 9 parts of Fe, 0.3 to 0.5 part of Cu and 0.8 to 1.0 part of Co into a crucible, heating and stirring until melting, refining, pouring and cooling to obtain an ingot mold; the ingot mold is immersed into a quenching agent, and quenching and heat treatment are conducted; the quenching agent disclosed by the invention is prepared from 2-5 parts of amino di (methylene phosphoric acid), epoxy propyl bisphenol fluorene acrylate, an ethylene boric anhydride pyridine complex and potassium persulfate. The prepared alloy is excellent in mechanical property and good in high temperature resistance, and the service life is effectively prolonged.

Description

Technical Field

[0001] The invention relates to the technical field of alloy smelting, in particular to a smelting process of a high-temperature resistant alloy. Background Art

[0002] Heat-resistant alloys, also known as high-temperature alloys, are alloys with stable organization and excellent mechanical, physical and chemical properties under high-temperature use conditions. They include heat-resistant steel, heat-resistant aluminum alloys, heat-resistant titanium alloys, high-temperature alloys, refractory alloys, etc. Heat-resistant alloys have certain tensile, creep, fatigue, physical, chemical and process properties at high temperatures.

[0003] Chinese patent CN111172414A: relates to a high-temperature resistant alloy casting smelting process under a reducing atmosphere, comprising the following steps: smelting: 1) using tungsten powder as a melt, metal nickel as a flux, and metal molybdenum as an element to increase high-temperature corrosion resistance, and using a medium frequency furnace for smelting. First, tungsten powder and metal nickel are added to the medium frequency furnace, and then metal molybdenum is added after melting. The weight contents of tungsten powder, metal nickel, and metal molybdenum are 5%, 65%, and 30%, respectively. Subsequently, the temperature of the medium frequency furnace is controlled between 1590°C and 1620°C for slag removal; Casting: Casting is performed using a silica sol investment casting process, and sand removal and cutting are performed after cooling after casting.

[0004] Chinese patent CN110894581A: discloses a high-temperature resistant alloy material for radiant tubes and a casting process thereof, wherein the high-temperature resistant alloy material for radiant tubes contains the following components in weight percentage: C: 0.50% to 0.80%, Cr: 18.0% to 25.0%, Ni: 29.0% to 35.0%, Si: 3% to 7%, W: 3.5% to 5.5%, Mo: 0.5% to 1.5%, Mn: 2% to 6.3%, Al: 10% to 12%, Ti: 0.5% to 1.5%, B: 1.6% to 2.5%, Co: 1.0% to 2.5%, and the balance is iron and unavoidable impurities, and the content of impurities is ≤3%.

[0005] Chinese patent CN106676366B: discloses a high temperature resistant alloy, which includes the following elements in weight percentage: Cr: 10-11; Co: 2-3; C: 0.3-0.5; Mo: 3-4; W: 10; La: 0.005-0.02; Si: 0.1-0.3; Al: 1-2; Ti: 2-3; Nd: 5-7; Nb: 0.7-1; Re: 5-6; Fe: 15-20.

[0006] The mechanical properties of the alloys prepared by the above patents and prior art need to be further improved, and the high temperature resistance is poor. After long-term use, they will cause burning, bending deformation, and fracture. Summary of the invention

[0007] In order to solve the above problems, the present invention provides a smelting process of a high temperature resistant alloy, and the operation steps are as follows:

[0008] S1: add 0.06-0.08 parts of C, 0.3-0.5 parts of Si, 0.8-1.0 parts of Mn, 0.008-0.01 parts of S, 14-17 parts of Cr, 70-75 parts of Ni, 0.4-1.0 parts of Al, 2.25-2.75 parts of Ti, 0.35-0.6 parts of Nb, 0.35-0.6 parts of Ta, 5-9 parts of Fe, 0.3-0.5 parts of Cu, and 0.8-1.0 parts of Co into a crucible, and heat and stir until melted;

[0009] S2: The molten steel is refined;

[0010] S3: After the refined molten steel is cooled, it is poured into the mold; after pouring, it is cooled in the furnace for 5-10 minutes, and the vacuum is broken to take out the ingot mold;

[0011] S4: Immerse the ingot mold into the quenching agent, quench, and heat treat.

[0012] When loading the crucible, the bottom should be tight and the top loose to avoid "bridging".

[0013] The S1 is heated to 1200-1350°C.

[0014] The refining temperature of S2 is 1675-1685°C and the refining time is 25-35 minutes.

[0015] The pouring temperature of S3 is 1440-1460°C.

[0016] The vacuum degree of S3 is 0.6-0.67Pa.

[0017] The quenching temperature is 530-560°C and the time is 10-15 minutes.

[0018] The heat treatment temperature is 180-220°C and the time is 10-15h

[0019] The preparation method of the quenching agent is:

[0020] H1: After nitrogen is introduced into the reaction kettle, 2-5 parts of amino di(methylene phosphoric acid), 6-12 parts of glycidyl bisphenol fluorene acrylate, and 400-500 parts of water are added, the pH is adjusted to 10 with sodium hydroxide, the temperature is raised to 75-95°C, and the reaction is carried out for 100-200 minutes;

[0021] H2: Add 0.02-0.2 parts of ethylene boric anhydride pyridine complex CAS: 442850-89-7 and 0.05-0.3 parts of potassium persulfate, raise the temperature to 60-70°C, stir and react for 50-100 minutes to obtain a quenching agent.

[0022] Reaction mechanism

[0023] Glycidyl bisphenol fluorene acrylate is a compound with epoxy groups and acrylate groups. Its structure contains multiple active sites and can react with different amino compounds.

[0024] Reaction of amino di(methylene phosphoric acid): The amino group in amino di(methylene phosphoric acid) can undergo a ring-opening addition reaction with the epoxy group in glycidyl bisphenol fluorene acrylate. During the reaction, the amino group attacks the epoxy group, causing the epoxy ring to open and form a new chemical bond.

[0025] The ethylene boric anhydride pyridine complex is then emulsion polymerized with an addition reactant to obtain a novel compound containing methylene phosphoric acid, boric anhydride pyridine complex and bisphenol fluorene as a quenching agent.

[0026] Technical Effects

[0027] The present invention provides a smelting process for a high temperature resistant alloy. Compared with the prior art, the present invention has the following significant effects:

[0028] 1. Composition and structure

[0029] The role of methylene phosphoric acid: It helps to reduce oxidation and decarburization on the surface of the workpiece, thereby maintaining the original structure and performance of the workpiece; the boric anhydride pyridine complex has unique chemical properties and can form a stable compound layer during the quenching process, which helps to improve the wear resistance and corrosion resistance of the workpiece; at the same time, the complex may also participate in regulating the cooling rate of the quenching medium so that the workpiece obtains a more uniform tissue distribution; bisphenol fluorene, as a compound containing an aromatic ring, can increase the high temperature stability and oxidation resistance of the quenching agent by adding it; in addition, bisphenol fluorene may also interact with other elements in the steel to affect the phase change process and microstructure of the steel.

[0030] 2. Microstructure changes

[0031] Grain refinement: The use of new quenching agents can lead to grain refinement of stainless steel during quenching; this is because rapid cooling can inhibit grain growth, resulting in a finer grain structure; this refined grain structure helps to improve the strength and toughness of steel.

[0032] The residual stress generated during the quenching process has an important influence on the performance of the workpiece; the use of new quenching agents may change the distribution and size of residual stress; it can reduce the residual stress level and improve its distribution state, thereby improving the dimensional stability and performance of the workpiece.

[0033] 3. Performance Improvement

[0034] Hardness and Strength: Stainless steel castings using the new quenchant have higher hardness and strength due to grain refinement and phase transformation control; this is particularly important in applications that need to withstand high loads and wear.

[0035] Corrosion resistance: The addition of boric anhydride pyridine complex and other ingredients may improve the corrosion resistance of stainless steel castings; this is because these ingredients form a dense protective film on the surface of the workpiece, which can effectively prevent the intrusion of corrosive media. DETAILED DESCRIPTION

[0036] In order to further explain the technical means and effects adopted by the present invention to achieve the predetermined invention purpose, the following is a detailed description in combination with embodiments and comparative examples:

[0037] 1. Hardness test: refer to ASTME10-18 for testing;

[0038] 2. Tests of tensile strength, yield strength, elongation after fracture and area shrinkage: Test in accordance with ASTM E8 / E8M-22;

[0039] 3. Durability test: Test the durability time at 1000℃ and 500MPa.

[0040] Example 1

[0041] A smelting process for a high temperature resistant alloy, the operating steps of which are:

[0042] S1: Add 0.06gC, 0.3gSi, 0.8gMn, 0.008gS, 14gCr, 70gNi, 0.4gAl, 2.25gTi, 0.35gNb, 0.35gTa, 5gFe, 0.3gCu and 0.8gCo into a crucible and heat and stir until melted;

[0043] S2: The molten steel is refined;

[0044] S3: After the refined molten steel is cooled, it is poured into the mold; after pouring, it is cooled in the furnace for 5 minutes, and the vacuum is broken to take out the ingot mold;

[0045] S4: Immerse the ingot mold into the quenching agent, quench, and heat treat.

[0046] When loading the crucible, the bottom should be tight and the top loose to avoid "bridging".

[0047] The S1 is heated to 1200°C.

[0048] The refining temperature of S2 is 1675°C and the refining time is 25 minutes.

[0049] The pouring temperature of S3 is 1440°C.

[0050] The vacuum degree of S3 is 0.6Pa.

[0051] The quenching temperature is 530° C. and the quenching time is 10 minutes.

[0052] The heat treatment temperature is 180°C and the time is 10h

[0053] The preparation method of the quenching agent is:

[0054] H1: After nitrogen is introduced into the reactor, 2 g of amino di(methylene phosphoric acid), 6 g of glycidyl bisphenol fluorene acrylate, and 400 g of water are added, the pH is adjusted to 10 with sodium hydroxide, the temperature is raised to 75°C, and the reaction is carried out for 100 minutes;

[0055] H2: Add 0.02 g of ethylene boric anhydride pyridine complex CAS: 442850-89-7 and 0.05 g of potassium persulfate, raise the temperature to 60°C, stir and react for 50 minutes to obtain a quenching agent.

[0056] Example 2

[0057] A smelting process for a high temperature resistant alloy, the operating steps of which are:

[0058] S1: Add 0.07gC, 0.4gSi, 0.9gMn, 0.009gS, 15gCr, 72gNi, 0.6gAl, 2.35gTi, 0.45gNb, 0.45gTa, 6gFe, 0.4gCu and 0.9gCo into a crucible and heat and stir until melted;

[0059] S2: The molten steel is refined;

[0060] S3: After the refined molten steel is cooled, it is poured into the mold; after pouring, it is cooled in the furnace for 6 minutes, and the vacuum is broken to take out the ingot mold;

[0061] S4: Immerse the ingot mold into the quenching agent, quench, and heat treat.

[0062] When loading the crucible, the bottom should be tight and the top loose to avoid "bridging".

[0063] The S1 is heated to 1250°C.

[0064] The refining temperature of S2 is 1678°C and the refining time is 28 minutes.

[0065] The pouring temperature of S3 is 1445°C.

[0066] The vacuum degree of S3 is 0.62Pa.

[0067] The quenching temperature is 540° C. and the quenching time is 12 minutes.

[0068] The heat treatment temperature is 190°C and the time is 12h

[0069] The preparation method of the quenching agent is:

[0070] H1: After nitrogen was introduced into the reactor, 3 g of amino di(methylene phosphoric acid), 8 g of glycidyl bisphenol fluorene acrylate, and 440 g of water were added, the pH was adjusted to 10 with sodium hydroxide, the temperature was raised to 80°C, and the reaction was carried out for 140 minutes;

[0071] H2: Add 0.1 g of ethylene boric anhydride pyridine complex CAS: 442850-89-7 and 0.1 g of potassium persulfate, raise the temperature to 65°C, stir and react for 60 minutes to obtain a quenching agent.

[0072] Example 3

[0073] A smelting process for a high temperature resistant alloy, the operating steps of which are:

[0074] S1: Add 0.07gC, 0.4gSi, 0.9gMn, 0.009gS, 16gCr, 74gNi, 0.8gAl, 2.65gTi, 0.55gNb, 0.55gTa, 8gFe, 0.4gCu and 0.9gCo into a crucible and heat and stir until melted;

[0075] S2: The molten steel is refined;

[0076] S3: After the refined molten steel is cooled, it is poured into the mold; after pouring, it is cooled in the furnace for 8 minutes, and the vacuum is broken to take out the ingot mold;

[0077] S4: Immerse the ingot mold into the quenching agent, quench, and heat treat.

[0078] When loading the crucible, the bottom should be tight and the top loose to avoid "bridging".

[0079] The S1 is heated to 1330°C.

[0080] The refining temperature of S2 is 1683°C and the refining time is 33 minutes.

[0081] The pouring temperature of S3 is 1455°C.

[0082] The vacuum degree of S3 is 0.65Pa.

[0083] The quenching temperature is 550° C. and the quenching time is 14 minutes.

[0084] The heat treatment temperature is 210°C and the time is 14h

[0085] The preparation method of the quenching agent is:

[0086] H1: After nitrogen is introduced into the reactor, 4 g of amino di(methylene phosphoric acid), 10 g of glycidyl bisphenol fluorene acrylate, and 480 g of water are added, the pH is adjusted to 10 with sodium hydroxide, the temperature is raised to 90°C, and the reaction is carried out for 180 minutes;

[0087] H2: Add 0.15 g of ethylene boric anhydride pyridine complex CAS: 442850-89-7 and 0.2 g of potassium persulfate, raise the temperature to 65°C, stir and react for 90 minutes to obtain a quenching agent.

[0088] Example 4

[0089] A smelting process for a high temperature resistant alloy, the operating steps of which are:

[0090] S1: Add 0.08gC, 0.5gSi, 1.0gMn, 0.01gS, 17gCr, 75gNi, 1.0gAl, 2.75gTi, 0.6gNb, 0.6gTa, 9gFe, 0.5gCu and 1.0gCo into a crucible and heat and stir until melted;

[0091] S2: The molten steel is refined;

[0092] S3: After the refined molten steel is cooled, it is poured into the mold; after pouring, it is cooled in the furnace for 10 minutes, and the vacuum is broken to take out the ingot mold;

[0093] S4: Immerse the ingot mold into the quenching agent, quench, and heat treat.

[0094] When loading the crucible, the bottom should be tight and the top loose to avoid "bridging".

[0095] The S1 is heated to 1350°C.

[0096] The refining temperature of S2 is 1685°C and the refining time is 35 minutes.

[0097] The pouring temperature of S3 is 1460°C.

[0098] The vacuum degree is 0.67Pa.

[0099] The quenching temperature is 560° C. and the quenching time is 15 minutes.

[0100] The heat treatment temperature is 220°C and the time is 15h

[0101] The preparation method of the quenching agent is:

[0102] H1: After nitrogen was introduced into the reactor, 5 g of aminodi(methylenephosphonic acid), 12 g of glycidyl bisphenol fluorene acrylate, and 500 g of water were added, the pH was adjusted to 10 with sodium hydroxide, the temperature was raised to 95°C, and the reaction was carried out for 200 minutes;

[0103] H2: Add 0.2 g of ethylene boric anhydride pyridine complex CAS: 442850-89-7 and 0.3 g of potassium persulfate, raise the temperature to 70°C, stir and react for 100 minutes to obtain a quenching agent.

[0104] Comparative Example 1

[0105] No quenching agent was added, and the rest was the same as in Example 1.

[0106] Comparative Example 2

[0107] No aminodi(methylenephosphonic acid) was added, and the other conditions were the same as in Example 1.

[0108] Comparative Example 3

[0109] The ethylene boric anhydride pyridine complex was not added, and the other steps were the same as in Example 1.

[0110] The test results are shown in Table 1.

[0111] Table 1

[0112] Hardness / HB Tensile strength / MPa Yield strength / MPa Elongation after break / % Sectional shrinkage / % Durable life / h Example 1 355 1170 790 19.8 22.2 108 Example 2 358 1172 793 20.0 22.4 112 Example 3 361 1174 797 20.3 22.7 117 Example 4 363 1175 800 20.5 23.0 120 Comparative Example 1 302 1053 661 16.4 18.8 83 Comparative Example 2 338 1136 735 18.1 19.9 95 Comparative Example 3 343 1145 744 18.6 20.5 99

[0113] Through the data analysis of the above embodiments and comparative examples, the alloy prepared by the present invention has excellent mechanical properties such as hardness, tensile strength, yield strength, elongation after fracture, and cross-sectional shrinkage; it has good high temperature resistance and its service life is effectively improved.

[0114] The above description is only a preferred embodiment of the present invention and does not limit the present invention in any form. Although the present invention has been disclosed as a preferred embodiment as above, it is not used to limit the present invention. Any technical personnel in this field can make some changes or modify the technical contents disclosed above into equivalent embodiments without departing from the scope of the technical solution of the present invention. However, any brief modifications, equivalent changes and modifications made to the above embodiments based on the technical essence of the present invention without departing from the content of the technical solution of the present invention are still within the scope of the technical solution of the present invention.

Claims

1. A smelting process for a high temperature resistant alloy, the operating steps of which are: S1: add 0.06-0.08 parts of C, 0.3-0.5 parts of Si, 0.8-1.0 parts of Mn, 0.008-0.01 parts of S, 14-17 parts of Cr, 70-75 parts of Ni, 0.4-1.0 parts of Al, 2.25-2.75 parts of Ti, 0.35-0.6 parts of Nb, 0.35-0.6 parts of Ta, 5-9 parts of Fe, 0.3-0.5 parts of Cu, and 0.8-1.0 parts of Co into a crucible, and heat and stir until melted; S2: The molten steel is refined; S3: After the refined molten steel is cooled, it is poured into the mold; after pouring, it is cooled in the furnace for 5-10 minutes, and the vacuum is broken to take out the ingot mold; S4: immersing the ingot mold into a quenching agent, quenching, and heat treatment; The preparation method of the quenching agent is: H1: After nitrogen is introduced into the reaction kettle, 2-5 parts of amino di(methylene phosphoric acid), 6-12 parts of glycidyl bisphenol fluorene acrylate, and 400-500 parts of water are added, the pH is adjusted to 10 with sodium hydroxide, the temperature is raised to 75-95°C, and the reaction is carried out for 100-200 minutes; H2: Add 0.02-0.2 parts of ethylene boric anhydride pyridine complex and 0.05-0.3 parts of potassium persulfate, raise the temperature to 60-70°C, stir and react for 50-100 minutes to obtain a quenching agent.

2. A smelting process for a high temperature resistant alloy according to claim 1, Features: When loading the crucible, the bottom should be tight and the top loose to avoid "bridging".

3. A smelting process for a high temperature resistant alloy according to claim 1, Features: The S1 is heated to 1200-1350°C.

4. A smelting process for a high temperature resistant alloy according to claim 1, Features: The refining temperature of S2 is 1675-1685°C and the refining time is 25-35 minutes.

5. A smelting process for a high temperature resistant alloy according to claim 1, Features: The pouring temperature of S3 is 1440-1460°C.

6. A smelting process for a high temperature resistant alloy according to claim 1, Features: The vacuum degree of S3 is 0.6-0.67Pa.

7. A smelting process for a high temperature resistant alloy according to claim 1, Features: The quenching temperature is 530-560°C and the time is 10-15 minutes.

8. A smelting process for a high temperature resistant alloy according to claim 1, Features: The heat treatment temperature is 180-220°C and the time is 10-15h.