CN114231855B - Preparation method of arc fuse of ODS steel - Google Patents
Preparation method of arc fuse of ODS steel Download PDFInfo
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Abstract
The invention provides an arc fuse preparation method of ODS steel, which is prepared by mixing Fe, cr, W, ti, si and Y 2 O 3 Mechanically alloying the powder by using a planetary ball mill, and adding B 2 O 3 、ZrSiO 4 And TiO 2 Mixing, drying in vacuum drying oven, filling the powder into O-shaped steel tube, rolling tightly with a rolling mill, rough-drawing, fine-drawing to obtain flux-cored wire, performing arc fuse additive manufacturing on the steel substrate by using the flux-cored wire as a consumable electrode, cutting, and polishing. The production efficiency is high, the process cost is low, the prepared ODS steel has uniform reinforced phase distribution, the room-temperature tensile strength sigma b is more than or equal to 1200MPa, the elongation is more than or equal to 15 percent, the tensile strength sigma b is more than or equal to 300MPa at the temperature of 800 ℃, and the ODS steel is similar to the traditional Fe-Cr-W-Ti-Y steel 2 O 3 The system alloy is equivalent. The ODS steel provided by the invention can meet the requirement of batch preparation of materials of nuclear fission fuel cladding tubes and first wall structures of nuclear fusion reactors.
Description
Technical Field
The invention belongs to the technical field of high-temperature alloy, and particularly relates to a preparation method of an ODS steel arc fuse.
Background
The ODS steel has great application potential in the aspect of first wall structural materials of nuclear fusion reactors and is the first choice structural material of supercritical water reactors and lead-cooled fast reactors at present due to the advantages of high thermal conductivity, low thermal expansion coefficient, low irradiation swelling rate, resistance to corrosion of liquid metals such as PbLi, pbBi, na and the like, good high-temperature creep resistance and the like. The excellent high-temperature performance is mainly due to the fact that Y-Ti-O nanoclusters with extremely small size and extremely high distribution density are uniformly dispersed in the matrix. The existing process for preparing the nanocluster-containing ODS steel comprises isostatic pressing, hot extrusion, discharge plasma sintering and the like, although excellent-performance materials can be effectively obtained, the process is complex, the cost is extremely high, the manufacturing efficiency is low, and the huge demand of fourth-generation nuclear reactors on structural materials is difficult to meet.
Therefore, the development of an efficient and low-cost production process for preparing the ODS steel with the performance meeting the requirements is necessary for successfully applying the ODS steel to the nuclear power industry.
Disclosure of Invention
Aiming at the problems, the invention provides a method for preparing ODS steel based on an arc fuse technology, which can realize high-efficiency and low-cost batch preparation of the ODS steel. Meanwhile, si is introduced into the components of the traditional ODS steel to enhance the oxidation resistance, and the high-temperature strength and the irradiation resistance are obviously improved through the composition of the Si and Ti, Y and O atoms in a matrix to form an ultra-micro structure.
The invention is realized by adopting the following technical scheme:
the preparation method of the ODS steel arc fuse is characterized by comprising the following specific steps of:
(1) Mechanical alloying: preparing Fe, cr, W, ti, si and Y2O3 powder into mixed powder according to the mass percentage: cr is more than or equal to 9 percent and less than or equal to 25 percent, W is more than or equal to 0 percent and less than or equal to 5 percent, ti is more than or equal to 0.1 percent and less than or equal to 1.0 percent, si is more than or equal to 0.1 percent and less than or equal to 5.0 percent, and Y is more than or equal to 0.1 percent and less than or equal to 5.0 percent 2 O 3 The weight percentage of the mixed powder is less than or equal to 1.0 percent, the balance is Fe, the mixed powder is mechanically alloyed by a planetary ball mill, the ball milling time is 10-100 h, the ball-material ratio is 7:1-30, the ball milling speed is 200-500 rpm, and high-purity argon is adopted for protection in the ball milling process;
(2) Preparing medicinal powder: the alloy powder prepared by the mechanical alloying and B 2 O 3 ,ZrSiO 4 And TiO 2 Mixing uniformly on a planet ball mill, adding B 2 O 3 ,ZrSiO 4 And TiO 2 The alloy powder comprises the following components in percentage by mass: b is more than or equal to 0.1 percent 2 O 3 ≤0.8％、0.5％≤ZrSiO 4 ≤1.0％、0.2％≤TiO 2 Less than or equal to 1.0 percent; the ball milling time is 0.5-10 h, the ball-to-material ratio is 5:1-10, the ball milling speed is 50-300 rpm, and the ball milling medium is absolute ethyl alcohol;
(3) And (3) drying: drying the ball-milled medicinal powder in a vacuum drying oven at the temperature of 60-120 ℃ for 0.5-10 h, wherein the vacuum degree is not higher than 1Pa;
(4) Forming a welding wire: filling the dried medicinal powder into an O-shaped steel pipe, tightly rolling by using a rolling mill, and roughly drawing and finely drawing to prepare a flux-cored wire with the diameter of a welding core being 0.5-3 mm;
(5) Arc fuse additive manufacturing: performing arc fuse additive manufacturing on the steel substrate by using the welding wire as a consumable electrode, wherein Ar-CO is adopted in the arc fuse implementation process 2 Protection with mixed gas of CO 2 20 to 25vol percent and the flow rate is 2.0 to 3.0L/min; the surfacing current is 200-300A, the voltage is 30-35V, the wire feeding speed of the flux-cored wire is 2-2.4 m/min, and the moving speed of a welding gun is 35-45 cm/min;
(6) And (3) post-treatment: cutting and separating the substrate from the ODS steel prepared by the arc fuse additive manufacturing,
and grinding the cut surface to obtain the ODS steel.
The drug core is added with B 2 O 3 、ZrSiO 4 And TiO 2 The electric arc welding method can effectively enhance the stability of the electric arc and adjust the viscosity of the molten slag, thereby improving the toughness of welding structures and beautifying the appearance of the formed product. By adopting the arc fuse additive manufacturing process, the ODS steel with excellent performance can be obtained, and meanwhile, the manufacturing efficiency is high, the process is simple, and the cost is low.
Further, the prepared ODS steel consists of a matrix and a disperse phase, wherein the volume fraction of the disperse phase is 0.1-5%.
Furthermore, the prepared ODS steel matrix is a ferrite structure, and the average grain size is 0.5-20 μm.
Furthermore, the disperse phase in the prepared ODS steel is a phase or microstructure composed of Ti, si, Y and O atoms in any atomic stoichiometric ratio, and the average size is 1-20 nm.
Furthermore, the prepared ODS steel has Ti, si, Y and O composition phases or microstructures in any atomic stoichiometric ratio, and the high-temperature strength and creep resistance of the traditional ODS steel can be greatly improved.
The preparation method of the invention adds Si, so that the ODS steel can obtain a complex microstructure, and simultaneously, the oxidation resistance of the material in the preparation process is improved.
The arc fuse process provided by the invention has high production efficiency and low cost, the prepared ODS steel has uniformly distributed strengthening phases, the room-temperature tensile strength sigma b is more than or equal to 1200MPa, the elongation is more than or equal to 15%, the tensile strength sigma b is more than or equal to 300MPa at the temperature of 800 ℃, and the prepared ODS steel is similar to the traditional Fe-Cr-W-Ti-Y process 2 O 3 The system alloy is equivalent. Therefore, the invention can meet the requirement of batch preparation of the nuclear fission fuel cladding tube and the first wall structure material of the nuclear fusion reactor.
Drawings
FIG. 1 is a TEM image of an ODS alloy prepared in example 3 of the present invention.
FIG. 2 is a diagram showing the analysis of the composition of nanophase A in FIG. 1 for preparing an ODS alloy according to example 3 of the present invention.
FIG. 3 is a diagram showing the analysis of the B composition of the nanophase shown in FIG. 1 for preparing an ODS alloy according to example 3 of the present invention.
Detailed Description
The present invention will be further described with reference to examples.
Example 1:
(1) Mixing Fe, cr, ti, si and Y 2 O 3 The powder is calculated by the mass fraction of 90.7% Fe, 9% Cr, 0.1% Ti, 0.1% Si, 0.1% Y 2 O 3 Preparing mixed powder, then placing the mixed powder in a planetary ball mill for mechanical alloying, wherein the ball milling time is 10 hours, the ball-material ratio is 7:1, the ball milling rotation speed is 200rpm, and high-purity argon is adopted for protection in the ball milling process;
(2) Prepared by mechanical alloyingAlloy powder and B 2 O 3 、ZrSiO 4 And TiO 2 Mixing uniformly on a planet ball mill, adding B 2 O 3 、ZrSiO 4 And TiO 2 2 The alloy powder comprises the following components in percentage by mass: 0.1% of 2 O 3 、0.5％ZrSiO 4 、0.2％TiO 2 (ii) a The ball milling time is 0.5h, the ball-to-material ratio is 5:1, the ball milling rotating speed is 50rpm, and the ball milling medium is absolute ethyl alcohol.
(3) Drying the ball-milled medicinal powder in a vacuum drying oven at 60 ℃ for 0.5h, wherein the vacuum degree is not higher than 1Pa;
(4) Filling the dried medicinal powder into an O-shaped low-carbon steel pipe, tightly rolling by using a rolling mill, and roughly drawing and finely drawing to prepare a flux-cored wire with the diameter of a welding core being 0.5mm;
(5) Performing arc fuse additive manufacturing on the steel substrate by using the welding wire as a consumable electrode, wherein Ar-CO is adopted in the arc fuse implementation process 2 Protection with mixed gas of CO 2 20vol% and a flow rate of 2.0L/min; the surfacing current is 200A, the voltage is 30V, the wire feeding speed of the flux-cored wire is 2m/min, and the moving speed of a welding gun is 35cm/min;
(6) And (3) post-treatment: the substrate was cut and separated from the ODS steel prepared by arc fuse additive manufacturing, and the cut surface was polished to obtain ODS steel, the properties of which are detailed in table 1.
Example 2:
(1) By weight percent, 63.6% Fe, 25% Cr, 5.0% W, 0.4% Ti, 5.0% Si, 1.0% Y 2 O 3 Preparing mixed powder, then placing the mixed powder in a planetary ball mill for mechanical alloying, wherein the ball milling time is 100 hours, the ball-material ratio is 30;
(2) The alloy powder prepared by the mechanical alloying and B 2 O 3 、ZrSiO 4 And TiO 2 Mixing uniformly on a planet ball mill. Addition of B 2 O 3 、ZrSiO 4 And TiO 2 The alloy powder comprises the following components in percentage by mass: 0.5% of 2 O 3 、1.0％ZrSiO 4 、1.0％TiO 2 (ii) a The ball milling time is 10h, the ball material ratio is 10, the ball milling speed is 300rpm, and the ball milling medium is absolute ethyl alcohol;
(3) Drying the ball-milled medicinal powder in a vacuum drying oven at 120 ℃ for 10h, wherein the vacuum degree is not higher than 1Pa;
(4) Filling the dried medicinal powder into an O-shaped low-carbon steel pipe, tightly rolling by using a rolling mill, and roughly drawing and finely drawing to prepare a flux-cored wire with the diameter of a welding core being 3mm;
(5) Performing arc fuse additive manufacturing on the steel substrate by using the welding wire as a consumable electrode, wherein Ar-CO is adopted in the arc fuse implementation process 2 Protection with mixed gas of CO 2 25vol%, with a flow rate of 3.0L/min; the surfacing current is 300A, the voltage is 35V, the wire feeding speed of the flux-cored wire is 2.4m/min, and the moving speed of a welding gun is 45cm/min;
(6) And (3) post-treatment: the substrate was cut and separated from the ODS steel prepared by arc fuse additive manufacturing, and the cut surface was polished to obtain ODS steel, the properties of which are detailed in table 1.
Example 3:
(1) 75.7% by mass of Fe, cr, W, ti, si and Y2O3 powder, fe, 18% by weight, 2.0% by weight of W, 1.0% by weight of Ti, 3.0% by weight of Si, 0.3% by weight of Y 2 O 3 Preparing mixed powder, then placing the mixed powder in a planetary ball mill for mechanical alloying, wherein the ball milling time is 100 hours, the ball-material ratio is 20:1, the ball milling speed is 300rpm, and high-purity argon is adopted for protection in the ball milling process;
(2) Alloy powder B prepared by mechanical alloying 2 O 3 、ZrSiO 4 And TiO 2 2 Mixing uniformly on a planet ball mill, adding B 2 O 3 、ZrSiO 4 And TiO 2 The alloy powder comprises the following components in percentage by mass: 0.7% of 2 O 3 、0.8％ZrSiO 4 、1.0％TiO 2 (ii) a The ball milling time is 2h, the ball-to-material ratio is 7:1, the ball milling rotating speed is 200rpm, and the ball milling medium is absolute ethyl alcohol;
(3) Drying the ball-milled medicinal powder in a vacuum drying oven at 90 ℃ for 3h, wherein the vacuum degree is not higher than 1Pa;
(4) Filling the dried medicinal powder into an O-shaped low-carbon steel pipe, tightly rolling by using a rolling mill, and roughly drawing and finely drawing to prepare a flux-cored wire with the diameter of 1.5mm;
(5) Performing arc fuse additive manufacturing on the steel substrate by using the welding wire as a consumable electrode, wherein Ar-CO is adopted in the arc fuse implementation process 2 Protection with mixed gas of CO 2 At 23vol%, the flow rate was 2.8L/min; surfacing current is 260A, voltage is 33V, wire feeding speed of the flux-cored wire is 2.2m/min, and moving speed of a welding gun is 40cm/min;
(6) And (3) post-treatment: the substrate was cut and separated from the ODS steel prepared by arc fuse additive manufacturing, and the cut surface was ground to obtain the ODS steel, the performance details of which are shown in table 1. A TEM image of the ODS steel is shown in FIG. 1, and a nanophase composition analysis of the ODS steel is shown in FIGS. 2 and 3.
Example 4:
(1) By weight percent, 76.7% of Fe, 16% of Cr, 3.0% of W, 0.5% of Ti, 3.0% of Si, 0.8% of Y 2 O 3 Preparing mixed powder, then placing the mixed powder in a planetary ball mill for mechanical alloying, wherein the ball milling time is 100h, the ball-material ratio is 25:1, the ball milling rotation speed is 320rpm, and high-purity argon is adopted for protection in the ball milling process;
(2) The alloy powder prepared by the mechanical alloying and B 2 O 3 、ZrSiO 4 And TiO 2 Mixing uniformly on a planet ball mill, adding B 2 O 3 、ZrSiO 4 And TiO 2 The alloy powder comprises the following components in percentage by mass: 0.65% of 2 O 3 、0.3％ZrSiO 4 、0.62％TiO 2 (ii) a The ball milling time is 8h, the ball-material ratio is 8:1, the ball milling rotating speed is 200rpm, and the ball milling medium is absolute ethyl alcohol.
(3) Drying the ball-milled medicinal powder in a vacuum drying oven at 95 ℃ for 8h, wherein the vacuum degree is not higher than 1Pa.
(4) And filling the dried medicinal powder into an O-shaped low-carbon steel pipe, tightly rolling by using a rolling mill, and roughly drawing and finely drawing to prepare a flux-cored wire with the diameter of 1.8mm.
(5) Performing arc fuse additive manufacturing on the steel substrate by using the welding wire as a consumable electrode, wherein Ar-CO is adopted in the arc fuse implementation process 2 Protection with mixed gas of CO 2 22vol% with a flow rate of 2.9L/min; the surfacing current is 275A, the voltage is 34V, the wire feeding speed of the flux-cored wire is selected to be 2.3m/min, and the moving speed of a welding gun is 42cm/min;
(6) And (3) post-treatment: the substrate was cut and separated from the ODS steel prepared by arc fuse additive manufacturing, and the cut surface was polished to obtain ODS steel, the properties of which are detailed in table 1.
Example 5:
(1) 80.6% of Fe, 14% of Cr, 3.0% of W, 0.4% of Ti, 1.5% of Si, 0.5% of Y 2 O 3 Preparing mixed powder, then placing the mixed powder in a planetary ball mill for mechanical alloying, wherein the ball milling time is 100 hours, the ball-material ratio is 20, the ball milling rotation speed is 350rpm, and high-purity argon is adopted for protection in the ball milling process;
(2) The alloy powder prepared by the mechanical alloying and B 2 O 3 、ZrSiO 4 And TiO 2 2 Mixing uniformly on a planet ball mill, adding B 2 O 3 、ZrSiO 4 And TiO 2 2 The alloy powder comprises the following components in percentage by mass: 0.8% of 2 O 3 、0.5％ZrSiO 4 、0.6％TiO 2 (ii) a The ball milling time is 6h, the ball-material ratio is 8:1, the ball milling rotating speed is 220rpm, and the ball milling medium is absolute ethyl alcohol;
(3) Drying the ball-milled medicinal powder in a vacuum drying oven at 85 ℃ for 4h, wherein the vacuum degree is not higher than 1Pa;
(4) Filling the dried medicinal powder into an O-shaped low-carbon steel pipe, tightly rolling by using a rolling mill, and roughly drawing and finely drawing to prepare a flux-cored wire with the diameter of 2.0mm;
(5) Performing arc fuse additive manufacturing on the steel substrate by using the welding wire as a consumable electrode, wherein Ar-CO is adopted in the arc fuse implementation process 2 Protection with mixed gas of CO 2 At 24vol%, the flow rate was 2.5L/min; the surfacing current is 280A, the voltageThe voltage is 32V, the wire feeding speed of the flux-cored wire is 2.1m/min, and the moving speed of a welding gun is 45cm/min;
(6) And (3) post-treatment: the substrate was cut and separated from the ODS steel prepared by arc fuse additive manufacturing, and the cut surface was polished to obtain ODS steel, the properties of which are detailed in table 1.
TABLE 1 mechanical properties of the examples
Claims (3)
1. The preparation method of the arc fuse of ODS steel is characterized by comprising the following specific steps of:
(1) Mechanical alloying: mixing Fe, cr, W, ti, si and Y 2 O 3 The powder is prepared into mixed powder according to the mass percentage: cr is more than or equal to 14 percent and less than or equal to 25 percent, W is more than or equal to 3 percent and less than or equal to 5 percent, ti is more than or equal to 0.5 percent and less than or equal to 1.0 percent, si is more than or equal to 1.5 percent and less than or equal to 5.0 percent, Y is more than or equal to 0.5 percent and less than or equal to 5 2 O 3 The weight percentage of the iron-based composite material is less than or equal to 1.0%, and the balance of Fe, the mixed powder is subjected to mechanical alloying by adopting a planetary ball mill, the ball milling time is 10 to 100h, the ball-feed ratio is 7;
(2) Preparing medicinal powder: the alloy powder prepared by the mechanical alloying and B 2 O 3 、ZrSiO 4 And TiO 2 Mixing uniformly on a planet ball mill, adding B 2 O 3 、ZrSiO 4 And TiO 2 The alloy powder comprises the following components in percentage by mass: b is more than or equal to 0.1 percent 2 O 3 ≤0.8%、0.5%≤ZrSiO 4 ≤1.0%、0.2%≤ TiO 2 Less than or equal to 1.0 percent; the ball milling time is 0.5 to 10 hours, the ball-material ratio is 5 to 1, the ball milling rotation speed is 50 to 300rpm, and the ball milling medium is absolute ethyl alcohol;
(3) And (3) drying: drying the ball-milled medicinal powder in a vacuum drying oven at the temperature of 60-120 ℃ for 0.5-10 h, wherein the vacuum degree is not higher than 1Pa;
(4) Forming a welding wire: filling the dried medicinal powder into an O-shaped steel pipe, tightly rolling by using a rolling mill, and carrying out rough drawing and fine drawing to prepare a flux-cored wire with the diameter of 0.5 to 3mm;
(5) Arc fuse additive manufacturing: performing arc fuse additive manufacturing on the steel substrate by using the welding wire as a consumable electrode, wherein Ar-CO is adopted in the arc fuse implementation process 2 Protection with mixed gas of CO 2 The flow rate is 20 to 25vol% and the flow rate is 2.0 to 3.0L/min; the surfacing current is 200 to 300A, the voltage is 30 to 35V, the wire feeding speed of the flux-cored wire is 2 to 2.4m/min, and the moving speed of a welding gun is 35 to 45cm/min;
(6) And (3) post-treatment: cutting and separating the substrate and the ODS steel prepared by the arc fuse additive manufacturing, and grinding a cutting surface to obtain the ODS steel; the reinforced phase of the ODS steel is uniformly distributed, and the room-temperature tensile strength sigma is b More than or equal to 1200MPa, elongation more than or equal to 15 percent and tensile strength sigma at 800 DEG C b ≥300MPa；
The dispersed phase in the prepared ODS steel is a phase or microstructure composed of Ti, si, Y and O atoms in any atomic stoichiometric ratio, and the average size is 1-20nm.
2. The ODS steel arc-fuse manufacturing method of claim 1, characterized in that the manufactured ODS steel consists of a matrix and a dispersed phase, wherein the dispersed phase accounts for 0.1-5% by volume.
3. The ODS steel arc-fuse manufacturing method of claim 2, characterized in that the ODS steel matrix manufactured is of ferritic structure, with an average grain size of 0.5 to 20 μm.
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