CN113926856B - Method for preparing dispersion-strengthened metal material in batch - Google Patents

Method for preparing dispersion-strengthened metal material in batch Download PDF

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CN113926856B
CN113926856B CN202110992691.8A CN202110992691A CN113926856B CN 113926856 B CN113926856 B CN 113926856B CN 202110992691 A CN202110992691 A CN 202110992691A CN 113926856 B CN113926856 B CN 113926856B
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dispersion
metal
coating
treatment
foil
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CN113926856A (en
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谌继明
郑鹏飞
张归航
李峰
钱伟
魏然
车通
刘星
张明
徐莉莎
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Southwestern Institute of Physics
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Southwestern Institute of Physics
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21B—ROLLING OF METAL
    • B21B1/00—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations
    • B21B1/40—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations for rolling foils which present special problems, e.g. because of thinness
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C17/00—Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls
    • B02C17/10—Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls with one or a few disintegrating members arranged in the container
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B08—CLEANING
    • B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
    • B08B3/04—Cleaning involving contact with liquid
    • B08B3/08—Cleaning involving contact with liquid the liquid having chemical or dissolving effect
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B08—CLEANING
    • B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
    • B08B3/04—Cleaning involving contact with liquid
    • B08B3/10—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration
    • B08B3/12—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration by sonic or ultrasonic vibrations
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21B—ROLLING OF METAL
    • B21B37/00—Control devices or methods specially adapted for metal-rolling mills or the work produced thereby
    • B21B37/16—Control of thickness, width, diameter or other transverse dimensions
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21B—ROLLING OF METAL
    • B21B37/00—Control devices or methods specially adapted for metal-rolling mills or the work produced thereby
    • B21B37/56—Elongation control
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21B—ROLLING OF METAL
    • B21B37/00—Control devices or methods specially adapted for metal-rolling mills or the work produced thereby
    • B21B37/74—Temperature control, e.g. by cooling or heating the rolls or the product
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21B—ROLLING OF METAL
    • B21B45/00—Devices for surface or other treatment of work, specially combined with or arranged in, or specially adapted for use in connection with, metal-rolling mills
    • B21B45/02—Devices for surface or other treatment of work, specially combined with or arranged in, or specially adapted for use in connection with, metal-rolling mills for lubricating, cooling, or cleaning
    • B21B45/0269—Cleaning
    • B21B45/0272—Cleaning compositions
    • 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
    • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/26—Methods of annealing
    • C21D1/30—Stress-relieving
    • 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
    • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/74—Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material
    • 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
    • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/74—Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material
    • C21D1/773—Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material under reduced pressure or vacuum
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14—Metallic material, boron or silicon
    • C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14—Metallic material, boron or silicon
    • C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
    • C23C14/165—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic sputtering
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C24/00—Coating starting from inorganic powder
    • C23C24/02—Coating starting from inorganic powder by application of pressure only
    • C23C24/04—Impact or kinetic deposition of particles
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E30/00—Energy generation of nuclear origin
    • Y02E30/10—Nuclear fusion reactors

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Abstract

The invention belongs to the field of material preparation, and particularly discloses a method for preparing a dispersion-strengthened metal material in batches, which comprises the following steps: cleaning the metal surface and then carrying out repeated cold rolling treatment; carrying out ultrasonic cleaning on the metal foil/plate; then, carrying out stress relief annealing treatment on the metal foil/plate under vacuum; coating the metal foil/plate: coating a dispersed phase raw material on the metal foil/plate to obtain a dispersed phase raw material coating; multi-pass hot rolling treatment: carrying out lamination and hot rolling pretreatment on the metal foil/plate; then carrying out multi-pass circulating 'lamination + vacuum hot rolling' treatment; densification treatment: and (3) placing the laminated metal foil into a mold, placing the laminated metal foil into a sheath for hot isostatic pressing treatment, and performing aging heat treatment to obtain the dispersion-strengthened metal material. The preparation method has simple process, high efficiency and good repeatability, and the quantity and uniform distribution of dispersed phase particles can be effectively regulated and controlled.

Description

Method for preparing dispersion-strengthened metal material in batches
Technical Field
The invention belongs to the field of material preparation, and particularly relates to a method for preparing a dispersion-strengthened metal material in batches.
Background
With the continuous development of science and technology, the service environment of the material is more and more complex and harsh, and the requirements on the performance of the material are higher and higher. For example, structural materials of fusion reactors, especially structural materials of cladding/first wall, are in severe environment, and require materials with excellent characteristics of low activation, high temperature strength, radiation swelling and radiation damage resistance, high thermal conductivity, low thermal expansion coefficient, good creep resistance, good processability, and coolant corrosion resistance, so that conventional materials are increasingly unable to meet the requirements of such characteristics, and materials with better research and design performance and capable of being produced in batch are urgently needed.
The oxide/carbide/nitride dispersion strengthening phase generally has higher thermal stability and hardness, and the dispersion strengthening alloy material suitable for different fields can be prepared by controlling the density, the size and the distribution of the oxide/carbide/nitride dispersion strengthening phase in a matrix material. The addition of the dispersed phase can not only improve the strength of the material, but also reduce the grain growth rate of the material at high temperature, so the dispersed phase is widely applied to the industrial fields of nuclear energy, electronics, automobiles, aerospace and the like.
The preparation method of the prior dispersion strengthening alloy material mainly comprises a smelting method and a mechanical alloying method. The smelting method is to put the matrix and the dispersed phase raw materials together in a desired ratio, melt them by a suitable method, and then cast the melt. However, if the dispersed phase starting material is nano-sized ceramic particles, it is not easy to uniformly disperse it in the metal matrix melt. Specifically, the particles tend to be clustered and unevenly distributed, and it is difficult to achieve homogenization even by vigorous stirring and ultrasonic dispersion. However, if the raw material of the dispersed phase is pure metal, for example, yttrium is doped in the smelting process, and then the subsequent internal oxidation is performed to generate the dispersed phase, the problem of uncontrollable yttrium content, such as ablation or low solubility, still cannot play an effective reinforcing role is often encountered. The more effective method is to mechanically grind the mixture of metal particles and dispersed phase raw materials in a powder metallurgy mode, but the method also has the problems of serious cold welding phenomenon, low powder forming rate and high content of introduced impurities; the quality and the efficiency are to be improved.
Therefore, it is highly desirable to develop a method for preparing a dispersion-strengthened alloy material with high quality that can be mass-produced.
Disclosure of Invention
The invention aims to provide a method for preparing a dispersion-strengthened metal material in batch, which has the advantages of simple process, high efficiency, good repeatability and effective regulation and control of the quantity and uniform distribution of dispersed phase particles.
The technical scheme for realizing the purpose of the invention is as follows:
a method for batch production of a dispersion strengthened metallic material, the method comprising the steps of:
step (1), processing metal foil/plate: cleaning the metal surface, and repeatedly cold rolling the metal surface after cleaning until the metal surface is processed into a metal foil/plate with the thickness of 0.1-10 mm; carrying out ultrasonic cleaning on the metal foil/plate by using an organic solvent to remove oil stains; then, carrying out stress relief annealing treatment on the metal foil/plate under vacuum;
step (2), metal foil/plate coating: performing dispersed phase raw material film coating on the metal foil/plate subjected to the stress relief annealing treatment to obtain a dispersed phase raw material coating, wherein the thickness of the dispersed phase raw material coating is 100nm-30 mu m;
step (3), multi-pass hot rolling treatment: laminating and hot rolling the metal foil/plate plated with the dispersed phase raw material film to obtain long foil with the thickness of 0.02-0.5 mm; then, carrying out multi-pass circulating 'lamination + vacuum hot rolling' treatment on the pretreated long foil until the thickness of the single-layer metal foil is 0.1-1 mu m;
step (4), densification treatment: and (3) placing the laminated metal foil subjected to the multi-pass hot rolling treatment into a die, placing the die into a sheath for hot isostatic pressing treatment, releasing pressure and cooling after the treatment, and performing aging heat treatment to obtain the dispersion-strengthened metal material.
The repeated cold rolling treatment after the cleaning treatment in the step (1) is specifically as follows: cold rolling the metal block, annealing the cold-rolled and hardened material in the thinning process under the protection of vacuum or inert atmosphere, continuously cold rolling after annealing, then annealing for many times, and repeatedly circulating until the metal block is processed into a metal foil/plate with the thickness of 0.1-10 mm.
The speed of cold rolling treatment in the step (1) is 0.5-5 m/min, the reduction amount of each cold rolling is 0.02-0.2mm, and the vacuum degree of vacuum stress relief annealing treatment is 1 multiplied by 10 -6 Pa～1×10 -3 Pa, the annealing temperature is 300-1000 ℃ according to different melting points of the material, and the number of times of repeated cold rolling is 5-100 times according to different thicknesses of the material.
The organic solvent in the step (1) is acetone or ethanol.
The ultrasonic frequency of the ultrasonic cleaning in the step (1) is 20-80kHz, and the time is 5-30min each time.
In the step (1), stress relief annealing treatment is carried out after ultrasonic cleaning, and the vacuum degree is 1 multiplied by 10 -6 ～1×10 -3 Pa, the temperature is 300-1000 ℃, and the time is 1-3 h.
The method for coating the dispersed phase raw material in the step (2) comprises the following steps: PVD coating, ion sputtering coating, cold spray coating, electrochemical coating, diffusion bonding, and the like.
The parameters of the PVD coating for the dispersed phase raw material coating in the step (2) are as follows: introducing high-purity argon, and maintaining the vacuum degree at 1 × 10 -2 Pa or so, pulse bias: 200-300V, duty ratio of 20-50%, arc current of 10-30A, and film plating time of 5-10 minutes.
The parameters of the ion sputtering coating for performing the dispersed phase raw material coating in the step (2) are as follows: background vacuum degree of 2X 10 -4 Pa, heating the base foil to 150 deg.C, starting to perform diffusion phase metal plating on the base foil with argon partial pressure of 0.05Pa, and sputtering each fixed surface for 10min to obtain a metal plating layer with thickness of 1 μm and uniform components and thickness.
The parameters of the dispersed phase raw material coating by adopting cold spraying coating in the step (2) are as follows: using 10 μm dispersoid phase metal powder as cold spraying raw material, performing roll-to-roll cold spraying of the base material foil at a speed of 0.1kg/h in an argon protective atmosphere, wherein the rotation speed of the foil roll is 0.5m/s, thereby uniformly coating a layer of cold spraying film of the dispersoid phase metal element with the thickness of 100nm on the surface of the base material foil.
The parameters of the dispersed phase raw material coating by adopting the electrochemical coating in the step (2) are as follows: preparing the salt containing the element to be plated into a 20-80% solution at the temperature of 0-20 ℃, and electrifying for 1-5 minutes at the voltage of 10-20V and the current of 10-30 mA.
The parameters of the diffusion phase raw material coating by adopting the diffusion connection coating in the step (2) are as follows: stacking the dispersed phase raw material metal foil with the thickness of 0.01-0.1mm and the reinforced metal foil/plate at intervals, and performing hot pressing or hot isostatic pressing at the temperature of 80-180MPa and 900-1200 ℃ for 1-3 hours, wherein the vacuum degree in a hot pressing furnace or in a hot isostatic pressing package is more than 1 x 10 -2 Pa。
The step (3) specifically comprises:
step (3.1), hot rolling pretreatment: cutting or folding the metal foil coated with the dispersed phase raw material into equal-length sections, and then carrying out hot rolling pretreatment to process the metal foil into long foil with the thickness of 0.02-0.5 mm;
step (3.2), hot rolling treatment: carrying out ultrasonic cleaning on the long foil at 20-80kHz by using an organic solvent, carrying out thermal stress removal annealing treatment under vacuum, cutting and folding the long foil into equal-length sections again after annealing treatment, and carrying out hot rolling treatment again;
step (3.3), multi-pass hot rolling treatment: the lamination and hot rolling processes are cycled until the thickness of the single-layer metal foil is 0.1-1 μm.
The hot rolling pretreatment in the step (3.1) has a vacuum degree of 1 x 10 -6 ～1×10 -3 Pa, the temperature is 300-1000 ℃ according to different materials, and the thickness is reduced by 5-30% in each hot rolling.
The solvent for ultrasonic cleaning in the step (3.2) is acetone, and the ultrasonic cleaning time is 5-30 minutes.
The vacuum degree of the thermal stress annealing treatment in the step (3.2) is 1 multiplied by 10 -6 ～1×10 -3 Pa, the annealing temperature is 300-1000 ℃ according to different melting points of the materials.
The hot rolling treatment in the step (3.2) is carried out, and the vacuum degree is 1 multiplied by 10 -6 ～1×10 -3 Pa, the temperature is selected to be 300-1000 ℃ according to different materials, and the thickness is reduced by 5-30% in each hot rolling.
And (4) in the step (4), the hot isostatic pressing temperature is 900-1200 ℃, the pressure is 80-180MPa, and the heat preservation and pressure maintaining time is 1-3 h.
The aging heat treatment in the step (4) is carried out, and the vacuum degree is 1 multiplied by 10 -6 Pa～1×10 -3 Pa, temperature of 600 ℃ and 1400 ℃, and time of 1-20 h.
The invention has the beneficial technical effects that:
1. the method for preparing the dispersion-strengthened metal material in batches utilizes certain ductility of base metal to process the base metal into metal foil, takes the dispersed phase as a target material, plates the metal foil surface by adopting the modes of PVD, CVD, electrochemical coating, cold spraying, ion sputtering and the like, and forms a second phase with controllable content and dispersion distribution in the base metal by adjusting the parameters of the coating such as thickness, rate and the like and subsequent rolling and heat treatment conditions; the method can not only avoid the problems of non-uniform components of the smelting method (such as component segregation in partial smelting materials reaches more than 90 percent), and limited solubility by thermodynamic conditions (such as yttrium content in smelting steel is only 10-100 ppm), but also overcome the difficulties that the powder metallurgy method has overhigh cost, long period (such as one month and one furnace), more impurities (such as oxygen content reaches more than 1 percent), and can not realize batch production (such as laboratory is only hundred grams and enterprise production is only 10 kilograms).
2. The method for preparing the dispersion-strengthened metal material in batches provided by the invention realizes large-scale batch production of the dispersion-strengthened metal material above hundred kilograms by combining rolling, stress relief annealing, spraying and hot isostatic pressing.
3. The method for preparing the dispersion-strengthened metal material in batches adopts the modes of spraying, sputtering and the like to realize the addition of the dispersed phase raw material, and the size (3-10nm) and the number (1 multiplied by 10) of the dispersed phase particles 22 -1×10 25 n/m 3 ) And uniform distribution (density deviation below 10%) can be effectively regulated and controlled.
4. The dispersion-strengthened metal material prepared by the method for preparing the dispersion-strengthened metal material in batches has the advantages of high efficiency (one week in one furnace), low impurity content (the content of non-compound oxygen is less than 300ppm), better performance (the strength of dispersion-strengthened steel is more than 1GPa, and the elongation is more than 10%) and the like.
Detailed Description
The present invention will be described in further detail with reference to examples.
Example 1
Grinding and polishing the surface of a 99.95 percent vanadium rod or vanadium plate, then repeatedly performing cold rolling at a cold rolling speed of 2 m/min, continuously performing cold rolling on a 10mm vanadium plate for 95 times with the thickness of about 0.1mm each time to obtain a 0.5mm thick vanadium plate, performing cold rolling work hardening to obtain a hardness of more than 200Hv, and performing stress relief annealing treatment on the vanadium plate in vacuum with the vacuum degree of 1 multiplied by 10 -4 Pa, 1000 ℃ and 3 hours, continuously cold rolling at the speed of 0.5 m/min after annealing treatment, reducing the thickness of about 0.05mm each time, and continuously performing 9 times until the vanadium foil with the thickness of 0.05mm is processed.
And then, putting the vanadium foil into acetone for ultrasonic cleaning of 20kHz for 4 times, 5min each time, replacing fresh acetone each time, wiping with ethanol, and drying with cold air to obtain the vanadium foil for later use.
Vanadium foil is placed in a vacuum degree of 1X 10 -6 ～1×10 -4 And (4) performing stress relief annealing under the condition of Pa, wherein the temperature is 1000 ℃, and the time is 1 h.
Placing the prepared vanadium foil on PVD coating equipment, taking dispersed phase yttrium metal as a target material, introducing high-purity argon, and keeping the vacuum degree at 1 × 10 -2 Pa, adjusting the test parameters to 200V of pulse bias, 10A of arc current and 20% of duty ratio, and starting to perform the film coating operation of the dispersed phase metal yttrium for 5 minutes to obtain an yttrium coating with the thickness of 100nm and uniform components and thickness.
The yttrium-coated vanadium foil was cut and multiply folded into 2mm thick long sections, followed by 1X 10 -6 Pa-1×10 -4 Hot rolling under the condition of Pa and under the protection of vacuum or inert gas Ar, at the temperature of 1000 ℃, and thinning by 0.1mm each time to form a multilayer long foil with the thickness of 0.5 mm.
Then cleaning in acetone under vacuum of 1 × 10 -6 Pa-1×10 -4 Annealing at 1000 deg.C for 1 hr under Pa, re-cutting or multi-folding, and repeating at 1 × 10 -6 Pa-1×10 -4 Hot rolling to 0.1mm under the condition of Pa vacuum and 1000 ℃; the cleaning, stress annealing, cutting or folding and hot rolling are repeatedly carried out for 3 times; and the thickness of the single-layer vanadium foil is reduced by 50 percent by each hot rolling until the thickness of the single-layer vanadium foil is 0.1 mu m.
And cleaning the final hot-rolled vanadium foil by acetone, putting the cleaned vanadium foil into a tungsten steel die, sealing the vanadium foil by using a stainless steel sheath, performing hot isostatic pressing sintering treatment at the temperature of 1200 ℃ under the pressure of 180MPa, and preserving heat and pressure for 3 hours. Cutting and cleaning after molding, and finally passing through a die with the diameter of 1 multiplied by 10 -6 Pa-1×10 -4 Aging heat treatment at 1400 ℃ for 3 hours under Pa vacuum to obtain Y 2 O 3 A dispersion strengthened vanadium material.
Example 2
The surface of a copper bar or a copper plate with the purity of 99.99 percent is ground and polished, and then cold rolling is repeatedly carried out, wherein the cold rolling speed is 5m/min, the copper bar with the diameter of 20mm is continuously subjected to cold rolling for 95 times, and the copper plate with the thickness of 1mm is obtained after the copper bar is reduced by about 0.2mm each time. After cold rolling work hardening, annealing the copper plate in vacuum with the vacuum degree of 1 × 10 based on the judgment that the copper plate is difficult to be re-rolled - 3 Pa, 300 ℃ and 3 hours. Continuously cold rolling after annealing treatment, wherein the cold rolling speed is 2 m/min,cold rolling for reducing the thickness of about 0.1mm each time, and rolling for 8 times until the copper foil with the thickness of 0.2mm is processed.
Then the vacuum degree is 1X 10 -3 Carrying out stress relief annealing under the condition of Pa, wherein the temperature is 300 ℃, and the time is 2 h; and after cooling, putting the copper foil into acetone for cleaning for 30 minutes twice, replacing fresh acetone each time, then flushing with ethanol, and drying with cold air to obtain the copper foil for later use.
Placing the prepared copper foil on an ion sputtering film plating machine, taking dispersed phase metal aluminum as a target material, and performing vacuum treatment under the background vacuum degree of 2 multiplied by 10 -4 And Pa, heating the copper foil to 150 ℃, starting to coat the copper foil with disperse-phase metallic aluminum by adopting argon partial pressure of 0.05Pa, and sputtering each fixed surface for 10 minutes to obtain a metallic aluminum coating with the thickness of 1 mu m and uniform components and thickness.
The aluminum film-plated copper foil is cut or multiply folded into 10 mm-thick long sections, followed by 1X 10 -3 Hot rolling under vacuum or under the protection of inert gas Ar under Pa at 300 deg.C for 13 times, reducing the thickness by 20% each time, and when the thickness reaches about 0.55mm, reducing the thickness by 0.1mm each time for 5 times to obtain long foil with thickness of 0.05 mm.
Cleaning the final hot-rolled composite copper foil by acetone, cutting into equal-length sections, laminating to a thickness which can be accommodated by the mold, putting into a stainless steel mold together, sealing by a pure iron sheath, performing hot isostatic pressing treatment at 900 ℃ and 80MPa, and keeping the temperature and pressure for 1 h. And after the heat preservation and pressure preservation are finished, releasing the pressure, slowly cooling, and then cooling along with the furnace. Obtaining a hot isostatic pressed bulk material, heat treating at 600 ℃ to 1X 10 -3 Vacuum aging heat treatment under Pa for 1 hr to convert Al 2 O 3 Dispersion strengthened copper material.
Example 3
Grinding and polishing the surface of a V-4Cr-4Ti alloy plate with any thickness and 99.9 percent of material components, then repeatedly performing cold rolling for reducing the thickness of about 0.1mm each time at the speed of 2 m/min, after the cold rolling is processed and hardened, enabling the hardness to reach more than 200Hv, performing stress relief annealing treatment on a vanadium plate in vacuum, and enabling the vacuum degree to be 1 multiplied by 10 -4 Pa, 1000 deg.C, 3 hours, annealing treatmentAnd (5) continuously cold rolling, and finally repeatedly cold rolling into a 10mm vanadium alloy plate.
And (3) alternately laminating the vanadium alloy plate and 30-micron-thick dysprosium foil, sealing the vanadium alloy plate and the dysprosium foil in a tungsten steel mold by using a pure iron sheath, performing hot isostatic pressing diffusion connection at the temperature of 1200 ℃ and under the pressure of 180MPa, and preserving heat and pressure for 3 hours.
Then the diffusion-connected composite board is cold-rolled, after the diffusion-connected composite board is hardened to 200Hv, the V-4Cr-4Ti composite board is processed at 1 x 10 -4 And (2) carrying out stress relief annealing heat treatment for 3 hours at the temperature of 1000 ℃ under Pa, continuously cold rolling for 95 times after the annealing treatment, carrying out cold rolling for reducing the thickness of about 0.1mm each time to obtain a vanadium plate with the thickness of 0.5mm, and then carrying out 5 cycles of cold rolling for reducing the thickness of about 0.1mm each time and stress relief annealing until the V-4Cr-4Ti alloy is used for processing a single-layer dysprosium vanadium alloy composite foil with the thickness of 1 mu m. And cleaning the composite foil by acetone for 4 times, then placing the composite foil into a stainless steel sheath, carrying out hot isostatic pressing treatment at 1200 ℃ and under the pressure of 180MPa, and carrying out heat preservation and pressure maintaining for 3 hours. And (4) after the heat preservation and pressure preservation are finished, releasing the pressure, slowly cooling, and then cooling along with the furnace. Obtaining a hot-isostatic-pressed bulk material, passing through a 1X 10 bed -4 Aging heat treatment for 3 hours at 1300 ℃ under Pa vacuum to obtain Dy 2 O 3 The dispersion-strengthened V-4Cr-4Ti alloy material.
Example 4
Purchasing a zirconium foil of 0.1mm thickness and 100mm width, then washing the zirconium metal foil in acetone four times, each time with fresh acetone under 80kHz ultrasonic wave for 5 minutes, wiping with alcohol, and then vacuum degree of 1 × 10 -1 And drying in a vacuum drying oven of Pa to obtain the metal zirconium foil for later use.
And (3) placing the prepared zirconium metal foil in cold spraying equipment for film coating, and performing roll-to-roll cold spraying on the zirconium foil at the speed of 0.1kg/h in the argon protection atmosphere by using 10-micron lanthanum powder as a cold spraying raw material, wherein the rotation speed of the foil roll is 0.5m/s, so that a layer of metal lanthanum cold spraying film with the thickness of 100nm can be uniformly coated on the surface of the zirconium foil.
Subsequently cutting and folding the lanthanum-plated zirconium foil into multiple 10mm thick laminates, separating 20 laminates by tantalum plates, sealing with tungsten steel mold and pure copper sheath, and performing 160MPa temperatureHot isostatic pressing at 800 ℃ for 2 hours. After hot isostatic pressing, the groups of zirconium lanthanum composite foil laminates were removed and subsequently evacuated at a vacuum of 1X 10 -6 Pa～1×10 -4 Pa, at 800 ℃ to thin each set of laminations to 0.1 mm.
Cleaning the thinned zirconium lanthanum composite foil in acetone, and then cutting and multi-folding the zirconium lanthanum composite foil into a lamination with the thickness of 200 mm; and finally, putting the zirconium composite foil lamination into a tungsten steel die and a copper clad sleeve, performing hot isostatic pressing treatment at the temperature of 800 ℃ and under the pressure of 160MPa, and preserving heat and pressure for 2 hours. After the heat preservation and pressure maintenance are finished, pressure is relieved, the block material is slowly cooled and then cooled along with the furnace, the block material after the hot isostatic pressing is obtained, and the block material is processed by 1 multiplied by 10 -4 Heat treatment under Pa vacuum at 900 deg.C for 1 hr to obtain La 2 O 3 A dispersion strengthened zirconium alloy material.
Example 5
In the general process, the yttrium oxide dispersion strengthening V-4Cr-4Ti alloy is prepared by mechanical alloying, and the method for preparing dispersion strengthening metal in batches adopts an innovative process, so that higher preparation efficiency, lower impurity content and more controllable material performance are obtained:
1. through a ball milling process of mechanical alloying, the V powder is subjected to cold welding and wall adhesion in the ball milling process, so that continuous ball milling cannot be performed, the V powder needs to be rotated and stopped at intervals to ensure cooling, and meanwhile, a ball milling tank needs to be opened for many times to strip adhered powder, and then ball milling can be continued to ensure the material yield. In addition, the ball milling tank has limited capacity, and mass production of more than 10 kg is difficult to realize. Generally, the preparation of 500 g of yttrium oxide dispersion-strengthened V-4Cr-4Ti alloy in a laboratory or 10 kg of yttrium oxide dispersion-strengthened V-4Cr-4Ti alloy in a special enterprise needs 2 months. The invention benefits from the exponential processing of lamination thinning, and can realize the preparation of the V-4Cr-4Ti alloy with the dispersion strengthening of the yttrium oxide of nearly 100 kilograms in 1 month.
2. The quantity and the uniform distribution of dispersed phase particles can be effectively regulated and controlled;
through the ball milling process of mechanical alloying, partial aggregation of yttrium element may exist in local areas, and finally, the yttrium element is difficult to remotely diffuse in a material matrix, so that the uniformity and the dispersion of the yttrium element are causedThe density of the dispersed phase fluctuates, and the uniformity of the yttrium content is less than 90 percent. And the typical yttria dispersed phase size>5nm, up to 50nm, density of 10 22 n/m 3 ～10 23 n/m 3 The tensile strength at room temperature is about 800MPa, and the elongation is<10 percent. According to the invention, the yttrium and the vanadium alloy foil are laminated at intervals, and after multi-pass uniform rolling, the yttrium can be uniformly diffused in the extremely thin vanadium alloy layer. The thickness of the coating film is selectable, the thickness of the vanadium alloy raw material foil is also selectable, the rolling times, the heat treatment temperature and the time condition are adjustable, the content and the uniformity of yttrium and the growth of dispersed phase nucleation can be controlled from multiple angles, and the density of yttrium oxide can reach 10 24 n/m 3 The magnitude, the dispersed phase size is adjustable between 3nm and 10nm, and the tensile strength at room temperature can be adjusted>1000MPa, elongation>10％。
3. The dispersion strengthened metal material has low impurity content.
Through the ball milling process of mechanical alloying, because of lacking the milling ball of mainly vanadium-containing alloy material, the WC impurity can be mixed into the carbide milling ball commonly used, and the oxygen content in the powder of ball milling is high, and the ball milling jar needs to be opened many times, and the gaseous impurity will be mixed into again in-process in addition. In the prior art of preparing yttrium oxide dispersion strengthened vanadium alloy by mechanical alloying, the finally measured oxygen content is more than 1 percent. In the invention, alloy bar, plate or foil is used, is a high-purity material, is protected from air in high-temperature treatment, and has short preparation time, so that the mixed oxygen content is extremely low and is generally less than 0.1 percent, the mixed oxygen is absorbed by yttrium to a great extent to form an yttrium oxide dispersed phase, and the oxygen in an amorphous state is less than 300 ppm.
The present invention has been described in detail with reference to the embodiments, but the present invention is not limited to the embodiments, and various changes can be made within the knowledge of those skilled in the art without departing from the gist of the present invention. The prior art can be adopted in the content which is not described in detail in the invention.

Claims (19)

1. A method for preparing a dispersion-strengthened metallic material in batch, the method comprising the steps of:
step (1), processing metal foil/plate: cleaning the metal surface, and repeatedly cold rolling the metal surface after cleaning until the metal surface is processed into a metal foil/plate with the thickness of 0.1-10 mm; carrying out ultrasonic cleaning on the metal foil/plate by using an organic solvent to remove oil stains; then, carrying out stress relief annealing treatment on the metal foil/plate under vacuum;
step (2), metal foil/plate coating: performing dispersion phase raw material film coating on the metal foil/plate after the stress relief annealing treatment to obtain a dispersion phase raw material plating layer, wherein the thickness of the dispersion phase raw material plating layer is 100nm-30 mu m;
step (3), multi-pass hot rolling treatment: laminating and hot rolling the metal foil/plate plated with the dispersed phase raw material film to obtain a long foil with the thickness of 0.02-0.5 mm; then, carrying out multi-pass circulating lamination and vacuum hot rolling treatment on the pretreated long foil until the thickness of the single-layer metal foil is 0.1-1 mu m;
step (4), densification treatment: and (3) placing the laminated metal foil subjected to the multi-pass hot rolling treatment into a die, placing the die into a sheath for hot isostatic pressing treatment, releasing pressure and cooling after the treatment, and performing aging heat treatment to obtain the dispersion-strengthened metal material.
2. The method for batch preparation of the dispersion-strengthened metal material as claimed in claim 1, wherein the repeated cold rolling after the cleaning in step (1) is specifically: and (2) carrying out cold rolling treatment on the metal block, then carrying out vacuum or inert atmosphere protection annealing treatment on the material subjected to cold rolling work hardening in the thinning process, continuing cold rolling after annealing treatment, then carrying out annealing heat treatment again, and repeatedly carrying out multiple cycles until the metal block is processed into a metal foil/plate with the thickness of 0.1-10 mm.
3. The method for preparing the dispersion-strengthened metal material in batches as claimed in claim 2, wherein the speed of the cold rolling treatment in the step (1) is 0.5-5 m/min, the reduction amount of each cold rolling is 0.02-0.2mm, and the vacuum degree of the vacuum stress relief annealing treatment is 1 x 10 -6 Pa～1×10 -3 Pa, the annealing temperature is 300-1000 ℃ according to the different melting points of the materials, and the number of times of repeated cold rolling is 5-100 times according to the different thicknesses of the materials.
4. The method for batch preparation of the dispersion-strengthened metal material as claimed in claim 2, wherein the organic solvent in step (1) is acetone or ethanol.
5. The method for preparing the dispersion-strengthened metal material in batches according to claim 4, wherein the ultrasonic frequency of the ultrasonic cleaning in the step (1) is 20-80kHz, and the time is 5-30min each time.
6. The method for batch preparation of dispersion-strengthened metallic materials as claimed in claim 5, wherein the step (1) is a stress-relief annealing treatment after ultrasonic cleaning with a degree of vacuum of 1 x 10 -6 ～1×10 -3 Pa, the temperature is 300-1000 ℃, and the time is 1-3 h.
7. The method for batch preparation of a dispersion-strengthened metal material according to claim 1, wherein the method for coating the dispersed phase raw material in the step (2) comprises: PVD coating, ion sputtering coating, cold spraying coating, electrochemical coating and diffusion bonding.
8. The method for batch preparation of a dispersion-strengthened metallic material according to claim 7, wherein the parameters of the PVD coating for the coating of the dispersed phase raw material in the step (2) are as follows: introducing high-purity argon, and maintaining the vacuum degree at 1 × 10 -2 Pa, pulse bias: 200-300V, duty ratio of 20-50%, arc current of 10-30A, and coating time of 5-10 min.
9. The method for batch production of a dispersion-strengthened metal material as claimed in claim 7, wherein the step (2) comprises performing dispersion by ion sputteringParameters of phase raw material coating: background vacuum degree of 2X 10 -4 And Pa, heating the base material foil to 150 ℃, starting to coat the base material foil with the dispersed phase metal by adopting argon partial pressure of 0.05Pa, and sputtering each fixed surface for 10min to obtain a metal coating with the thickness of 1 mu m and uniform components and thickness.
10. The method for batch preparation of dispersion-strengthened metallic materials according to claim 7, wherein the parameters of the diffusion phase raw material coating in step (2) by cold spray coating are as follows: using 10 μm dispersoid phase metal powder as cold spraying raw material, performing roll-to-roll cold spraying of the base material foil at a speed of 0.1kg/h in an argon protective atmosphere, wherein the rotation speed of the foil roll is 0.5m/s, thereby uniformly coating a layer of cold spraying film of the dispersoid phase metal element with the thickness of 100nm on the surface of the base material foil.
11. The method according to claim 7, wherein the step (2) comprises performing the dispersion phase raw material coating by electrochemical coating according to the following parameters: preparing the salt containing the plated element into a 20-80% solution at the temperature of 0-20 ℃, and electrifying for 1-5 min at the voltage of 10-20V and the current of 10-30 mA.
12. The method for batch preparation of a dispersion-strengthened metal material according to claim 7, wherein the step (2) comprises the following steps of performing the coating of the dispersed phase raw material by using diffusion bonding coating: stacking the dispersed phase raw material metal foil with the thickness of 0.01-0.1mm and the reinforced metal foil/plate at intervals in a multi-layer mode, and carrying out hot pressing or hot isostatic pressing at the temperature of 900-1200 ℃ under the pressure of 80-180MPa for 1-3h, wherein the vacuum degree in a hot pressing furnace or in a hot isostatic pressing package is more than 1 x 10 -2 Pa。
13. The method for batch preparation of the dispersion-strengthened metal material as claimed in claim 1, wherein the step (3) comprises:
step (3.1), hot rolling pretreatment: cutting or folding the metal foil coated with the dispersed phase raw material into equal-length sections, and then carrying out hot rolling pretreatment to process the metal foil into long foil with the thickness of 0.02-0.5 mm;
step (3.2), hot rolling treatment: carrying out ultrasonic cleaning on the long foil by using an organic solvent at 20-80kHz, carrying out thermal stress removal annealing treatment under vacuum, cutting and folding the long foil into equal-length sections again after annealing treatment, and carrying out hot rolling treatment again;
step (3.3), multi-pass hot rolling treatment: the laminating and hot rolling processes are carried out in a cycle until the thickness of the single-layer metal foil is 0.1 to 1 μm.
14. The method for mass production of dispersion-strengthened metallic material according to claim 13, wherein the hot rolling pretreatment in the step (3.1) is carried out under a vacuum of 1 x 10 -6 ～1×10 -3 Pa, the temperature is 300-1000 ℃ according to different materials, and the thickness is reduced by 5-30% in each hot rolling.
15. The method for batch preparation of the dispersion-strengthened metal material as claimed in claim 14, wherein the solvent for ultrasonic cleaning in step (3.2) is acetone, and the ultrasonic cleaning time is 5-30 min.
16. The method for batch production of dispersion-strengthened metallic materials according to claim 15, wherein the degree of vacuum of the thermal stress annealing treatment in step (3.2) is 1 x 10 -6 ～1×10 -3 Pa, and the annealing temperature is 300-1000 ℃ according to different melting points of the material.
17. The method for mass production of dispersion-strengthened metallic material according to claim 16, wherein the step (3.2) of hot rolling is carried out under a vacuum of 1 x 10 -6 ～1×10 -3 Pa, the temperature is selected to be 300-1000 ℃ according to different materials, and the thickness is reduced by 5-30% in each hot rolling.
18. The method for batch preparation of dispersion-strengthened metal materials as claimed in claim 1, wherein the hot isostatic pressing temperature in step (4) is 900-1200 ℃, the pressure is 80-180MPa, and the holding time is 1-3 h.
19. The method for mass production of a dispersion-strengthened metal material as claimed in claim 18, wherein the aging heat treatment in the step (4) is carried out under a vacuum degree of 1 x 10 -6 Pa～1×10 -3 Pa, the temperature is 600-1400 ℃, and the time is 1-20 h.
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