CN112981178B - Zinc-based soluble metal material and preparation and processing method thereof - Google Patents
Zinc-based soluble metal material and preparation and processing method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C18/00—Alloys based on zinc
- C22C18/02—Alloys based on zinc with copper as the next major constituent
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/03—Making non-ferrous alloys by melting using master alloys
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C18/00—Alloys based on zinc
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/002—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working by rapid cooling or quenching; cooling agents used therefor
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
- C22F1/165—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon of zinc or cadmium or alloys based thereon
Abstract
The invention relates to a zinc-based dissolvable metal material and a preparation and processing method thereof, belonging to the technical field of industrial zinc alloy. The metal material comprises the following components in percentage by mass: cu: 0.5-3.0%, Fe: 0.5-2.0%, Mg: 1.2-4.5% and the balance of zinc. Preheating a zinc ingot and a crucible, placing part of zinc in the crucible, heating until the zinc ingot is completely melted, adding the zinc ingot in batches, and completely covering the zinc ingot with a melt each time until the total amount of the zinc ingot is expected; adopting protective gas for protection; adding preheated Mg-Cu intermediate alloy, and raising the temperature of the crucible; adding Fe powder, carrying out surface treatment on the iron powder, and carrying out electromagnetic stirring and ultrasonic stirring on the melt; extruding to obtain a bar; water cooling or air cooling to room temperature; and deforming again to obtain the final product. The invention carries out optimization design from two aspects of components and deformation processing, realizes the regulation and control of the corrosion rate of the final alloy, and meets the requirements of development and development of the degradable bridge plug for oil exploitation.
Description
Technical Field
The invention relates to a zinc-based dissolvable metal material and a preparation and processing method thereof, belonging to the technical field of industrial zinc alloy.
Background
In the field of petroleum, fracturing refers to a method of forming cracks in oil and gas layers by using the action of water power in the process of oil or gas production, and is also called hydraulic fracturing. Fracturing is the process of artificially cracking stratum, improving the flowing environment of oil in underground and increasing the yield of oil well, and plays an important role in improving the flowing condition of oil well bottom, slowing down the interlamination and improving the oil layer utilization condition. Classified hydraulic (oil) pressure fracturing and high-energy air pressure fracturing, and can be divided into single packer layering, double packer layering, bridge plug packer layering and sliding sleeve packer layering according to the types of the plugging devices. The bridge plug is produced along with the appearance of a permanent bridge plug, is formed in the 80 s, is used as an underground plugging tool for an oil field, and is widely used for plugging a lower well section during the layered fracturing, layered acidification and layered oil testing construction of an oil-water well in the exploration and development of the oil field. The problems of complex operations of setting, salvaging and unsealing and low success rate of use are solved well. The underground plugging tool can replace releasing, a packer and cement injection plugging in function, and is safe, reliable, low in cost and complete in function. Currently, bridge plugs can be classified into four types, namely fishable bridge plugs, drillable bridge plugs, large-bore bridge plugs and soluble bridge plugs. The fishable bridge plug is a type of bridge plug which can be repeatedly used and is put into a preset position in a well along with an oil pipe, and after setting and releasing are finished, a fishing tool is put into the well for butt joint and fishing; most parts of the quick drillable bridge plug are made of composite materials, and a small number of parts are made of materials such as high polymers, metals and the like. The composite material ensures the quick drillability of the bridge plug; after fracturing is completed, an internal bridge plug is quickly drilled and removed in a short time by generally driving a power motor and a milling tool by a continuous oil pipe operating machine; the large-drift-diameter bridge plug has a larger inner channel and can directly meet the requirement of well completion production without drilling the bridge plug by being matched with a soluble fracturing ball. The components of the fracturing-soluble ball are mainly divided into 2 types of polymeric materials and alloy materials. The soluble bridge plug is divided into soluble engineering plastic bridge plug (composite material bridge plug) and alloy metal bridge plug, and the key technology is soluble design. The magnesium alloy has the characteristics of small density, high specific strength and specific stiffness, active chemical property and the like, and is an ideal material for high-strength and quick-dissolving bridge plugs. The rapid dissolution of the bridge plug is in fact a result of the rapid corrosion of magnesium and its alloys. Although magnesium alloy is the main material of choice for dissolvable bridge plug at present, it must be surface treated before use, and has limited bearing capacity, and there is uncertainty about the complex and varied environment underground, and some environment conditions can not even be used. Compared with the prior art, the zinc alloy has more various corrosion characteristics, the matrix of the zinc alloy has better corrosion resistance than magnesium, and the surface treatment process is relatively simple; in addition, the corrosion rate can be further improved by adjusting the components in the alloy, and therefore, the zinc alloy is more advantageous as a material for dissolving the bridge plug than the magnesium alloy.
Disclosure of Invention
The invention provides a zinc-based degradable alloy and a preparation and processing method thereof, which are used as alternative materials of a degradable bridge plug and can meet the application requirements of the dissolvable bridge plug on more occasions.
A zinc-based dissolvable metal material is a zinc-based degradable alloy, and comprises the following components in percentage by mass: cu: 0.5-3.0%, Fe: 0.5-2.0%, Mg: 1.2-4.5% and the balance of zinc.
The Cu element can form a MgZnCu phase with the matrix Zn and Mg, the phase can change the electrode potential of the whole alloy, and the controllability of the corrosion performance of the matrix can be realized by adjusting the Cu element and the Mg element.
Fe element and Zn can form a Zn-Fe needle phase, so that the shape and the appearance can be changed, recrystallization can be induced, nucleation can be promoted, and the corrosion rate of a matrix can be changed.
The preparation method of the zinc-based dissolvable metal material comprises the following steps:
(1) proportioning according to mass percent, wherein Cu and Mg are added in the form of Mg-Cu master alloy, and Fe is added in the form of powder;
(2) preheating a zinc ingot and a crucible to remove moisture, then placing part of preheated zinc in the crucible, slowly heating the crucible, further heating until the zinc ingot is completely melted, and then continuously adding the zinc ingots in batches to ensure that the zinc ingot is completely covered by a melt each time until the expected total amount is reached; protective gas is adopted for protection in the process;
(3) adding preheated Mg-Cu intermediate alloy into the melt, and simultaneously raising the temperature of the crucible;
(4) after the Mg-Cu intermediate alloy is completely dissolved, adding Fe powder, carrying out surface treatment on the iron powder, and simultaneously carrying out electromagnetic stirring and ultrasonic stirring on the melt;
(5) cooling the zinc melt, then carrying out semi-solid stirring, continuously cooling, and extruding into a bar;
(6) carrying out water cooling or air cooling on the extruded bar to room temperature;
(7) and deforming the bar again according to the requirements of the corrosion speed and the specification of the material, wherein the final deformation mode is extrusion to obtain a final product with the required specification.
In the step (1), the mass percent of Cu in the Mg-Cu intermediate alloy is 35-65%.
In the step (2), the preheating temperature of the zinc ingot and the crucible is 100-150 ℃, zinc which accounts for 25-30% of the total mass after preheating is placed in the crucible at the beginning, the crucible is slowly heated, the initial temperature does not exceed 400 ℃, then the temperature is kept for 5-10 minutes, and the zinc ingot is further heated until the zinc ingot is completely melted; the crucible temperature does not exceed 600 ℃ at most. In the heating process, protective gas is adopted for protection in the whole process to prevent zinc oxidation, the protective atmosphere is a mixture of tetrafluoroethane and argon, and the volume ratio of tetrafluoroethane to argon is 1: 20-1: 25.
In the step (3), the preheating temperature of the Mg-Cu intermediate alloy is 200-300 ℃, and the surface is ensured to have no water vapor; the weight of the single Mg-Cu master alloy is not more than 100 g; in the process of adding preheated Mg-Cu intermediate alloy into the melt, the temperature of the crucible is raised to 650-700 ℃.
In the step (4), the iron powder needs to be subjected to surface treatment to prevent oxidation in the heating process, typically including iron powder surface carbonization treatment or nitridation treatment, and the like, and the rapid dispersion of the Fe powder can be accelerated by applying electromagnetic stirring and ultrasonic stirring to the melt.
The surface treatment of iron powder is generally a carbonization or nitridation surface treatment of iron powder, in which the surface carbonization is a heat treatment with carbon monoxide and the surface nitridation is a heat treatment with ammonia gas. When the surface is carbonized or nitrided, firstly the surface of the iron powder is cleaned, gasoline is adopted for cleaning, then the vacuum pumping is carried out, the gas of carbon monoxide or ammonia gas is filled, the temperature is increased to between 100 and 800 ℃, the temperature is kept for a period of time at 800 ℃ and 500 and the temperature is reduced to the room temperature, and the iron powder with the carbonized or nitrided surface is obtained.
In the step (5), the zinc melt is cooled to 390-410 ℃, then semi-solid stirring is carried out, the temperature is continuously cooled to 300-350 ℃, and bars with the diameter of 100-300 mm are extruded.
And (7) deforming the bar again, wherein the deforming comprises forging, extruding or drawing and the like, and the final product is the bar with the diameter of 70-200 mm.
The zinc-based dissolvable metal material can be applied to preparing a dissolvable bridge plug. The zinc-based dissolvable alloy can obtain the required corrosion speed by adjusting the components in the alloy, is very suitable for being used as a material for a dissolvable bridge plug, and simultaneously has better corrosion resistance of a matrix and relatively simple surface treatment process.
The invention has the advantages that:
the invention adds Mg, Fe and Cu elements in the zinc matrix to form a compound or simple substance phase with larger potential difference with the matrix, and each phase has different electrode potential, thus the corrosion rate of the alloy can be adjusted by using the change of components. In addition, zinc itself has a hexagonal structure and has a sharp anisotropic characteristic, so that a certain texture can be generated by plastic deformation processing, and the corrosion rate of the alloy can be changed. In conclusion, the method is optimally designed from two aspects of components and deformation processing, realizes the regulation and control of the corrosion rate of the final target alloy, and further meets the requirements of development and development of the degradable bridge plug for oil exploitation.
Detailed Description
The zinc-based degradable alloy comprises the following main components: cu: 0.5-3.0%, Fe: 0.5-2.0%, Mg: 1.2-4.5% and the balance of zinc. Wherein Cu and Mg are added in the form of Mg- (35-65%) Cu master alloy, and Fe is added in the form of powder. The above are all mass percentages.
Firstly preheating a zinc ingot and a crucible to remove water, wherein the preheating temperature is 100-150 ℃, then placing 25-30% of zinc in the crucible by the total mass after preheating, slowly heating the crucible, wherein the initial temperature is not more than 400 ℃, then preserving heat for 5-10 minutes, further heating until the zinc ingot is completely melted, and then continuously adding the zinc ingot in batches to ensure that the zinc ingot can be completely covered by the melt each time until the expected total amount is reached. The crucible temperature does not exceed 600 ℃ at most. In the heating process, protective gas is adopted for protection in the whole process to prevent zinc oxidation, and the mixture of tetrafluoroethane and argon is adopted in the protective atmosphere in a ratio of 1: 20-1: 25. Adding preheated Mg-Cu intermediate alloy into the melt, wherein the preheating temperature is 200-300 ℃, ensuring that the surface has no water vapor, and in the adding process, the weight of a single intermediate alloy does not exceed 100 g, and simultaneously, the temperature of a crucible is increased to 650-700 ℃. And after the Mg-Cu intermediate alloy is completely dissolved, adding Fe powder, wherein the iron powder needs to be subjected to surface treatment to prevent oxidation in the heating process, and in addition, in order to accelerate the rapid dispersion of the Fe powder, applying electromagnetic stirring and ultrasonic stirring to the melt. And cooling the zinc melt to 390-410 ℃, then carrying out semi-solid stirring, continuously cooling to 300-350 ℃, and extruding into a bar with the diameter of 100-300 mm. The extruded rod is rapidly water-cooled or air-cooled to room temperature. According to the requirements of the corrosion speed and specification of the material, the bar can be deformed again, including forging, extruding, drawing and the like, but the final deformation mode is extrusion, and the specification of the final product is 70-200 mm.
In the following examples, the surface treatment of the iron powder is generally carried out by subjecting the iron powder to a surface treatment of carbonization or nitridation. And during surface carbonization treatment, firstly, cleaning the surface of the iron powder by adopting gasoline, then vacuumizing, charging carbon monoxide, heating to 500 ℃, preserving heat for 3 hours, and then cooling to room temperature to obtain the surface carbonized iron powder. And in the surface nitriding treatment, firstly, cleaning the surface of the iron powder by adopting gasoline, then vacuumizing, filling ammonia gas, heating to 600 ℃, preserving heat for 3 hours, and then cooling to room temperature to obtain the iron powder with the nitrided surface.
Example 1
The zinc-based dissolvable material prepared in this example includes the following component ratios: cu: 0.5%, Fe: 0.5%, Mg: 1.2 percent and the balance of zinc. Wherein Cu and Mg are added in the form of Mg-30% Cu master alloy, and Fe is added in the form of powder. The above are all mass percentages.
The preparation method of the zinc-based dissolvable material prepared in the embodiment comprises the following steps:
(1) preheating a zinc ingot and a crucible to remove water, wherein the preheating temperature is 100 ℃, then placing 25% of zinc of the total mass after preheating into the crucible, slowly heating the crucible, wherein the initial temperature is not more than 400 ℃, then preserving heat for 10 minutes, further heating until the zinc ingot is completely melted, and then continuously adding the zinc ingot in batches to ensure that the zinc ingot can be completely covered by a melt each time until the expected total amount is reached. The crucible temperature does not exceed 600 ℃ at most. In the heating process, protective gas is adopted for protection in the whole process to prevent zinc oxidation, and the protective atmosphere is a mixture of tetrafluoroethane and argon in a volume ratio of 1: 20.
(2) Adding preheated Mg-Cu intermediate alloy into the melt, wherein the preheating temperature is 200 ℃, ensuring that the surface has no water vapor, and in the adding process, the weight of a single intermediate alloy does not exceed 100 g, and simultaneously, the temperature of a crucible is increased to 650 ℃.
(3) And after the Mg-Cu intermediate alloy is completely dissolved, adding Fe powder, wherein the iron powder needs to be subjected to surface carbonization treatment to prevent oxidation in the heating process, and in addition, in order to accelerate the rapid dispersion of the Fe powder, applying electromagnetic stirring and ultrasonic stirring to the melt.
(4) And cooling the zinc melt to 410 ℃, then carrying out semi-solid stirring, continuously cooling to 300 ℃, and extruding into a bar with the diameter of 100 mm.
(5) And (4) rapidly cooling the extruded bar to room temperature by water.
(6) And (4) deforming the bar again according to the requirements of the corrosion speed and specification of the material, wherein the bar comprises forging and extruding, and the specification of a final product is 70mm in diameter.
Example 2
The zinc-based dissolvable material prepared in this example includes the following component ratios: cu: 3%, Fe: 0.5%, Mg: 1.6 percent and the balance of zinc. Wherein Cu and Mg are added in the form of Mg-65% Cu master alloy, and Fe is added in powder form. The above are all mass percentages.
(1) Preheating a zinc ingot and a crucible to remove water, wherein the preheating temperature is 100 ℃, then placing zinc with 25% of the total mass after preheating into the crucible, slowly heating the crucible, wherein the initial temperature is not more than 400 ℃, then preserving heat for 8 minutes, further heating until the zinc ingot is completely melted, and then continuously adding the zinc ingot in batches to ensure that the zinc ingot can be completely covered by a melt each time until the expected total amount is reached. The crucible temperature does not exceed 600 ℃ at most. In the heating process, protective gas is adopted for protection in the whole process to prevent zinc oxidation, and the protective atmosphere is a mixture of tetrafluoroethane and argon in a volume ratio of 1: 23.
(2) Adding preheated Mg-Cu intermediate alloy into the melt, wherein the preheating temperature is 200 ℃, ensuring that the surface has no water vapor, and in the adding process, the weight of a single intermediate alloy does not exceed 100 g, and simultaneously, the temperature of a crucible is increased to 650 ℃.
(3) And after the Mg-Cu intermediate alloy is completely dissolved, adding Fe powder, wherein the iron powder needs to be subjected to surface carbonization treatment to prevent oxidation in the heating process, and in addition, in order to accelerate the rapid dispersion of the Fe powder, applying electromagnetic stirring and ultrasonic stirring to the melt.
(4) And cooling the zinc melt to 410 ℃, then carrying out semi-solid stirring, continuously cooling to 300 ℃, and extruding into a bar with the diameter of 125 mm.
(5) And (4) rapidly cooling the extruded bar to room temperature by water.
(6) According to the requirements of the corrosion speed and specification of the material, the bar can be deformed again, including forging, drawing and extruding, and the specification of the final product is 90mm in diameter.
Example 3
The zinc-based dissolvable material prepared in this example includes the following component ratios: cu: 1%, Fe: 0.5%, Mg: 2.0 percent and the balance of zinc. Wherein Cu and Mg are added in the form of Mg-35% Cu master alloy, and Fe is added in the form of powder. The above are all mass percentages.
(1) Preheating a zinc ingot and a crucible to remove water, wherein the preheating temperature is 125 ℃, then placing zinc with the total mass of 30% of the preheated zinc into the crucible, slowly heating the crucible, keeping the initial temperature not more than 400 ℃, then keeping the temperature for 9 minutes, further heating until the zinc ingot is completely molten, and then continuously adding the zinc ingot in batches to ensure that the zinc ingot can be completely covered by a melt each time until the expected total amount is reached. The crucible temperature does not exceed 600 ℃ at most. In the heating process, protective gas is adopted for protection in the whole process to prevent zinc oxidation, and the protective atmosphere is a mixture of tetrafluoroethane and argon in a volume ratio of 1: 25.
(2) Adding preheated Mg-Cu intermediate alloy into the melt, wherein the preheating temperature is 250 ℃, ensuring that the surface has no water vapor, and in the adding process, the weight of a single intermediate alloy does not exceed 100 g, and simultaneously, the temperature of a crucible is increased to 675 ℃.
(3) And after the Mg-Cu intermediate alloy is completely dissolved, adding Fe powder, wherein the iron powder needs to be subjected to surface nitriding treatment to prevent oxidation in the heating process, and in addition, in order to accelerate the rapid dispersion of the Fe powder, applying electromagnetic stirring and ultrasonic stirring to the melt.
(4) And cooling the zinc melt to 410 ℃, then carrying out semi-solid stirring, continuously cooling to 300 ℃, and extruding into a bar with the diameter of 150 mm.
(5) And (4) rapidly cooling the extruded bar to room temperature by water.
(6) And (4) extruding the bar again according to the requirements of the corrosion speed and specification of the material, wherein the specification of the final product is 110mm in diameter.
Example 4
The zinc-based dissolvable material prepared in this example includes the following component ratios: cu: 1.5%, Fe: 0.5%, Mg: 2.8 percent and the balance of zinc. Wherein Cu and Mg are added in the form of Mg-35% Cu master alloy, and Fe is added in the form of powder. The above are all mass percentages.
(1) Preheating a zinc ingot and a crucible to remove water, wherein the preheating temperature is 125 ℃, then placing zinc with the total mass of 30% of the preheated zinc into the crucible, slowly heating the crucible, keeping the initial temperature not more than 400 ℃, then keeping the temperature for 5 minutes, further heating until the zinc ingot is completely molten, and then continuously adding the zinc ingot in batches to ensure that the zinc ingot can be completely covered by a melt each time until the expected total amount is reached. The crucible temperature does not exceed 600 ℃ at most. In the heating process, protective gas is adopted for protection in the whole process to prevent zinc oxidation, and the protective atmosphere is a mixture of tetrafluoroethane and argon in a volume ratio of 1: 22.
(2) Adding preheated Mg-Cu intermediate alloy into the melt, wherein the preheating temperature is 250 ℃, ensuring that the surface has no water vapor, and in the adding process, the weight of a single intermediate alloy does not exceed 100 g, and simultaneously, the temperature of a crucible is increased to 675 ℃.
(3) And after the Mg-Cu intermediate alloy is completely dissolved, adding Fe powder, wherein the iron powder needs to be subjected to surface nitriding treatment to prevent oxidation in the heating process, and in addition, in order to accelerate the rapid dispersion of the Fe powder, applying electromagnetic stirring and ultrasonic stirring to the melt.
(4) And cooling the zinc melt to 410 ℃, then carrying out semi-solid stirring, continuously cooling to 300 ℃, and extruding into a bar with the diameter of 175 mm.
(5) And (4) rapidly cooling the extruded bar to room temperature by water.
(6) And (4) extruding the bar again according to the requirements of the corrosion speed and specification of the material, wherein the specification of the final product is 130mm in diameter.
Example 5
The zinc-based dissolvable material prepared in this example includes the following component ratios: cu: 2.0%, Fe: 0.5%, Mg: 3.8 percent, and the balance of zinc. Wherein Cu and Mg are added in the form of Mg-35% Cu master alloy, and Fe is added in the form of powder. The above are all mass percentages.
(1) Preheating a zinc ingot and a crucible to remove water, wherein the preheating temperature is 150 ℃, then placing zinc with 25% of the total mass after preheating into the crucible, slowly heating the crucible, wherein the initial temperature is not more than 400 ℃, then preserving heat for 7 minutes, further heating until the zinc ingot is completely melted, and then continuously adding the zinc ingot in batches to ensure that the zinc ingot can be completely covered by a melt each time until the expected total amount is reached. The crucible temperature does not exceed 600 ℃ at most. In the heating process, protective gas is adopted for protection in the whole process to prevent zinc oxidation, and the protective atmosphere is a mixture of tetrafluoroethane and argon in a volume ratio of 1: 24.
(2) Adding preheated Mg-Cu intermediate alloy into the melt, wherein the preheating temperature is 300 ℃, ensuring that the surface has no water vapor, and in the adding process, the weight of a single intermediate alloy does not exceed 100 g, and simultaneously, the temperature of a crucible is increased to 700 ℃.
(3) And after the Mg-Cu intermediate alloy is completely dissolved, adding Fe powder, wherein the iron powder needs to be subjected to surface nitriding treatment to prevent oxidation in the heating process, and in addition, in order to accelerate the rapid dispersion of the Fe powder, applying electromagnetic stirring and ultrasonic stirring to the melt.
(4) Cooling the zinc melt to 410 ℃, then carrying out semi-solid stirring, continuously cooling to 300 ℃, and extruding into a bar with the diameter of 200 mm.
(5) The extruded rods were air cooled to room temperature.
(6) And (4) deforming the bar again according to the requirements of the corrosion speed and specification of the material, wherein the bar comprises forging and extruding, and the specification of a final product is 150mm in diameter.
Example 6
The zinc-based dissolvable material prepared in this example includes the following component ratios: cu: 2.5%, Fe: 0.5%, Mg: 1.4 percent and the balance of zinc. Wherein Cu and Mg are added in the form of Mg-35% Cu master alloy, and Fe is added in the form of powder. The above are all mass percentages.
(1) Preheating a zinc ingot and a crucible to remove water, wherein the preheating temperature is 150 ℃, then placing zinc with 25% of the total mass after preheating into the crucible, slowly heating the crucible, wherein the initial temperature is not more than 400 ℃, then preserving heat for 7 minutes, further heating until the zinc ingot is completely melted, and then continuously adding the zinc ingot in batches to ensure that the zinc ingot can be completely covered by a melt each time until the expected total amount is reached. The crucible temperature does not exceed 600 ℃ at most. In the heating process, protective gas is adopted for protection in the whole process to prevent zinc oxidation, and the protective atmosphere is a mixture of tetrafluoroethane and argon in a volume ratio of 1: 21.
(2) Adding preheated Mg-Cu intermediate alloy into the melt, wherein the preheating temperature is 300 ℃, ensuring that the surface has no water vapor, and in the adding process, the weight of a single intermediate alloy does not exceed 100 g, and simultaneously, the temperature of a crucible is increased to 700 ℃.
(3) And after the Mg-Cu intermediate alloy is completely dissolved, adding Fe powder, wherein the iron powder needs to be subjected to surface carbonization treatment to prevent oxidation in the heating process, and in addition, in order to accelerate the rapid dispersion of the Fe powder, applying electromagnetic stirring and ultrasonic stirring to the melt.
(4) And cooling the zinc melt to 400 ℃, then carrying out semi-solid stirring, continuously cooling to 300 ℃, and extruding into a bar with the diameter of 225 mm.
(5) The extruded rods were air cooled to room temperature.
(6) And (4) deforming the bar again according to the requirements of the corrosion speed and specification of the material, wherein the bar comprises forging and extruding, and the specification of a final product is 170mm in diameter.
Example 7
The zinc-based dissolvable material prepared in this example includes the following component ratios: cu: 3%, Fe: 1%, Mg: 1.6 percent and the balance of zinc. Wherein Cu and Mg are added in the form of Mg-65% Cu master alloy, and Fe is added in powder form. The above are all mass percentages.
(1) Preheating a zinc ingot and a crucible to remove water, wherein the preheating temperature is 100 ℃, then placing zinc with 25% of the total mass after preheating into the crucible, slowly heating the crucible, wherein the initial temperature is not more than 400 ℃, then preserving heat for 6 minutes, further heating until the zinc ingot is completely melted, and then continuously adding the zinc ingot in batches to ensure that the zinc ingot can be completely covered by a melt each time until the expected total amount is reached. The crucible temperature does not exceed 600 ℃ at most. In the heating process, protective gas is adopted for protection in the whole process to prevent zinc oxidation, and the protective atmosphere is a mixture of tetrafluoroethane and argon in a volume ratio of 1: 25.
(2) Adding preheated Mg-Cu intermediate alloy into the melt, wherein the preheating temperature is 225 ℃, ensuring that the surface has no water vapor, and in the adding process, the weight of a single intermediate alloy does not exceed 100 g, and simultaneously, the temperature of a crucible is increased to 680 ℃.
(3) And after the Mg-Cu intermediate alloy is completely dissolved, adding Fe powder, wherein the iron powder needs to be subjected to surface carbonization treatment to prevent oxidation in the heating process, and in addition, in order to accelerate the rapid dispersion of the Fe powder, applying electromagnetic stirring and ultrasonic stirring to the melt.
(4) And cooling the zinc melt to 390 ℃, then carrying out semi-solid stirring, continuously cooling to 300 ℃, and extruding into a bar with the diameter of 250 mm.
(5) And (4) rapidly cooling the extruded bar to room temperature by water.
(6) And (3) deforming the bar again according to the requirements of the corrosion speed and specification of the material, wherein the deformation comprises forging, drawing and extruding, the final deformation mode is extruding, and the specification of the final product is 120mm in diameter.
Example 8
The zinc-based dissolvable material prepared in this example includes the following component ratios: cu: 3.0%, Fe: 1.5%, Mg: 1.6 percent and the balance of zinc. Wherein Cu and Mg are added in the form of Mg-65% Cu master alloy, and Fe is added in powder form. The above are all mass percentages.
(1) Preheating a zinc ingot and a crucible to remove water, wherein the preheating temperature is 125 ℃, then placing zinc with the total mass of 30% of the preheated zinc into the crucible, slowly heating the crucible, keeping the initial temperature not more than 400 ℃, then keeping the temperature for 6 minutes, further heating until the zinc ingot is completely molten, and then continuously adding the zinc ingot in batches to ensure that the zinc ingot can be completely covered by a melt each time until the expected total amount is reached. The crucible temperature does not exceed 600 ℃ at most. In the heating process, protective gas is adopted for protection in the whole process to prevent zinc oxidation, and the protective atmosphere is a mixture of tetrafluoroethane and argon in a volume ratio of 1: 20.
(2) Adding preheated Mg-Cu intermediate alloy into the melt, wherein the preheating temperature is 225 ℃, ensuring that the surface has no water vapor, and in the adding process, the weight of a single intermediate alloy does not exceed 100 g, and simultaneously, the temperature of a crucible is increased to 680 ℃.
(3) And after the Mg-Cu intermediate alloy is completely dissolved, adding Fe powder, wherein the iron powder needs to be subjected to surface nitriding treatment to prevent oxidation in the heating process, and in addition, in order to accelerate the rapid dispersion of the Fe powder, applying electromagnetic stirring and ultrasonic stirring to the melt.
(4) And cooling the zinc melt to 390 ℃, then carrying out semi-solid stirring, continuously cooling to 300 ℃, and extruding into a bar with the diameter of 275 mm.
(5) And (4) rapidly cooling the extruded bar to room temperature by water.
(6) And (4) deforming the bar again according to the requirements of the corrosion speed and specification of the material, wherein the bar comprises forging and extruding, and the specification of a final product is 100mm in diameter.
Example 9
The zinc-based dissolvable material prepared in this example includes the following component ratios: cu: 3%, Fe: 2.0%, Mg: 1.6 percent and the balance of zinc. Wherein Cu and Mg are added in the form of Mg-65% Cu master alloy, and Fe is added in powder form. The above are all mass percentages.
(1) Preheating a zinc ingot and a crucible to remove water, wherein the preheating temperature is 150 ℃, then placing zinc with the total mass of 30% of the preheated zinc into the crucible, slowly heating the crucible, keeping the initial temperature not more than 400 ℃, then keeping the temperature for 8 minutes, further heating until the zinc ingot is completely molten, and then continuously adding the zinc ingot in batches to ensure that the zinc ingot can be completely covered by a melt each time until the expected total amount is reached. The crucible temperature does not exceed 600 ℃ at most. In the heating process, protective gas is adopted for protection in the whole process to prevent zinc oxidation, and the protective atmosphere is a mixture of tetrafluoroethane and argon in a volume ratio of 1: 20.
(2) Adding preheated Mg-Cu intermediate alloy into the melt, wherein the preheating temperature is 275 ℃, ensuring that the surface has no water vapor, and in the adding process, the weight of a single intermediate alloy does not exceed 100 g, and simultaneously, the temperature of a crucible is increased to 680 ℃.
(3) And after the Mg-Cu intermediate alloy is completely dissolved, adding Fe powder, wherein the iron powder needs to be subjected to surface nitriding treatment to prevent oxidation in the heating process, and in addition, in order to accelerate the rapid dispersion of the Fe powder, applying electromagnetic stirring and ultrasonic stirring to the melt.
(4) And cooling the zinc melt to 390 ℃, then carrying out semi-solid stirring, continuously cooling to 300 ℃, and extruding into a bar with the diameter of 300 mm.
(5) And (4) rapidly cooling the extruded bar to room temperature by water.
(6) And (4) deforming the bar again according to the requirements of the corrosion speed and specification of the material, wherein the bar comprises forging and extruding, and the specification of a final product is 200mm in diameter.
Example 10
The zinc-based dissolvable material prepared in this example includes the following component ratios: cu: 3%, Fe: 2.0%, Mg: 1.6 percent and the balance of zinc. Wherein Cu and Mg are added in the form of Mg-65% Cu master alloy, and Fe is added in powder form. The above are all mass percentages.
(1) Preheating a zinc ingot and a crucible to remove water, wherein the preheating temperature is 125 ℃, then placing zinc with the total mass of 30% of the preheated zinc into the crucible, slowly heating the crucible, keeping the initial temperature not more than 400 ℃, then keeping the temperature for 8 minutes, further heating until the zinc ingot is completely molten, and then continuously adding the zinc ingot in batches to ensure that the zinc ingot can be completely covered by a melt each time until the expected total amount is reached. The crucible temperature does not exceed 600 ℃ at most. In the heating process, protective gas is adopted for protection in the whole process to prevent zinc oxidation, and the protective atmosphere is a mixture of tetrafluoroethane and argon in a volume ratio of 1: 25.
(2) Adding preheated Mg-Cu intermediate alloy into the melt, wherein the preheating temperature is 275 ℃, ensuring that the surface has no water vapor, and in the adding process, the weight of a single intermediate alloy does not exceed 100 g, and simultaneously, the temperature of a crucible is increased to 650 ℃.
(3) And after the Mg-Cu intermediate alloy is completely dissolved, adding Fe powder, wherein the iron powder needs to be subjected to surface carbonization treatment to prevent oxidation in the heating process, and in addition, in order to accelerate the rapid dispersion of the Fe powder, applying electromagnetic stirring and ultrasonic stirring to the melt.
(4) And cooling the zinc melt to 400 ℃, then carrying out semi-solid stirring, continuously cooling to 300 ℃, and extruding into a bar with the diameter of 300 mm.
(5) And (4) rapidly cooling the extruded bar to room temperature by water.
(6) And (4) extruding the bar again according to the requirements of the corrosion speed and specification of the material, wherein the specification of the final product is 80mm in diameter.
The zinc-based dissolvable materials prepared in examples 1-10 were tested and the results are shown in table 1.
Table 1 test performance of zinc-based dissolvable materials prepared in examples 1-10
| Examples | Working pressure (MPa) | Corrosion time (hours) |
| 1 | 70 | 48 |
| 2 | 75 | 52 |
| 3 | 70 | 96 |
| 4 | 65 | 70 |
| 5 | 72 | 70 |
| 6 | 45 | 100 |
| 7 | 68 | 35 |
| 8 | 48 | 48 |
| 9 | 62 | 39 |
| 10 | 55 | 48 |
The above embodiments are only used for illustrating but not limiting the technical solutions of the present invention, and although the above embodiments describe the present invention in detail, those skilled in the art should understand that: modifications and equivalents may be made thereto without departing from the spirit and scope of the invention and any modifications and equivalents may fall within the scope of the claims.
Claims (10)
1. A method for preparing a zinc-based soluble metal material comprises the following steps:
(1) the material is prepared according to the mass percentage, wherein Cu: 0.5-3.0%, Fe: 0.5-2.0%, Mg: 1.2-4.5% and the balance of zinc; cu and Mg are added in the form of Mg-Cu master alloy, and Fe is added in the form of powder;
(2) preheating a zinc ingot and a crucible to remove moisture, then placing part of preheated zinc in the crucible, slowly heating the crucible, further heating until the zinc ingot is completely melted, and then continuously adding the zinc ingots in batches to ensure that the zinc ingot is completely covered by a melt each time until the expected total amount is reached; protective gas is adopted for protection in the process;
(3) adding preheated Mg-Cu intermediate alloy into the melt, and simultaneously raising the temperature of the crucible;
(4) after the Mg-Cu intermediate alloy is completely dissolved, adding Fe powder, carrying out surface treatment on the iron powder, and simultaneously carrying out electromagnetic stirring and ultrasonic stirring on the melt;
(5) cooling the zinc melt, then carrying out semi-solid stirring, continuously cooling, and extruding into a bar;
(6) carrying out water cooling or air cooling on the extruded bar to room temperature;
(7) and deforming the bar again according to the requirements of the corrosion speed and the specification of the material, wherein the final deformation mode is extrusion, and obtaining a final product with the required specification.
2. The method of claim 1, wherein the zinc-based dissolvable metallic material comprises: in the Mg-Cu intermediate alloy, the mass percent of Cu is 35-65%.
3. The method of claim 1, wherein the zinc-based dissolvable metallic material comprises: the preheating temperature of the zinc ingot and the crucible is 100-150 ℃, zinc which accounts for 25-30% of the total mass after preheating is placed in the crucible at the beginning, the crucible is slowly heated, the initial temperature does not exceed 400 ℃, then the temperature is kept for 5-10 minutes, and the zinc ingot is further heated until the zinc ingot is completely melted; the crucible temperature does not exceed 600 ℃ at most.
4. The method of claim 1, wherein the zinc-based dissolvable metallic material comprises: the protective gas is tetrafluoroethane and argon, and the volume ratio of the tetrafluoroethane to the argon is 1: 20-1: 25.
5. The method of claim 1, wherein the zinc-based dissolvable metallic material comprises: the preheating temperature of the Mg-Cu intermediate alloy is 200-300 ℃; the weight of the single Mg-Cu master alloy is not more than 100 g; in the process of adding Mg-Cu intermediate alloy into the melt, the temperature of the crucible is raised to 650-700 ℃.
6. The method of claim 1, wherein the zinc-based dissolvable metallic material comprises: the iron powder is subjected to surface carbonization or surface nitridation treatment.
7. The method of claim 1, wherein the zinc-based dissolvable metallic material comprises: and cooling the zinc melt to 390-410 ℃, then carrying out semi-solid stirring, continuously cooling to 300-350 ℃, and extruding into a bar with the diameter of 100-300 mm.
8. The method of claim 1, wherein the zinc-based dissolvable metallic material comprises: the secondary deformation comprises forging, extruding or drawing, and the final product is a bar with the diameter of 70-200 mm.
9. A zinc-based dissolvable metallic material produced according to the method of claim 1.
10. Use of a zinc-based dissolvable metallic material according to claim 9 for the preparation of a dissolvable bridge plug.
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