CN110952013B - Degradable magnesium alloy downhole tool bridge plug material and preparation method thereof - Google Patents
Degradable magnesium alloy downhole tool bridge plug material and preparation method thereof Download PDFInfo
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- CN110952013B CN110952013B CN201911343147.XA CN201911343147A CN110952013B CN 110952013 B CN110952013 B CN 110952013B CN 201911343147 A CN201911343147 A CN 201911343147A CN 110952013 B CN110952013 B CN 110952013B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C23/00—Alloys based on magnesium
- C22C23/02—Alloys based on magnesium with aluminium 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
- C22C1/00—Making non-ferrous alloys
- C22C1/06—Making non-ferrous alloys with the use of special agents for refining or deoxidising
Abstract
The invention relates to the technical field of preparation of degradable magnesium alloy materials, and particularly relates to a degradable magnesium alloy downhole tool bridge plug material and a preparation method thereof. Weighing Zn, Mn, Al, Mg, Cu, Ni and Sb metals or metal alloys according to the formula proportion of the invention, preparing the metals or metal alloys by a standard process, processing the obtained cast ingots into target alloy materials, and then processing the materials into specified structural forms; in order to meet the mechanical properties and corrosion rate required by customers for using the material in different places, the material can also realize the structural form of a target product through extrusion deformation. The magnesium alloy has good crystal form and high mechanical strength, can be dissolved in solution containing electrolyte, can be completely degraded after completing the work task by utilizing the soluble magnesium alloy to manufacture the tool for constructing the bridge plug material of the underground tool, and has no problems of easy jamming and channel blockage, thereby saving the drilling and grinding recovery process, reducing the engineering difficulty and improving the construction efficiency.
Description
Technical Field
The invention relates to the technical field of preparation of degradable magnesium alloy materials, in particular to a degradable magnesium alloy downhole tool bridge plug material and a preparation method thereof.
Background
The low and medium osmotic pressure petroleum field or oil extraction well causes low natural productivity because of low underground osmotic pressure, and the high osmotic pressure petroleum field or oil extraction well causes low petroleum exploitation efficiency, low yield and even no oil production because of reduced osmotic pressure and narrow or blocked oil outlet channel in the later stage of oil exploitation, forcing the petroleum exploitation enterprises to adopt various advanced, high and new technologies and other methods to improve the exploitation efficiency and the oil output. The underground fracturing technology is one of the advanced technologies, plugging materials and consumables are required in the fracturing technology operation, and the oil components which are designed to perform temporary functions or are only temporarily required, such as key operation materials and consumables for plugging, such as fracturing balls and target darts, and the like, are conveyed to a preset underground position through an underground tool to perform subsection, layered plugging and fracturing until the underground operation is completed. After the underground operation is finished, the plugging materials and consumables are communicated from the underground to the aboveground, so that the petroleum and oil gas can be smoothly sprayed out of the well, and the exploitation is realized. In the conventional technology, a milling operation is adopted to remove plugging materials and consumables, such as fracturing balls and target darts for plugging, and scraps of the fracturing balls and the target darts bring technical difficulty or difficulty to the flowback operation due to different types and densities of the materials.
China has rich low-permeability oil and gas resources and has great exploration and development potential. In recent decades, the method has made great discovery in the exploration of low-permeability sandstone, marine carbonate and volcanic rock, and forms an international first-class development matching technology. Mature technologies for developing low-permeability oil and gas fields include water injection, fracturing, gas injection and the like. Future steady production, stimulation of oil and gas production will depend more on these low permeability unconventional oil and gas resources. Most of oil and gas resources are distributed in strata with different depths, and the multi-layer multi-section fracturing technology can be adopted to improve the productivity of a single well by simultaneously transforming a plurality of strata, so that the construction efficiency is improved. The development of these unconventional oil and gas resources must rely on reservoir reformation technology such as hydraulic fracturing, acid fracturing, etc., of which multi-layer multi-stage fracturing using downhole tools is a technology commonly used at present. In multi-layer multi-section fracturing, fracturing reconstruction is carried out layer by layer after interval intervals are separated by packing tools (such as fracturing balls and bridge plugs), and the packing tools are discharged back out of a shaft after construction of all the interval intervals is finished so as to conveniently get through a well and realize oil and gas exploitation.
At present, most common packing tools are made of steel, and have the defects of difficult drilling and milling, long time consumption, difficult flowback of powder and fragments after drilling and the like. The steel material of the first generation has difficulty in flowback due to high specific gravity; although the second generation composite material solves the problem of large specific gravity, the second generation composite material cannot be completely degraded, so that the second generation composite material has the problems of easy jamming and channel blockage, and the production and processing of raw materials depend on import, so that the cost is high; the oil-water-based drilling fluid cannot be completely degraded in the underground exploitation process, and has the characteristic of easy jamming. The application aims to provide a third-generation degradable material, can be widely applied to the field of oil exploitation, has the performance superior to that of a second-generation material, can be completely degraded, does not have the problems of easy jamming and channel blockage, can reduce the production cost, and is mainly used for assembling bridge plug material processing parts of underground tools.
Disclosure of Invention
In order to solve the above problems, a first aspect of the present invention provides a degradable magnesium alloy bridge plug material for a downhole tool, which comprises the following components by weight:
zinc (Zn): 0.45% -0.9%;
copper (Cu): 0.1% -0.5%;
manganese (Mn): 0.2% -0.5%;
nickel (Ni): 0.1% -0.5%;
aluminum (Al): 8% -9.5%;
antimony (Sb): 0.1% -0.5%;
the balance of magnesium (Mg) and inevitable impurities, and the sum of the weight percentages of the components is 100 percent.
As a preferable technical scheme, the degradable magnesium alloy downhole tool bridge plug material comprises the following components in percentage by weight:
zinc (Zn): 0.6 to 0.8 percent;
copper (Cu): 0.2 to 0.4 percent;
manganese (Mn): 0.25 to 0.4 percent;
nickel (Ni): 0.2 to 0.4 percent;
aluminum (Al): 8.5 to 9.2 percent;
antimony (Sb): 0.15 to 0.4 percent;
the balance of magnesium (Mg) and inevitable impurities, and the sum of the weight percentages of the components is 100 percent.
As a preferable technical scheme, the degradable magnesium alloy downhole tool bridge plug material comprises the following components in percentage by weight:
zinc (Zn): 0.7 percent;
copper (Cu): 0.3 percent;
manganese (Mn): 0.3 percent;
nickel (Ni): 0.25 percent;
aluminum (Al): 9.2 percent;
antimony (Sb): 0.3 percent;
the balance of magnesium (Mg) and inevitable impurities, and the sum of the weight percentages of the components is 100 percent.
As a preferable technical scheme, the degradable magnesium alloy downhole tool bridge plug material is used for producing construction tools in the oil and gas field exploitation process.
The second aspect of the invention provides a preparation method of a degradable magnesium alloy downhole tool bridge plug material, which at least comprises the following steps:
(1) smelting preparation: cleaning the interior of the crucible, hanging the crucible into a resistance furnace, starting an electric furnace until the crucible is heated to be dark red, and scattering a second fusing agent on the surface;
(2) adding materials and refining: taking metal magnesium, metal zinc, metal aluminum, metal copper, a magnesium-manganese intermediate alloy, a magnesium-nickel intermediate alloy and antimony trioxide as raw materials, mixing the raw materials according to the composition and the weight percentage content, under the protection of inert gas, firstly adding the metal magnesium, the metal zinc and the metal aluminum, preheating the magnesium-manganese intermediate alloy and the magnesium-nickel intermediate alloy on a furnace platform, then adding the magnesium-manganese intermediate alloy and the antimony trioxide at 750 ℃, finally adding the magnesium-nickel intermediate alloy and the metal copper at 780 ℃, and uniformly stirring to alloy the raw materials;
(3) intermediate sampling: sampling to detect chemical components, sealing the cover and standing for one hour after the chemical components are qualified;
(4) and (3) casting rod forming: and (4) after the sample in the step (3) is qualified, semi-continuously casting the sample at 740 ℃ to form a casting bar.
As a preferable technical proposal, in the step (1), in the preparation of smelting, the temperature of the molten liquid in the crucible heated by the electric furnace is controlled at 690-780 ℃.
As a preferable technical scheme, in the step (2), the purities of the metal magnesium, the metal zinc, the metal aluminum and the metal copper are respectively more than or equal to 99.9 percent.
As a preferable technical scheme, in the charging and refining process in the step (2), the melt is fully stirred in the whole process, and a second fusing agent is thrown to extinguish fire so as to alloy the melt.
As a preferable technical scheme, before the sampling in the step (3), the temperature is 760 ℃ for refining, five types of flux are thrown, the alloy liquid is uniformly stirred to be bright, and then the sampling operation is carried out after the alloy liquid is kept stand for ten minutes.
As a preferable technical scheme, after the cast rod is formed in the step (4), a hot extrusion process is further included.
Has the advantages that: the invention provides a degradable magnesium alloy downhole tool bridge plug material and a preparation method thereof, which utilize soluble magnesium alloy to manufacture a fracturing construction tool, the tool is automatically ablated in the well after completing a work task, and then is mixed in liquid and reversely discharged through a pipeline, so that the degradable magnesium alloy downhole tool bridge plug material can be completely degraded without the problems of easy jamming and channel blockage, thereby omitting a drilling and grinding recovery process, reducing the engineering difficulty and improving the construction efficiency.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention. In the drawings:
FIG. 1 is a gold phase diagram of the extruded bridge plug material at the center of the diameter (0.5D).
FIG. 2 is a gold phase diagram of one quarter (0.25D) of the diameter of the extruded bridge plug material.
FIG. 3 is a metallographic image of a semi-continuously cast bridge plug material at the center of the diameter (0.5D).
FIG. 4 is a gold phase diagram of a semi-continuously cast bridge plug material at one-quarter of its diameter (0.25D)
FIG. 5 is a corrosion curve of an extruded bridge plug material.
FIG. 6 is a corrosion curve for a semi-continuously cast bridge plug material.
Detailed Description
The technical features in the technical solutions provided by the present invention are further clearly and completely described below with reference to the specific embodiments, but the scope of protection of the present invention is not limited thereto.
"preferred", "more preferred", and the like, in the present invention, refer to embodiments of the invention that may provide certain benefits, under certain circumstances. However, other embodiments may be preferred, under the same or other circumstances. Furthermore, the recitation of one or more preferred embodiments does not imply that other embodiments are not useful, nor is it intended to exclude other embodiments from the scope of the invention.
The invention provides a degradable magnesium alloy downhole tool bridge plug material, which comprises the following components in percentage by weight:
zinc (Zn): 0.45% -0.9%;
copper (Cu): 0.1% -0.5%;
manganese (Mn): 0.2% -0.5%;
nickel (Ni): 0.1% -0.5%;
aluminum (Al): 8% -9.5%;
antimony (Sb): 0.1% -0.5%;
the balance of magnesium (Mg) and inevitable impurities, and the sum of the weight percentages of the components is 100 percent.
In a preferred embodiment, the degradable magnesium alloy bridge plug material for the downhole tool comprises the following components in percentage by weight:
zinc (Zn): 0.6 to 0.8 percent;
copper (Cu): 0.2 to 0.4 percent;
manganese (Mn): 0.25 to 0.4 percent;
nickel (Ni): 0.2 to 0.4 percent;
aluminum (Al): 8.5 to 9.2 percent;
antimony (Sb): 0.15 to 0.4 percent;
the balance of magnesium (Mg) and inevitable impurities, and the sum of the weight percentages of the components is 100 percent.
In a more preferred embodiment, the degradable magnesium alloy bridge plug material for the downhole tool comprises the following components in percentage by weight:
zinc (Zn): 0.7 percent;
copper (Cu): 0.3 percent;
manganese (Mn): 0.3 percent;
nickel (Ni): 0.25 percent;
aluminum (Al): 9.2 percent;
antimony (Sb): 0.3 percent;
the balance of magnesium (Mg) and inevitable impurities, and the sum of the weight percentages of the components is 100 percent.
In a preferred embodiment, the degradable magnesium alloy downhole tool bridge plug material is used for producing construction tools in oil and gas field exploitation.
The second aspect of the invention provides a preparation method of a degradable magnesium alloy downhole tool bridge plug material, which at least comprises the following steps:
(1) smelting preparation: cleaning the interior of the crucible, hanging the crucible into a resistance furnace, starting an electric furnace until the crucible is heated to be dark red, and scattering a second fusing agent on the surface;
(2) adding materials and refining: taking metal magnesium, metal zinc, metal aluminum, metal copper, a magnesium-manganese intermediate alloy, a magnesium-nickel intermediate alloy and antimony trioxide as raw materials, mixing the raw materials according to the composition and the weight percentage content, under the protection of inert gas, firstly adding the metal magnesium, the metal zinc and the metal aluminum, preheating the magnesium-manganese intermediate alloy and the magnesium-nickel intermediate alloy on a furnace platform, then adding the magnesium-manganese intermediate alloy and the antimony trioxide at 750 ℃, finally adding the magnesium-nickel intermediate alloy and the metal copper at 780 ℃, and uniformly stirring to alloy the raw materials;
(3) intermediate sampling: sampling to detect chemical components, sealing the cover and standing for one hour after the chemical components are qualified;
(4) and (3) casting rod forming: and (4) after the sample in the step (3) is qualified, semi-continuously casting the sample at 740 ℃ to form a casting bar.
Step (1) preparation for melting
In a preferred embodiment, in the step (1), in the preparation for smelting, the temperature of the molten metal in the crucible heated by the electric furnace is controlled at 690-780 ℃.
The crucible is cleaned in the step (1), so that impurities can be prevented from entering the alloy in the smelting process to cause defects.
The second fusing agent (RJ-2) is a eutectic body formed by melting and mixing chlorides such as potassium chloride, magnesium chloride, barium chloride and the like at high temperature, can also be synthesized by adding a small amount of barium chloride into carnallite and magnesium oxide for burning or other methods, and can be used for producing magnesium-containing alloys such as magnesium alloy or aluminum magnesium alloy and the like. When the metal magnesium is smelted at high temperature, the massive magnesium is easy to oxidize and burn, and when the metal magnesium is discharged, a proper amount of flux II is added, which can be used as an isolating agent to isolate the magnesium from air and water vapor, thereby inhibiting the oxidation and burning of the metal magnesium. When the metal magnesium alloy is smelted, the second fusing agent is added for smelting, and because the fusing agent has higher density and better adsorption effect on impurities, the effect of removing non-metallic inclusions can be achieved, and the impurity oxides and nitrides are precipitated from the molten liquid, the second fusing agent can be used as a smelting agent and a protective agent of magnesium and the magnesium alloy; in addition, the second flux can also be used for magnesium aluminum alloy welding agents and metal fluxes. The second flux has different applications, wherein the content of each component is different, and other impurities or residual unreacted raw materials can be introduced in the smelting process, so that the content of magnesium oxide in the second flux needs to be measured.
Step (2) material feeding and refining
In a preferred embodiment, in the step (2), the purities of the metal magnesium, the metal zinc, the metal aluminum and the metal copper are respectively more than or equal to 99.9 percent.
In a preferred embodiment, during the charging refining process in the step (2), the melt is fully stirred in the whole process, and a second fusing agent is thrown to extinguish fire so as to alloy the melt.
In a preferred embodiment, during the charging and refining process in the step (2), when the magnesium-manganese intermediate alloy and the magnesium-nickel intermediate alloy are placed on a furnace platform for preheating, a thermocouple is used for measuring the temperature of the molten liquid in the crucible.
In a preferred embodiment, in step (2), the inert gas is argon.
Step (3) intermediate sampling
In a preferred embodiment, before the sampling in the middle of the step (3), the temperature is 760 ℃ for refining, the five-melting agent is thrown, the alloy liquid is uniformly stirred to be bright, and then the sampling operation is carried out after the alloy liquid is kept for ten minutes.
The No. five fluxing agent (RJ-5) is prepared by melting potassium chloride, magnesium chloride, barium chloride, calcium fluoride and the like at high temperature, casting into blocks, crushing, grinding into powder by a ball mill, and sieving to obtain a product; the product mainly has the effects of enhancing the refining capacity of the magnesium alloy and is used as a refining agent, wherein magnesium chloride has a main active component, has a good covering effect and a certain refining capacity on a magnesium melt, and the melting point, the surface tension and the viscosity of the flux can be obviously reduced by adding potassium chloride, so that the stability of the flux is improved; the density of the flux can be increased by adding barium chloride, so that the flux and the magnesium melt are easier to separate; the calcium fluoride can be used as a thickening agent and can also improve the stability and refining capacity of the flux.
Step (4) cast rod forming
And (4) after the sample in the step (3) is qualified, semi-continuously casting the sample at 740 ℃ to form a casting bar.
According to the invention, magnesium is used as a base material, and metal Al and Zn materials are combined with magnesium to precipitate a strengthening phase, so that the alloy strength is improved, and the tensile property of the alloy is improved; the Cu and Ni are elements which seriously affect the corrosion resistance of the magnesium alloy, and the content components of the Cu and Ni are strictly controlled, but the invention utilizes the characteristics of the Cu and Ni elements to improve the corrosion rate of the alloy to meet the product requirement. The metal Mn material mainly plays a role in hindering the growth of alloy grains in the alloy, improves the yield strength of the alloy and improves the weldability of the alloy; the addition of the metal antimony is mainly to refine alloy crystal grains, improve the mechanical property of the alloy, increase and improve the fluidity of the alloy and facilitate semi-continuous casting.
In a preferred embodiment, after the step (4) of forming the cast rod, a step (5) of hot extrusion is further included.
Step (5) hot extrusion process
In a preferred embodiment, the hot extrusion process comprises at least the following steps:
A) homogenizing: preserving heat for 16h at the temperature of 360-400 ℃, and discharging and air cooling;
B) carrying out hot extrusion treatment;
C) t5 aging treatment: keeping the temperature at 175-200 ℃ for 10-16 h.
In a more preferred embodiment, the hot extrusion process comprises at least the following steps:
A) homogenizing: preserving heat for 16h at 380 ℃, discharging and air cooling;
B) carrying out hot extrusion treatment;
C) t5 aging treatment: keeping the temperature at 185 ℃ for 13 h.
In a preferred embodiment, the heating temperature of the mold in the step B) of the hot extrusion treatment is 300-
The heating temperature of the blank is 300-380 ℃.
In a more preferred embodiment, in the step B) hot extrusion process, the mold is heated to a temperature of
The blank heating temperature is 340 ℃ at 360 ℃.
The bridge plug material with high performance and low corrosion can be obtained by a hot extrusion process.
Hereinafter, the present invention will be described in more detail by way of examples, but it should be understood that these examples are merely illustrative and not restrictive.
Examples
Example 1
The embodiment 1 of the invention provides a degradable magnesium alloy downhole tool bridge plug material, which comprises the following components in percentage by weight:
zinc (Zn): 0.7 percent;
copper (Cu): 0.3 percent;
manganese (Mn): 0.3 percent;
nickel (Ni): 0.25 percent;
aluminum (Al): 9.2 percent;
antimony (Sb): 0.3 percent;
the balance of magnesium (Mg) and inevitable impurities, and the sum of the weight percentages of the components is 100 percent.
The degradable magnesium alloy downhole tool bridge plug material is used for producing construction tools in the oil and gas field exploitation process.
The embodiment 1 of the invention also provides a preparation method of the degradable magnesium alloy downhole tool bridge plug material, which comprises the following steps:
(1) smelting preparation: cleaning the interior of the crucible, hoisting the crucible into a resistance furnace, starting the electric furnace, controlling the temperature of the molten liquid in the crucible heated by the electric furnace at 690-780 ℃ until the crucible is heated to dark red, and scattering a No. two fusing agent (RJ-2) on the surface;
(2) adding materials and refining: taking metal magnesium, metal zinc, metal aluminum, metal copper, a magnesium-manganese intermediate alloy, a magnesium-nickel intermediate alloy and antimony trioxide as raw materials, mixing the raw materials according to the weight percentage of the components, firstly adding the metal magnesium, the metal zinc and the metal aluminum, placing the magnesium-manganese intermediate alloy and the magnesium-nickel intermediate alloy on a furnace platform for preheating, then adding the magnesium-manganese intermediate alloy and the antimony trioxide at 750 ℃, finally adding the magnesium-nickel intermediate alloy and the metal copper at 780 ℃, introducing inert gas argon, removing harmful hydrogen in an alloy liquid, and uniformly stirring to alloy the alloy liquid; fully stirring the molten liquid in the whole process, and throwing a second fusing agent (RJ-2) to extinguish fire so as to alloy the molten liquid;
(3) intermediate sampling: refining at 760 ℃, throwing a No. five fusing agent (RJ-5), uniformly stirring to enable the alloy liquid to be bright, standing for ten minutes and then sampling; sampling to detect chemical components, sealing the cover and standing for one hour after the chemical components are qualified;
(4) and (3) casting rod forming: and (4) after the sample in the step (3) is qualified, semi-continuously casting the alloy into a casting bar at 740 ℃, and covering protective gas in the crystallizer to prevent the alloy from burning.
In the step (2), the purities of the metal magnesium, the metal zinc, the metal aluminum and the metal copper are respectively more than or equal to 99.9 percent.
Example 2
The embodiment 2 of the invention provides a degradable magnesium alloy downhole tool bridge plug material, which comprises the following components in percentage by weight:
zinc (Zn): 0.7 percent;
copper (Cu): 0.3 percent;
manganese (Mn): 0.3 percent;
nickel (Ni): 0.25 percent;
aluminum (Al): 9.2 percent;
antimony (Sb): 0.3 percent;
the balance of magnesium (Mg) and inevitable impurities, and the sum of the weight percentages of the components is 100 percent.
The degradable magnesium alloy downhole tool bridge plug material is used for producing construction tools in the oil and gas field exploitation process.
The embodiment 2 of the invention also provides a preparation method of the degradable magnesium alloy downhole tool bridge plug material, which comprises the following steps:
(1) smelting preparation: cleaning the interior of the crucible, hoisting the crucible into a resistance furnace, starting the electric furnace, controlling the temperature of the molten liquid in the crucible heated by the electric furnace at 690-780 ℃ until the crucible is heated to dark red, and scattering a No. two fusing agent (RJ-2) on the surface;
(2) adding materials and refining: taking metal magnesium, metal zinc, metal aluminum, metal copper, a magnesium-manganese intermediate alloy, a magnesium-nickel intermediate alloy and antimony trioxide as raw materials, mixing the raw materials according to the weight percentage of the components, firstly adding the metal magnesium, the metal zinc and the metal aluminum, placing the magnesium-manganese intermediate alloy and the magnesium-nickel intermediate alloy on a furnace platform for preheating, then adding the magnesium-manganese intermediate alloy and the antimony trioxide at 750 ℃, finally adding the magnesium-nickel intermediate alloy and the metal copper at 780 ℃, introducing inert gas argon, removing harmful hydrogen in an alloy liquid, and uniformly stirring to alloy the alloy liquid; fully stirring the molten liquid in the whole process, and throwing a second fusing agent (RJ-2) to extinguish fire so as to alloy the molten liquid;
(3) intermediate sampling: refining at 760 ℃, throwing a No. five fusing agent (RJ-5), uniformly stirring to enable the alloy liquid to be bright, standing for ten minutes and then sampling; sampling to detect chemical components, sealing the cover and standing for one hour after the chemical components are qualified;
(4) and (3) casting rod forming: and (4) after the sample in the step (3) is qualified, semi-continuously casting the alloy into a casting bar at 740 ℃, and covering protective gas in the crystallizer to prevent the alloy from burning.
In the step (2), the purities of the metal magnesium, the metal zinc, the metal aluminum and the metal copper are respectively more than or equal to 99.9 percent.
And (5) after the cast rod is formed in the step (4), performing hot extrusion process.
The hot extrusion process comprises the following steps:
A) homogenizing: preserving heat for 16h at 380 ℃, discharging and air cooling;
B) carrying out hot extrusion treatment;
C) t5 aging treatment: keeping the temperature at 185 ℃ for 13 h.
In the step B) of hot extrusion treatment, the heating temperature of the die is 360 ℃, and the heating temperature of the blank is 340 ℃.
Example 3
The embodiment 3 of the invention provides a degradable magnesium alloy downhole tool bridge plug material and a preparation method of the degradable magnesium alloy downhole tool bridge plug material, and the specific implementation mode is the same as that of the embodiment 1, except that the degradable magnesium alloy downhole tool bridge plug material comprises the following components in percentage by weight:
zinc (Zn): 0.6 percent;
copper (Cu): 0.2 percent;
manganese (Mn): 0.25 percent;
nickel (Ni): 0.2 percent;
aluminum (Al): 8.5 percent;
antimony (Sb): 0.15 percent;
the balance of magnesium (Mg) and inevitable impurities, and the sum of the weight percentages of the components is 100 percent.
Example 4
The embodiment 4 of the invention provides a degradable magnesium alloy downhole tool bridge plug material and a preparation method of the degradable magnesium alloy downhole tool bridge plug material, and the specific implementation mode is the same as that of the embodiment 2, except that the degradable magnesium alloy downhole tool bridge plug material comprises the following components in percentage by weight:
zinc (Zn): 0.6 percent;
copper (Cu): 0.2 percent;
manganese (Mn): 0.25 percent;
nickel (Ni): 0.2 percent;
aluminum (Al): 8.5 percent;
antimony (Sb): 0.15 percent;
the balance of magnesium (Mg) and inevitable impurities, and the sum of the weight percentages of the components is 100 percent.
Example 5
The embodiment 5 of the invention provides a degradable magnesium alloy downhole tool bridge plug material and a preparation method thereof, and the specific implementation mode is the same as that of the embodiment 1, and the difference is that the degradable magnesium alloy downhole tool bridge plug material comprises the following components in percentage by weight:
zinc (Zn): 0.45 percent;
copper (Cu): 0.1 percent;
manganese (Mn): 0.2 percent;
nickel (Ni): 0.1 percent;
aluminum (Al): 8 percent;
antimony (Sb): 0.1 percent;
the balance of magnesium (Mg) and inevitable impurities, and the sum of the weight percentages of the components is 100 percent.
Example 6
The embodiment 6 of the invention provides a degradable magnesium alloy downhole tool bridge plug material and a preparation method thereof, and the specific implementation mode is the same as that of the embodiment 2, and the difference is that the degradable magnesium alloy downhole tool bridge plug material comprises the following components in percentage by weight:
zinc (Zn): 0.45 percent;
copper (Cu): 0.1 percent;
manganese (Mn): 0.2 percent;
nickel (Ni): 0.1 percent;
aluminum (Al): 8 percent;
antimony (Sb): 0.1 percent;
the balance of magnesium (Mg) and inevitable impurities, and the sum of the weight percentages of the components is 100 percent.
Example 7
The embodiment 7 of the invention provides a degradable magnesium alloy downhole tool bridge plug material and a preparation method of the degradable magnesium alloy downhole tool bridge plug material, and the specific implementation mode is the same as that of the embodiment 1, except that the degradable magnesium alloy downhole tool bridge plug material comprises the following components in percentage by weight:
zinc (Zn): 0.9 percent;
copper (Cu): 0.5 percent;
manganese (Mn): 0.5 percent;
nickel (Ni): 0.5 percent;
aluminum (Al): 9.5 percent;
antimony (Sb): 0.5 percent;
the balance of magnesium (Mg) and inevitable impurities, and the sum of the weight percentages of the components is 100 percent.
Example 8
The embodiment 8 of the invention provides a degradable magnesium alloy downhole tool bridge plug material and a preparation method thereof, and the specific implementation mode is the same as that of the embodiment 2, and the difference is that the degradable magnesium alloy downhole tool bridge plug material comprises the following components in percentage by weight:
zinc (Zn): 0.9 percent;
copper (Cu): 0.5 percent;
manganese (Mn): 0.5 percent;
nickel (Ni): 0.5 percent;
aluminum (Al): 9.5 percent;
antimony (Sb): 0.5 percent;
the balance of magnesium (Mg) and inevitable impurities, and the sum of the weight percentages of the components is 100 percent.
Example 9
The embodiment 9 of the invention provides a degradable magnesium alloy downhole tool bridge plug material and a preparation method of the degradable magnesium alloy downhole tool bridge plug material, and the specific implementation mode is the same as that of the embodiment 1, except that the degradable magnesium alloy downhole tool bridge plug material comprises the following components in percentage by weight:
zinc (Zn): 0.4 percent;
copper (Cu): 0.05 percent;
manganese (Mn): 0.1 percent;
nickel (Ni): 0.7 percent;
aluminum (Al): 8 percent;
antimony (Sb): 0.05 percent;
the balance of magnesium (Mg) and inevitable impurities, and the sum of the weight percentages of the components is 100 percent.
Example 10
The embodiment 10 of the invention provides a degradable magnesium alloy downhole tool bridge plug material and a preparation method of the degradable magnesium alloy downhole tool bridge plug material, and the specific implementation mode is the same as that of the embodiment 2, except that the degradable magnesium alloy downhole tool bridge plug material comprises the following components in percentage by weight:
zinc (Zn): 0.4 percent;
copper (Cu): 0.05 percent;
manganese (Mn): 0.1 percent;
nickel (Ni): 0.7 percent;
aluminum (Al): 8 percent;
antimony (Sb): 0.05 percent;
the balance of magnesium (Mg) and inevitable impurities, and the sum of the weight percentages of the components is 100 percent.
Performance evaluation
1. Mechanical properties
And (3) carrying out mechanical property test on the bridge plug material of the degradable magnesium alloy downhole tool obtained in the examples 1-10 according to GB/T13820-2018.
2. Corrosion rate
The degradable magnesium alloy downhole tool bridge plug materials obtained in examples 1-10 were subjected to corrosion testing in a 3% potassium chloride solution at 92 ℃.
The results are shown in Table 1.
TABLE 1 bridge plug materials of degradable magnesium alloy downhole tools obtained in examples 1-10
The experimental result shows that the magnesium alloy has high mechanical strength and can be dissolved in the solution containing electrolyte. The magnesium alloy is used for manufacturing the tool for constructing the bridge plug material of the underground tool, the tool can be completely degraded after completing the work task, the problems of easy jamming and channel blockage do not exist, the drilling and grinding recovery process is omitted, the engineering difficulty is reduced, and the construction efficiency is improved.
The foregoing examples are merely illustrative and serve to explain some of the features of the method of the present invention. The appended claims are intended to claim as broad a scope as is contemplated, and the examples presented herein are merely illustrative of selected implementations in accordance with all possible combinations of examples. Accordingly, it is applicants' intention that the appended claims are not to be limited by the choice of examples illustrating features of the invention. The use of some numerical ranges in the claims also includes sub-ranges within their range, and variations in these ranges are also to be construed as being covered by the appended claims where possible.
Claims (9)
1. The degradable magnesium alloy bridge plug material for the downhole tool is characterized by comprising the following components in percentage by weight:
zinc (Zn): 0.45% -0.9%;
copper (Cu): 0.1% -0.5%;
manganese (Mn): 0.2% -0.5%;
nickel (Ni): 0.1% -0.5%;
aluminum (Al): 8% -9.5%;
antimony (Sb): 0.1% -0.5%;
the balance of magnesium (Mg) and inevitable impurities, wherein the sum of the weight percentages of the components is 100 percent;
the preparation method of the degradable magnesium alloy downhole tool bridge plug material comprises the following steps:
(1) smelting preparation: cleaning the interior of the crucible, hanging the crucible into a resistance furnace, starting the resistance furnace until the crucible is heated to be dark red, and scattering a second fusing agent on the surface of the crucible;
(2) adding materials and refining: taking metal magnesium, metal zinc, metal aluminum, metal copper, a magnesium-manganese intermediate alloy, a magnesium-nickel intermediate alloy and antimony trioxide as raw materials, mixing the raw materials according to the composition and the weight percentage content, under the protection of inert gas, firstly adding the metal magnesium, the metal zinc and the metal aluminum, preheating the magnesium-manganese intermediate alloy and the magnesium-nickel intermediate alloy on a furnace platform, then adding the magnesium-manganese intermediate alloy and the antimony trioxide at 750 ℃, finally adding the magnesium-nickel intermediate alloy and the metal copper at 780 ℃, and uniformly stirring to alloy the raw materials;
(3) intermediate sampling: sampling to detect chemical components, sealing the cover and standing for one hour after the chemical components are qualified;
(4) and (3) casting rod forming: after the sample in the step (3) is qualified, semi-continuously casting the sample at 740 ℃ to form a casting bar;
(5) and (3) hot extrusion process: and (4) carrying out a hot extrusion process on the sample in the step (4).
2. The degradable magnesium alloy bridge plug material for the downhole tool of claim 1, wherein the degradable magnesium alloy bridge plug material comprises the following components in percentage by weight:
zinc (Zn): 0.6 to 0.8 percent;
copper (Cu): 0.2 to 0.4 percent;
manganese (Mn): 0.25 to 0.4 percent;
nickel (Ni): 0.2 to 0.4 percent;
aluminum (Al): 8.5 to 9.2 percent;
antimony (Sb): 0.15 to 0.4 percent;
the balance of magnesium (Mg) and inevitable impurities, and the sum of the weight percentages of the components is 100 percent.
3. The degradable magnesium alloy bridge plug material for the downhole tool of claim 2, wherein the degradable magnesium alloy bridge plug material comprises the following components in percentage by weight:
zinc (Zn): 0.7 percent;
copper (Cu): 0.3 percent;
manganese (Mn): 0.3 percent;
nickel (Ni): 0.25 percent;
aluminum (Al): 9.2 percent;
antimony (Sb): 0.3 percent;
the balance of magnesium (Mg) and inevitable impurities, and the sum of the weight percentages of the components is 100 percent.
4. The degradable magnesium alloy downhole tool bridge plug material of any one of claims 1-3, wherein the degradable magnesium alloy downhole tool bridge plug material is used for a construction tool in a production oil and gas field exploitation process.
5. A method for preparing a degradable magnesium alloy bridge plug material for a downhole tool according to any one of claims 1 to 4, wherein the method at least comprises the following steps:
(1) smelting preparation: cleaning the interior of the crucible, hanging the crucible into a resistance furnace, starting the resistance furnace until the crucible is heated to be dark red, and scattering a second fusing agent on the surface of the crucible;
(2) adding materials and refining: taking metal magnesium, metal zinc, metal aluminum, metal copper, a magnesium-manganese intermediate alloy, a magnesium-nickel intermediate alloy and antimony trioxide as raw materials, mixing the raw materials according to the composition and the weight percentage content, under the protection of inert gas, firstly adding the metal magnesium, the metal zinc and the metal aluminum, preheating the magnesium-manganese intermediate alloy and the magnesium-nickel intermediate alloy on a furnace platform, then adding the magnesium-manganese intermediate alloy and the antimony trioxide at 750 ℃, finally adding the magnesium-nickel intermediate alloy and the metal copper at 780 ℃, and uniformly stirring to alloy the raw materials;
(3) intermediate sampling: sampling to detect chemical components, sealing the cover and standing for one hour after the chemical components are qualified;
(4) and (3) casting rod forming: after the sample in the step (3) is qualified, semi-continuously casting the sample at 740 ℃ to form a casting bar;
(5) and (4) after the cast rod is formed in the step (4), a hot extrusion process is further included.
6. The method for preparing the bridge plug material of the degradable magnesium alloy downhole tool as claimed in claim 5, wherein in the step (1), in preparation for smelting, the temperature of the molten liquid in the crucible heated by the resistance furnace is controlled at 690-780 ℃.
7. The method for preparing the degradable magnesium alloy bridge plug material for the downhole tool according to claim 5, wherein in the step (2), the purities of the metal magnesium, the metal zinc, the metal aluminum and the metal copper are respectively more than or equal to 99.9%.
8. The method for preparing a bridge plug material of a degradable magnesium alloy downhole tool according to claim 5, wherein during the charging and refining process in the step (2), the melt is fully stirred and sprayed with a second fusing agent to extinguish fire, so that the melt is alloyed.
9. The method for preparing the bridge plug material of the degradable magnesium alloy downhole tool according to claim 5, wherein before the sampling in the step (3), the temperature is 760 ℃ for refining, a fifth fusing agent is thrown, after the alloy liquid is uniformly stirred to be bright, the alloy liquid is kept stand for ten minutes, and then the sampling operation is carried out.
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| PCT/CN2020/126647 WO2021129178A1 (en) | 2019-12-24 | 2020-11-05 | Degradable magnesium alloy downhole tool bridge plug material and preparation method therefor |
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| CN111996428A (en) * | 2020-08-28 | 2020-11-27 | 深圳市苏德技术有限公司 | Soluble magnesium alloy and preparation method and application thereof |
| CN115053003A (en) * | 2021-01-08 | 2022-09-13 | 上海格邦自动化科技有限公司 | Rapidly-dissolved high-plasticity soluble magnesium alloy material and preparation method thereof |
| CN115466890B (en) * | 2022-09-19 | 2023-12-01 | 重庆科技学院 | High-strength and high-toughness Cu-containing magnesium alloy material capable of being rapidly degraded and preparation method thereof |
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| US11167343B2 (en) * | 2014-02-21 | 2021-11-09 | Terves, Llc | Galvanically-active in situ formed particles for controlled rate dissolving tools |
| GB201413327D0 (en) * | 2014-07-28 | 2014-09-10 | Magnesium Elektron Ltd | Corrodible downhole article |
| JP6692411B2 (en) * | 2016-03-31 | 2020-05-13 | 株式会社栗本鐵工所 | Degradable Mg alloy |
| JP2017206757A (en) * | 2016-05-20 | 2017-11-24 | 不二ライトメタル株式会社 | Resolvable magnesium alloy |
| CN106929726B (en) * | 2017-02-20 | 2018-06-29 | 岳阳宇航新材料有限公司 | A kind of degradable magnesium alloy downhole tool submount material and preparation method thereof |
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