CN112708813A - Soluble magnesium alloy material for oil and gas exploitation tool and preparation method thereof - Google Patents
Soluble magnesium alloy material for oil and gas exploitation tool and preparation method thereof Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title abstract description 8
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- 238000005260 corrosion Methods 0.000 claims abstract description 62
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- 238000000034 method Methods 0.000 claims abstract description 38
- 229910052802 copper Inorganic materials 0.000 claims abstract description 33
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 28
- 230000008569 process Effects 0.000 claims abstract description 28
- 238000010438 heat treatment Methods 0.000 claims abstract description 17
- 239000011777 magnesium Substances 0.000 claims description 43
- 238000001125 extrusion Methods 0.000 claims description 42
- 229910052749 magnesium Inorganic materials 0.000 claims description 14
- 229910052748 manganese Inorganic materials 0.000 claims description 13
- 229910052710 silicon Inorganic materials 0.000 claims description 13
- 238000003723 Smelting Methods 0.000 claims description 12
- 230000032683 aging Effects 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 12
- 229910052726 zirconium Inorganic materials 0.000 claims description 12
- 239000000155 melt Substances 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 11
- 229910052712 strontium Inorganic materials 0.000 claims description 10
- 229910052718 tin Inorganic materials 0.000 claims description 10
- 229910052727 yttrium Inorganic materials 0.000 claims description 10
- 239000013078 crystal Substances 0.000 claims description 9
- 230000000694 effects Effects 0.000 claims description 9
- 238000004519 manufacturing process Methods 0.000 claims description 9
- 229910052725 zinc Inorganic materials 0.000 claims description 9
- 229910019083 Mg-Ni Inorganic materials 0.000 claims description 8
- 229910019403 Mg—Ni Inorganic materials 0.000 claims description 8
- 229910052791 calcium Inorganic materials 0.000 claims description 8
- 239000008399 tap water Substances 0.000 claims description 8
- 235000020679 tap water Nutrition 0.000 claims description 8
- 230000005484 gravity Effects 0.000 claims description 7
- 238000005728 strengthening Methods 0.000 claims description 7
- 238000001192 hot extrusion Methods 0.000 claims description 6
- 239000002893 slag Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 238000005266 casting Methods 0.000 claims description 5
- 229910002059 quaternary alloy Inorganic materials 0.000 claims description 5
- 229910017518 Cu Zn Inorganic materials 0.000 claims description 4
- 229910017752 Cu-Zn Inorganic materials 0.000 claims description 4
- 229910017943 Cu—Zn Inorganic materials 0.000 claims description 4
- TVZPLCNGKSPOJA-UHFFFAOYSA-N copper zinc Chemical compound [Cu].[Zn] TVZPLCNGKSPOJA-UHFFFAOYSA-N 0.000 claims description 4
- 229910002058 ternary alloy Inorganic materials 0.000 claims description 4
- 230000015572 biosynthetic process Effects 0.000 claims description 3
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- 239000003921 oil Substances 0.000 description 16
- 239000011701 zinc Substances 0.000 description 12
- 239000006104 solid solution Substances 0.000 description 10
- 239000011572 manganese Substances 0.000 description 9
- 239000000463 material Substances 0.000 description 8
- 238000005553 drilling Methods 0.000 description 4
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- 238000007670 refining Methods 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- 229910019758 Mg2Ni Inorganic materials 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
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- 239000007787 solid Substances 0.000 description 3
- 229910000838 Al alloy Inorganic materials 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
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- 238000005275 alloying Methods 0.000 description 2
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- -1 magnesium-aluminum-zinc Chemical compound 0.000 description 2
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- 229910000914 Mn alloy Inorganic materials 0.000 description 1
- 229910000676 Si alloy Inorganic materials 0.000 description 1
- 229910001297 Zn alloy Inorganic materials 0.000 description 1
- MKPXGEVFQSIKGE-UHFFFAOYSA-N [Mg].[Si] Chemical compound [Mg].[Si] MKPXGEVFQSIKGE-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
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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
-
- 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
-
- 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
- C22C23/06—Alloys based on magnesium with a rare earth metal as the next major constituent
-
- 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
- C22F1/06—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of magnesium or alloys based thereon
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- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
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- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a soluble magnesium alloy material for an oil and gas exploitation tool and a preparation method thereof. Ni and Cu are used as main elements to form Mg-Ni-Cu alloy, and the type and content of Mg-Ni-Cu alloy elements are regulated to form soluble magnesium alloy containing different second phases, so that the potential difference between the matrix and the second phases is changed, and the alloy dissolution is accelerated. The corrosion rate of Mg-Ni-Cu alloy in 0.05% KCl solution at 50 ℃ is 3-35 Mg-cm‑2·h‑1The corrosion rates in 3% KCl solution at 25 ℃ and 93 ℃ are respectively 8-30 mg-cm‑2·h‑1And 130-285 mg/cm‑2·h‑1. The soluble Mg-Ni-Cu alloy prepared by the invention has the advantages of good toughness, good corrosion resistance and good corrosion resistanceSimple process, low cost, high dissolving speed and the like, and can meet the dissolving requirements of different oil and gas exploitation tools. In addition, the mechanical property can be further improved by regulating and controlling a heat treatment system and a deformation process, so that excellent comprehensive properties are obtained. The Mg-Ni-Cu soluble magnesium alloy has wide application prospect in the field of oil and gas exploitation.
Description
Technical Field
The invention relates to a soluble magnesium alloy material for oil and gas exploitation tools and a preparation method thereof.
Background
In recent years, the production of low permeability fields, most of which are distributed in formations of different depths, has been increasingly appreciated as the exploration of unconventional fields has gained important findings. At present, the commonly used technologies for low-permeability oil and gas field exploitation include water injection, fracturing and the like. The staged fracturing technology of the horizontal well is an important means for improving low-permeability oil gas and increasing the yield of the oil gas well.
Downhole tools (e.g., fracturing balls, bridge plugs, etc.) are important components of oil and gas production. Most downhole tool materials use steel and composite materials. Steel cannot dissolve or the dissolution rate is too slow to facilitate flowback operations. Composites tend to crush and become brittle, their compressive strength does not meet the required performance requirements, and in some cases, certain composites containing fibers or polymers may block the channels of oil drilling. In severe cases, drilling must be performed again, which leads to an increase in cost.
Therefore, it is necessary to research and develop soluble tool materials under oil wells, such as soluble fracturing bridge plugs and fracturing balls, and the like, and the soluble fracturing bridge plugs and fracturing balls have the advantages that the soluble fracturing bridge plugs and fracturing balls can be completely dissolved within a certain time after fracturing operation is completed, secondary drilling is not needed, and the oil and gas exploitation efficiency can be greatly improved.
The magnesium alloy has a low density (1.8 g/cm)3) And corrosion potential (-2.37V, 25 ℃), high specific strength and specific stiffness, making it a preferred material for soluble tools. For example, a ball seat inside the sliding sleeve is prepared by adopting a soluble magnesium alloy material, and a corrosion inhibition material is coated on the surface. During the fracturing process, the corrosion inhibiting material is first abraded by the fracturing sand, and then the ball seat reacts with the injected fracturing fluid (typically consisting of a pad fluid, a sand-carrying fluid, and a displacement fluid). After the fracturing work is finished, the ball seat can be automatically dissolved under the action of the flowback liquid, so that the drilling removal at the later stage is avoided, and the cost is reduced.
In CN 106536773A, the Temocie Welch et al, magnesium electronics, Inc. provided that at least 50mg/cm could be achieved at 93 deg.C under 15% KCl2Magnesium alloy per day corrosion rate and gives the corrosion rate and mechanical properties (mainly yield strength, tensile strength and elongation) of the alloy under different environments. Different oil and gas fields are in different environments, such as 3% KCl, clear water (0.05% KCl) and the like, and the performance requirements of the alloy are different due to different temperatures, and all the requirements are considered.
The Baker Hughes corporation in CN 107002475A discloses an anchoring device method, which comprises: providing a degradable substrate with a first hardness and applying a granular gripping material to the outer extent of the degradable substrate, wherein the granular gripping material has a second hardness greater than the first hardness. The degradable substrate is mainly magnesium alloy, including binary or ternary magnesium alloy such as magnesium-silicon alloy, magnesium-aluminum-zinc alloy, magnesium-aluminum-manganese alloy and the like. Although the inventor of intelligent et al provides the element composition of the alloy, the specific composition and the preparation method of the alloy are not mentioned, and the mechanical property and the corrosion rate of the alloy material are not given.
Gaurav Agrawal patented soluble tooling and methods in US 2011/0132619 a1 in the name of Baker Hughes corporation, where the soluble tooling is formed from a metal powder comprising a continuous cellular nanomatrix, a particulate material dispersed in the cellular nanomatrix, and a solid bond layer extending throughout the nanomatrix. Wherein the particulate material consists essentially of Mg-Zn, Mg-Al, Mg-Mn, Mg-Zn-Y, Mg-Al-Si or Mg-Al-Zn, and the nanomatrix consists essentially of Al, Zn, Mn, Mg, Mo, W, Cu, Fe, Si, Ca, Co, Ta, Re or Ni or an oxide, carbide or nitride thereof, or a combination of any of the foregoing materials. In the metallurgical bonding of powders, the conditions are relatively harsh, such as the application of pressure and temperature. The problem with this powder metallurgy method is that the cost of the product increases, the process is more complex and not suitable for the production of large size downhole tools, such as soluble fracture plugs.
Lynn Frazier discloses a downhole tool made from a soluble aluminum/magnesium alloy and a polymeric acid (patent US 10,352,125B 2) which relates to a downhole tool comprising slips, mandrels, etc. In one embodiment, the aluminum alloy is formed by Al and Mg, Si, Cu, Li or Mn, Zn and In metal elements, and the elements can improve the strength of the alloy or increase the downhole dissolution rate, but the content of the elements In the alloy and the specific alloy components are not involved, the indexes of the alloy such as tensile strength, yield strength and elongation cannot be known, and the indexes cannot be compared with the requirements of actual working conditions.
Therefore, in view of the composition and process requirements of soluble magnesium alloy materials for oil and gas production tools, the designed soluble magnesium alloy not only needs to control the corrosion rate to meet the requirements of certain specific downhole tools, but also has certain mechanical properties.
Disclosure of Invention
The invention mainly relates to a soluble magnesium alloy material and a preparation method thereof, which are mainly applied to soluble tools for oil and gas exploitation, but are not limited to the preparation and use of oil and gas well tools completely, and can also be applied to other fields.
The invention relates to a soluble magnesium alloy material for an oil and gas exploitation tool, which is characterized in that: the alloy has a yield strength of 140-270 MPa, a tensile strength of 220-305 MPa and an elongation of 1-14%. The corrosion rate in 0.05 percent KCl solution at 50 ℃ is 3-35 mg-cm-2·h-1The corrosion rates in 3% KCl solutions at 25 ℃ and 93 ℃ are respectively 8-30 mg-cm-2·h-1And 130-285 mg/cm-2·h-1。
Furthermore, the soluble magnesium alloy takes Ni and Cu as main elements to form Mg-Ni-Cu series ternary alloy;
ni: 1.5-10.0 wt.%, Cu: 1.5-10.0 wt.%, the balance being Mg;
formation of Mg in ternary Mg-Ni-Cu alloys2Ni and Mg2The dual phase structure of Cu promotes the corrosion of the alloy.
Further, the soluble magnesium alloy forms a Mg-Ni-Cu ternary alloy with Ni and Cu as main elements, and more preferably comprises the following alloy components:
ni: 2.0-6.0 wt.%, Cu: 2.0-6.0 wt.%, and the balance being Mg.
Furthermore, the soluble magnesium alloy takes Ni and Cu as main elements, and M element is added into Mg-Ni-Cu alloy to form Mg-Ni-Cu-M quaternary alloy;
Ni：1.5～10.0wt.％，Cu：1.5～10.0wt.％；
the other elements are one of Ag, Ca, Sn, Si and Sr elements, wherein the ratio of Ag: 0.1-5.0 wt.%, Ca: 0.1-5.0 wt.%, Sn: 0.1-5.0 wt.%, Si: 0.1-5.0 wt.%, Sr: 0.1-5.0 wt.%;
the balance being Mg, the contents of Ni and Cu being greater than the contents of the elements represented by M;
when the M element is Ag, Mg is formed in the Mg-Ni-Cu alloy in addition to the two-phase structure4An Ag phase; when the M element is Ca, Mg is formed in the Mg-Ni-Cu alloy in addition to the two-phase structure2A Ca phase; when M is Sn, Mg is formed in the Mg-Ni-Cu alloy in addition to the two-phase structure2A Sn phase; when M is Si, Mg is formed in the Mg-Ni-Cu alloy in addition to the two-phase structure2A Si phase; when M is Sr, Mg is formed in the Mg-Ni-Cu alloy in addition to the two-phase structure17Sr12And (4) phase(s). Different second phases formed by adding M element in Mg-Ni-Cu series alloy can effectively block dislocation movement and generate strengthening effect.
Further, the soluble magnesium alloy is formed by adding an M element to a Mg-Ni-Cu alloy with Ni and Cu as main elements to form a Mg-Ni-Cu-M quaternary alloy, and more preferably comprises the following alloy components:
Ni：1.5～6.0wt.％；Cu：1.5～6.0wt.％；
m element is one of Ag, Ca, Sn, Si and Sr elements, wherein Ag: 0.5-4.0 wt.%, Ca: 0.5-2.5 wt.%, Sn: 0.5-2.0 wt.%, Si: 0.5-4.0 wt.%, Sr: 0.5-4.0 wt.%;
the balance being Mg, the contents of Ni and Cu being greater than the contents of the elements represented by M.
Furthermore, the soluble magnesium alloy takes Ni and Cu as main elements, and H and I elements are added on the basis of Mg-Ni-Cu system to form Mg-Ni-Cu-M-N system quinary alloy;
Ni：2.0～10.0wt.％；Cu：2.0～10.0wt.％；
h is Gd and one of Y elements, wherein the ratio of Gd: 0.5-9.0 wt.%, Y: 0.5-6.0 wt.%;
i is one of Zn, Mn and Zr, wherein Zn: 0.1-1.0 wt.%, Mn: 0.1-1.0 wt.%, Zr: 0.01-0.2 wt.%;
the balance being Mg, the contents of Ni and Cu being higher than the contents of elements represented by H and I;
LPSO phases (Mg-Ni/Cu-Gd/Y and Mg-Ni/Cu-Zn) with different shapes and compositions are formed in the Zn-containing Mg-Ni-Cu series quinary alloy, and play a role in the corrosion and mechanical properties of the Mg-Ni-Cu series alloy; the Mg-Ni-Cu series quinary alloy containing Mn and Zr can refine crystal grains and improve mechanical strength.
Furthermore, the soluble magnesium alloy takes Ni and Cu as main elements, and H and I elements are added on the basis of Mg-Ni-Cu system to form Mg-Ni-Cu-M-N system quinary alloy, and more preferable alloy components are as follows:
Ni：2.0～6.0wt.％；Cu：2.0～6.0wt.％；
m is Gd and one of Y elements, wherein the ratio of Gd: 1.0-4.0 wt.%, Y: 1.0-4.0 wt.%;
n is one of Zn, Mn and Zr, wherein Zn: 0.5-1.0 wt.%, Mn: 0.5-1.0 wt.%, Zr: 0.1-0.2 wt.%;
the balance being Mg, the contents of Ni and Cu being higher than the contents of the elements represented by M and N.
In the conventional magnesium alloy, Ni and Cu as harmful elements deteriorate the corrosion properties of the alloy, and the higher the content is, the more remarkable the reduction in corrosion properties is. In order to meet the requirement of high corrosion rate required by oil well exploitation, Ni and Cu are used as main elements to form Mg-Ni-Cu series alloy which contains Mg2Ni and Mg2The Cu dual-phase structure and the Cu dual-phase structure have the effect of overlapping the influence on the corrosion performance of the alloy and play a role together.
In the actual service process of the soluble tool, besides corrosion performance, the mechanical property of the alloy is also an important index, and alloying is one of effective methods for improving the performance of the magnesium alloy.
Of Ag in magnesium alloysThe solid solubility is high, the solid solution and aging strengthening effects can be generated, and when Ag is added into Mg-Ni-Cu, Mg is formed4An Ag phase. After solution and extrusion deformation, Mg4The second phase of Ag can block dislocation movement in the deformation process, the mechanical strength of the alloy is improved, and meanwhile, the addition of Ag plays a role in promoting corrosion and accelerating the corrosion.
Because the magnesium alloy is in a close-packed hexagonal structure, basal plane slippage systems are few, and the addition of Ca can weaken the texture, thereby improving the plastic forming capability and the plasticity of the magnesium alloy, and simultaneously forming Mg in the Mg-Ni-Cu alloy2The Ca phase is separated out at the grain boundary to promote the dynamic recrystallization process, thereby achieving the effect of refining grains.
Sn can reduce the critical slitting stress of the conical surface of the magnesium alloy, improve the forming capability of the magnesium alloy and reduce the cracking tendency in the deformation process. Adding Sn to Mg-Ni-Cu alloy to form Mg2The Sn phase is distributed in the crystal interior and the crystal boundary and is an effective strengthening phase.
Si is also used as an impurity element in the traditional magnesium alloy, and Si is added into Mg-Ni-Cu alloy to form Mg2The Si phase also promotes corrosion and improves the castability of the alloy.
Sr has lower solid solubility in magnesium alloy, and can inhibit the growth of crystal grains in the smelting process of Mg-Ni-Cu alloy, thereby achieving stronger grain refinement effect.
Rare earth elements Gd and Y are added into the Mg-Ni-Cu alloy, so that not only can crystal grains be refined, but also the effect of solid solution strengthening is achieved, and the mechanical property of the alloy is improved. When the magnesium alloy contains Ni, Cu and rare earth, an LPSO phase can be formed, for example, the Mg, the Ni and the Y form 14H-LPSO, which plays an important role in strengthening the alloy.
Zn plays a role in solid solution strengthening in the magnesium alloy and has important significance for improving the strength of the alloy. LPSO phases (Mg-Ni/Cu-Gd/Y and Mg-Ni/Cu-Zn) with different shapes and compositions are formed in the Mg-Ni-Cu series quinary alloy containing Zn and RE, and play a role in the corrosion and mechanical properties of the Mg-Ni-Cu series alloy.
The Mn element has a certain grain refining effect and can improve the strength of the Mg-Ni-Cu alloy to a certain extent.
The Zr added into the magnesium alloy has obvious grain refining effect. According to Hall-Petch relation, the strength and the elongation of the alloy can be effectively improved by grain refinement. However, when the Zr content exceeds 0.2 wt.%, Ni and Zr form a precipitate phase, thereby impairing the mechanical properties of the Mg-Ni-Cu based alloy.
The preparation method of the soluble magnesium alloy comprises any 1 of the following 2 methods:
the process A comprises the following steps: gravity casting → water cooling after solution treatment → preheating before extrusion → hot extrusion deformation;
and a process B: gravity casting → water cooling after solution treatment → preheating before extrusion → hot extrusion deformation → aging.
The process is carried out at SF6And CO2Under the protection of gas, smelting at 700-720 ℃, carrying out slag removal and stirring on the melt, heating to 750-760 ℃, preserving heat for 15-20 minutes, and then pouring into a mold by gravity to obtain a needed ingot; the temperature of the solution treatment is 350-520 ℃, the time is 8-24 h, and the solution treatment is immediately carried out and then the solution treatment is put into tap water for cooling at room temperature. The preheating temperature of the sample, the extrusion die and the extrusion cylinder before extrusion is consistent with the extrusion temperature, the preheating time of the sample is 1.5-2.0 h, the preheating time of the extrusion die and the extrusion cylinder is 4-6 h, the extrusion temperature is 350-480 ℃, the extrusion ratio is 7: 1-22.5: 1, and the bar is immediately placed into tap water for cooling after extrusion.
And further, the process B is only to add aging treatment on the basis of the process A, the aging temperature is 175-200 ℃, the aging time is 20-60 hours, and the rod is immediately placed into tap water for cooling after aging.
The invention is not limited to this process route and equivalent performance can be achieved by other different process schemes.
The corrosion rate of the alloy is evaluated by a weight loss method, and the product of the surface area of the alloy and the time is obtained in a unit of mg cm within a certain time (preferably 0.5, 1, 2, 4, 6, 8h and the like) according to the difference ratio of the mass (mg) of the alloy before corrosion to the mass (mg) of the alloy after corrosion-2·h-1。
Compared with the prior art, the invention has the following beneficial effects:
1) in the conventional magnesium alloy, Ni and Cu are used as impurity elements, and the contents thereof are strictly limited. In order to meet the high corrosion rate required by oil and gas exploitation tools, the invention forms Mg-Ni-Cu alloy by introducing Ni and Cu as main alloy elements, wherein the alloy contains Mg2Ni and Mg2And the amount, the shape and the size of the second phase of the Cu are controlled by adjusting the contents of Ni and Cu, so that the corrosion rate of the Mg-Ni-Cu alloy is controlled.
2) On the basis of Mg-Ni-Cu series alloy, other different elements such as Ca, Si and the like are added to form Mg-Ni-Cu series quaternary alloy, and Mg is removed from the alloy2Ni and Mg2In addition to the Cu biphase, Mg is also formed2Ca、Mg2Si and other second phases which can effectively block dislocation movement, improve the mechanical property of the alloy and obtain Mg-Ni-Cu soluble magnesium alloy with excellent comprehensive properties.
3) The rare earth elements are added into the Mg-Ni-Cu alloy, LPSO phases (14H-LPSO or 18R-LPSO) with different shapes and structures can be formed, the LPSO phases (Mg-Ni/Cu-Gd/Y and Mg-Ni/Cu-Zn) with different shapes and compositions are formed in the Zn-containing Mg-Ni-Cu alloy by adding Zn, Zr and the like on the basis, and the corrosion and mechanical properties of the Mg-Ni-Cu alloy are acted together; zr is added to refine the crystal grains of the Mg-Ni-Cu alloy and improve the mechanical strength.
4) The soluble magnesium alloy material is obtained through heat treatment and deformation processes, the process is simple, the cost is low, the efficiency is high, the distribution, the size, the morphology and the like of the microstructure and the second phase in the alloy can be improved, and simultaneously, the mechanical property and the corrosion property of the Mg-Ni-Cu alloy are improved through refining crystal grains through the deformation process.
5) The method can be used for preparing large-size downhole soluble tools such as soluble bridge plugs and the like by adopting traditional casting, hot deformation processes and the like.
6) The potential difference between the substrate and the second phase is changed by adding alloying elements, so that the corrosion rate of the alloy is regulated and controlled, and the use requirement of underground working conditions is met.
7) The soluble magnesium alloy can be completely dissolved in KCl solution, and formed corrosion products are discharged along with the return discharge liquid after underground operation, so that blockage is not generated.
8) By regulating and controlling parameters such as a heat treatment system, an extrusion ratio, an extrusion temperature and the like, the alloy has uniform internal structure and fine crystal grains, thereby effectively improving the mechanical property of the alloy. By the alloy design and process regulation of the invention, the soluble magnesium alloy material with excellent comprehensive mechanical and corrosion properties is obtained.
The term "corrosion performance" referred to in the present invention has the same meaning as the terms of corrosion rate, corrosion behavior and the like.
The soluble magnesium alloy is mainly used for oil and gas exploitation tools, and can obtain required tool components after being processed and processed, and simultaneously obtain the mechanical property and the corrosion property required by a fracturing tool.
The production tool is preferably a fracturing ball, ball seat, packer, etc., more preferably a fracturing ball.
Drawings
The invention will be further described with reference to the following drawings, in which:
FIG. 1 is a photograph of the alloy of example 1 after solutionizing.
FIG. 2 is a scanning magnified photograph of the alloy of example 1 after solutionizing.
FIG. 3 is an as-cast microstructure of the Mg-6Ni-5Cu-2.5Ag alloy in example 4.
FIG. 4 is a microstructure diagram of the Mg-6Ni-5Cu-2.5Ag alloy of example 4 after solution treatment at 450 ℃ for 12 hours.
Detailed Description
Example 1.
At SF6And CO2Under the protection of gas, smelting at 710-720 ℃, carrying out slag dragging and stirring treatment on the melt, heating to 755-760 ℃, preserving the temperature for 15 minutes, and then pouring into a mold to obtain an ingot with a soluble magnesium alloy component of Mg-6Ni-5Cu-2Ca (wt.%). Carrying out solution treatment on the cast ingot at 450 ℃ for 12h, extruding the solid solution alloy at 420 ℃ with the extrusion ratio of 22.5, and finally obtaining the extruded bar.
To simulate different environments of oil exploitation, the research of the temperature at room temperature (25 ℃) and the research of the temperature at room temperatureThe corrosion rate of the alloy at 93 ℃, 3% of KCl and 0.05% of KCl at 50 ℃ is tested by a weight loss method. The mechanical property test is carried out according to the national standard, and the strain rate is 10-3/s。
The mechanical properties and corrosion properties of the alloy Mg-6Ni-5Cu-2Ca are shown in Table 1.
Example 2.
At SF6And CO2Under the protection of gas, smelting at 700-710 ℃, carrying out slag dragging and stirring treatment on the melt, heating to 750-755 ℃, preserving heat for 18 minutes, and then pouring into a mold to finally obtain an ingot with a soluble magnesium alloy component of Mg-4Ni-5Cu-2Y-0.5Mn (wt.%). And (3) carrying out heat treatment on the cast ingot at 520 ℃ for 12h, carrying out hot extrusion deformation on the solid solution alloy at 480 ℃ with the extrusion ratio of 7, and carrying out aging on the extruded alloy at 250 ℃ for 15h to obtain an aged bar.
The corrosion rate and mechanical properties were measured in the same manner as in example 1.
The alloy Mg-4Ni-5Cu-2Y-0.5Mn has mechanical properties and corrosion properties shown in Table 1.
Example 3.
At SF6And CO2Under the protection of gas, smelting at 715-720 ℃, carrying out slag-dragging and stirring treatment on the melt, heating to 750-760 ℃, preserving heat for 16 minutes, and then pouring into a mold to obtain an ingot with a soluble magnesium alloy component of Mg-1.5Ni-4Cu-1Sn (wt.%). Carrying out solution treatment on the cast ingot at 480 ℃ for 24h, extruding the solid solution alloy at 430 ℃ with the extrusion ratio of 15.6, and finally obtaining the extruded bar.
The corrosion rate and mechanical properties were measured in the same manner as in example 1.
The mechanical properties and corrosion properties of the alloy Mg-1.5Ni-4Cu-1Sn are shown in Table 1.
Example 4.
At SF6And CO2Under the protection of gas, smelting at 700-710 ℃, carrying out slag-dragging and stirring treatment on the melt, heating to 750-760 ℃, keeping the temperature for 15 minutes, and then pouringAnd (3) injecting the mixture into a mold to obtain an ingot with a soluble magnesium alloy composition of Mg-6Ni-5Cu-2.5Ag (wt.%). Carrying out solution treatment on the cast ingot at 450 ℃ for 12h, extruding the solid solution alloy at 370 ℃ and the extrusion ratio of 22.5, and finally obtaining the extruded bar.
The corrosion rate and mechanical properties were measured in the same manner as in example 1.
The mechanical properties and corrosion properties of the alloy Mg-6Ni-5Cu-2.5Ag are shown in Table 1.
Example 5.
At SF6And CO2Under the protection of gas, smelting at 700-710 ℃, carrying out slag-dragging and stirring treatment on the melt, heating to 750-760 ℃, preserving heat for 20 minutes, and then pouring into a mold to obtain an ingot with a soluble magnesium alloy component of Mg-5Ni-3Cu-1Si (wt.%). And (3) carrying out solution treatment on the cast ingot at 465 ℃ for 12h, extruding the solid solution alloy at 440 ℃ with the extrusion ratio of 15.6, and finally obtaining the extruded bar.
The corrosion rate and mechanical properties were measured in the same manner as in example 1.
The mechanical properties and corrosion properties of the alloy Mg-5Ni-3Cu-1Si are shown in Table 1.
Example 6
At SF6And CO2Under the protection of gas, smelting at 700-720 ℃, carrying out slag-dragging and stirring treatment on the melt, heating to 750-760 ℃, preserving heat for 15-20 minutes, and then pouring into a mold to obtain an ingot with a soluble magnesium alloy component of Mg-5Ni-3.5Cu (wt.%). Carrying out solution treatment on the cast ingot at 450 ℃ for 12h, extruding the solid solution alloy at 420 ℃ with the extrusion ratio of 22.5, and finally obtaining the extruded bar.
The corrosion rate and mechanical properties were measured in the same manner as in example 1.
The mechanical properties and corrosion properties of the alloy Mg-5Ni-3.5Cu are shown in Table 1.
Example 7
At SF6And CO2Smelting at 700-710 ℃ under the protection of gasAnd carrying out slag dragging and stirring treatment on the melt, heating to 750-760 ℃, preserving heat for 15 minutes, and then pouring into a mold to obtain an ingot with a soluble magnesium alloy component of Mg-3Ni-2Cu-2Gd-0.2Zr (wt.%). The cast ingot is subjected to solution treatment at 500 ℃ for 20 h. The hot extrusion temperature was 460 ℃ and the extrusion ratio was 16.7, to obtain an extruded rod.
The corrosion rate and mechanical properties were measured in the same manner as in example 1.
The alloy Mg-3Ni-2Cu-2Gd-0.2Zr has the mechanical properties and the corrosion properties shown in Table 1.
Example 8
At SF6And CO2Under the protection of gas, smelting at 705-715 ℃, carrying out slag-dragging and stirring treatment on the melt, heating to 750-760 ℃, preserving the temperature for 20 minutes, and then pouring into a mold to obtain an ingot with a soluble magnesium alloy component of Mg-3Ni-3Cu-1Gd-0.5Zn (wt.%). Carrying out solution treatment on the cast ingot at 500 ℃ for 12h, extruding the solid solution alloy at 480 ℃ with the extrusion ratio of 7, and carrying out aging treatment on the extruded alloy at 150 ℃ for 60h to finally obtain an aged bar.
The corrosion rate and mechanical properties were measured in the same manner as in example 1.
The alloy Mg-3Ni-3Cu-1Gd-0.5Zn has the mechanical properties and the corrosion properties shown in the table 1.
Table 1 shows the mechanical and corrosion properties of all alloys in the examples.
All of the examples according to the present invention show that the Mg-Ni-Cu based alloy has excellent corrosion performance when Ni and Cu are used as main elements. On the premise of maintaining the required corrosion rate, some other elements are added into the Mg-Ni-Cu alloy, and the coordination of the relationship between the mechanical property and the corrosion property of the Mg-Ni-Cu alloy is realized by means of heat treatment and deformation processes.
In both FIG. 1 and FIG. 2, the alpha-Mg matrix phase, Mg2Ni、Mg2Cu and other elements. Furthermore, the utility modelGenerally, the same is true of the alloys of the other embodiments.
In different embodiments, the composition, morphology, size and distribution of the second phase are different, the potentials of the alpha-Mg matrix and the second phase are different, the generated potential difference is different, and different corrosion rates are finally obtained. After heat treatment and deformation, the alloy has different capabilities of hindering dislocation movement, thereby obtaining different mechanical properties.
Claims (10)
1. A soluble magnesium alloy material for oil and gas exploitation tools is characterized in that: the yield strength of the alloy is 140-270 MPa, the tensile strength is 220-305 MPa, and the elongation is 1-14%; the corrosion rate of the alloy in 0.05 percent KCl solution at 50 ℃ is 3-35 mg-cm-2·h-1The corrosion rates in 3% KCl solutions at 25 ℃ and 93 ℃ are respectively 8-30 mg-cm-2·h-1And 130-285 mg/cm-2·h-1。
2. The soluble magnesium alloy material according to claim 1, wherein Ni and Cu are used as main elements to form a Mg-Ni-Cu-based ternary alloy;
ni: 1.5-10.0 wt.%, Cu: 1.5-10.0 wt.%, the balance being Mg;
formation of Mg in ternary Mg-Ni-Cu alloys2Ni and Mg2The dual phase structure of Cu promotes the corrosion of the alloy.
3. The soluble magnesium alloy material according to claim 2, wherein Ni and Cu are used as main elements to form a Mg-Ni-Cu-based ternary alloy, and the alloy components are:
ni: 2.0-6.0 wt.%, Cu: 2.0-6.0 wt.%, and the balance being Mg.
4. The soluble magnesium alloy material for oil and gas exploitation tool as claimed in claim 1, wherein Ni and Cu are used as main elements, and an M element is added to an Mg-Ni-Cu-based alloy to form an Mg-Ni-Cu-M-based quaternary alloy;
Ni：1.5～10.0wt.％，Cu：1.5～10.0wt.％；
m element is one of Ag, Ca, Sn, Si and Sr elements, wherein Ag: 0.1-5.0 wt.%, Ca: 0.1-5.0 wt.%, Sn: 0.1-5.0 wt.%, Si: 0.1-5.0 wt.%, Sr: 0.1-5.0 wt.%;
the balance being Mg, the contents of Ni and Cu being greater than the contents of the elements represented by M;
when the M element is Ag, Mg is formed in the Mg-Ni-Cu alloy in addition to the two-phase structure4An Ag phase; when the M element is Ca, Mg is formed in the Mg-Ni-Cu alloy in addition to the two-phase structure2A Ca phase; when M is Sn, Mg is formed in the Mg-Ni-Cu alloy in addition to the two-phase structure2A Sn phase; when M is Si, Mg is formed in the Mg-Ni-Cu alloy in addition to the two-phase structure2A Si phase; when M is Sr, Mg is formed in the Mg-Ni-Cu alloy in addition to the two-phase structure17Sr12Phase (1); different second phases formed by adding M element in Mg-Ni-Cu series alloy can effectively block dislocation movement and generate strengthening effect.
5. The soluble magnesium alloy material for oil and gas exploitation tool as claimed in claim 4, wherein the alloy composition of the Mg-Ni-Cu-M system quaternary alloy is:
Ni：1.5～6.0wt.％；Cu：1.5～6.0wt.％；
the other elements are one of Ag, Ca, Sn, Si and Sr elements, wherein the ratio of Ag: 0.5-4.0 wt.%, Ca: 0.5-2.5 wt.%, Sn: 0.5-2.0 wt.%, Si: 0.5-4.0 wt.%, Sr: 0.5-4.0 wt.%;
the balance being Mg, the contents of Ni and Cu being greater than the contents of the elements represented by M.
6. The soluble magnesium alloy material for oil and gas exploitation tool as claimed in claim 1, wherein Ni and Cu are used as main elements, and H and I elements are added on the basis of Mg-Ni-Cu to form Mg-Ni-Cu-M-N series quinary alloy;
Ni：2.0～10.0wt.％；Cu：2.0～10.0wt.％；
h is Gd and one of Y elements, wherein the ratio of Gd: 0.5-9.0 wt.%, Y: 0.5-6.0 wt.%;
i is one of Zn, Mn and Zr, wherein Zn: 0.1-1.2 wt.%, Mn: 0.1-1.2 wt.%, Zr: 0.01-0.2 wt.%;
the balance being Mg, the contents of Ni and Cu being higher than the contents of elements represented by H and I;
LPSO phases (Mg-Ni/Cu-Gd/Y and Mg-Ni/Cu-Zn) with different shapes and compositions are formed in the Zn-containing Mg-Ni-Cu series quinary alloy, and play a role in the corrosion and mechanical properties of the Mg-Ni-Cu series alloy; the Mg-Ni-Cu series quinary alloy containing Mn and Zr can refine crystal grains and improve mechanical strength.
7. The soluble magnesium alloy material for oil and gas exploitation tool according to claim 6, wherein the-Ni-Cu-H-I series quinary alloy comprises:
Ni：2.0～6.0wt.％；Cu：2.0～6.0wt.％；
m is Gd and one of Y elements, wherein the ratio of Gd: 1.0-4.0 wt.%, Y: 1.0-4.0 wt.%;
n is one of Zn, Mn and Zr, wherein Zn: 0.5-1.0 wt.%, Mn: 0.5-1.0 wt.%, Zr: 0.1-0.2 wt.%;
the balance being Mg, the contents of Ni and Cu being higher than the contents of the elements represented by M and N.
8. The method for producing a soluble magnesium alloy material for oil and gas production tools as claimed in claims 1 to 7, wherein the process is any 1 of the following 2:
the process A comprises the following steps: gravity casting → water cooling after solution treatment → preheating before extrusion → hot extrusion deformation;
and a process B: gravity casting → water cooling after solution treatment → preheating before extrusion → hot extrusion deformation → aging.
9. The method for preparing a soluble magnesium alloy material for oil and gas production tools as claimed in claim 8, wherein the process A is carried out in SF6And CO2Under the protection of gas, smelting at 700-720 ℃, carrying out slag removal and stirring on the melt, heating to 750-760 ℃, preserving heat for 15-20 minutes, and then pouring into a mold by gravity to obtain a needed ingot; solution treatmentThe temperature is 350-520 ℃, the time is 8-24 h, and the mixture is immediately put into tap water for cooling at room temperature after solution treatment; the preheating temperature of the sample, the extrusion die and the extrusion cylinder before extrusion is consistent with the extrusion temperature, the preheating time of the sample is 1.5-2.0 h, the preheating time of the extrusion die and the extrusion cylinder is 4-6 h, the extrusion temperature is 350-480 ℃, the extrusion ratio is 7: 1-22.5: 1, and the bar is immediately placed into tap water for cooling after extrusion.
10. The method for preparing a soluble magnesium alloy material for oil and gas production tools as claimed in claim 8, wherein the process B is carried out in SF6And CO2Under the protection of gas, smelting at 700-720 ℃, carrying out slag removal and stirring on the melt, heating to 750-760 ℃, preserving heat for 15-20 minutes, and then pouring into a mold by gravity to obtain a needed ingot; the temperature of the solution treatment is 350-520 ℃, the time is 8-24 h, and the solution treated product is immediately placed into tap water at room temperature for cooling; preheating temperatures of a sample, an extrusion die and an extrusion cylinder before extrusion are consistent with the extrusion temperature, wherein the preheating time of the sample is 1.5-2.0 h, the preheating time of the extrusion die and the extrusion cylinder is 4-6 h, the extrusion temperature is 350-480 ℃, the extrusion ratio is 7: 1-22.5: 1, and a bar is immediately placed into tap water for cooling after extrusion; the aging temperature is 175-200 ℃, the aging time is 20-60 h, and the bar is immediately placed into tap water for cooling after aging.
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| CN113355570A (en) * | 2021-06-23 | 2021-09-07 | 西安四方超轻材料有限公司 | High-elongation soluble magnesium-lithium alloy material and preparation method thereof |
| CN114892056A (en) * | 2022-06-15 | 2022-08-12 | 兰州理工大学 | LPSO strengthening phase-containing soluble magnesium alloy for fracturing temporary plugging tool and preparation method thereof |
| CN115896572A (en) * | 2022-12-01 | 2023-04-04 | 中南大学 | High-strength high-toughness high-speed dissolved magnesium alloy and preparation method thereof |
| CN116024471A (en) * | 2022-12-01 | 2023-04-28 | 中南大学 | High-strength plastic multi-water-soluble channel magnesium alloy and preparation method thereof |
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| CN115896572A (en) * | 2022-12-01 | 2023-04-04 | 中南大学 | High-strength high-toughness high-speed dissolved magnesium alloy and preparation method thereof |
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| CN116024471B (en) * | 2022-12-01 | 2024-07-02 | 中南大学 | High-strength plastic multi-water-soluble channel magnesium alloy and preparation method thereof |
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Effective date of registration: 20231220 Address after: No. 2 Development Road, Industrial Park, Huaihua City, Hunan Province, 418005 Patentee after: Hunan Baohuifeng New Material Technology Co.,Ltd. Address before: 100083 No. 30, Haidian District, Beijing, Xueyuan Road Patentee before: University OF SCIENCE AND TECHNOLOGY BEIJING |