CN109161769B - Functional rapidly-soluble rare earth magnesium alloy material and preparation method thereof - Google Patents
Functional rapidly-soluble rare earth magnesium alloy material and preparation method thereof Download PDFInfo
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- 239000000956 alloy Substances 0.000 title claims abstract description 52
- 229910000861 Mg alloy Inorganic materials 0.000 title claims abstract description 23
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 13
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 13
- 238000002360 preparation method Methods 0.000 title claims abstract description 6
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 36
- 238000005266 casting Methods 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 15
- 230000032683 aging Effects 0.000 claims abstract description 13
- 238000001192 hot extrusion Methods 0.000 claims abstract description 8
- 239000011777 magnesium Substances 0.000 claims abstract description 7
- 229910052751 metal Inorganic materials 0.000 claims abstract description 7
- 239000002184 metal Substances 0.000 claims abstract description 7
- 238000003723 Smelting Methods 0.000 claims abstract description 6
- 230000008569 process Effects 0.000 claims abstract description 5
- 150000002739 metals Chemical class 0.000 claims abstract description 4
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 3
- 229910052733 gallium Inorganic materials 0.000 claims abstract description 3
- 229910052738 indium Inorganic materials 0.000 claims abstract description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 3
- 238000001125 extrusion Methods 0.000 claims description 29
- 239000002994 raw material Substances 0.000 claims description 15
- 238000001816 cooling Methods 0.000 claims description 8
- 238000005498 polishing Methods 0.000 claims description 8
- 238000005303 weighing Methods 0.000 claims description 8
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 7
- 229910052802 copper Inorganic materials 0.000 claims description 7
- 239000010949 copper Substances 0.000 claims description 7
- 238000000265 homogenisation Methods 0.000 claims description 5
- 239000000155 melt Substances 0.000 claims description 5
- 238000002844 melting Methods 0.000 claims description 3
- 230000008018 melting Effects 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 2
- 244000137852 Petrea volubilis Species 0.000 claims description 2
- 229910002804 graphite Inorganic materials 0.000 claims description 2
- 239000010439 graphite Substances 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 229910052749 magnesium Inorganic materials 0.000 claims description 2
- 238000010309 melting process Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 239000012266 salt solution Substances 0.000 claims description 2
- 238000004321 preservation Methods 0.000 claims 1
- 238000003801 milling Methods 0.000 abstract description 3
- 238000010276 construction Methods 0.000 abstract description 2
- 239000003792 electrolyte Substances 0.000 abstract 1
- 230000007797 corrosion Effects 0.000 description 13
- 238000005260 corrosion Methods 0.000 description 13
- 239000000243 solution Substances 0.000 description 12
- 238000012545 processing Methods 0.000 description 11
- 238000004090 dissolution Methods 0.000 description 6
- 238000005553 drilling Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000012856 packing Methods 0.000 description 3
- 229910000831 Steel Inorganic materials 0.000 description 2
- 230000000903 blocking effect Effects 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 238000005275 alloying Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000012634 fragment Substances 0.000 description 1
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- C22C—ALLOYS
- C22C23/00—Alloys based on magnesium
- C22C23/06—Alloys based on magnesium with a rare earth metal 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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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C23/00—Alloys based on magnesium
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- 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
- C22C23/00—Alloys based on magnesium
- C22C23/04—Alloys based on magnesium with zinc or cadmium 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
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- C22C30/02—Alloys containing less than 50% by weight of each constituent containing copper
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- C22C30/04—Alloys containing less than 50% by weight of each constituent containing tin or lead
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C30/00—Alloys containing less than 50% by weight of each constituent
- C22C30/06—Alloys containing less than 50% by weight of each constituent containing 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
- C22F1/06—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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Abstract
The invention discloses a functional fast soluble rare earth magnesium alloy material and a preparation method thereof, belonging to the field of nonferrous metals. The magnesium alloy consists of Mg a Gd b Y c Zr d Ni e M f N g Wherein M is one or the combination of two elements of Ga and In, N is one or the combination of more than one of Al, mn, ca, zn, cu, sn, sr, li, la, ce, pr, nd, ge, ag, si and the like, and the target alloy is obtained by smelting casting, solution treatment, hot extrusion and aging treatment. Compared with the prior art, the magnesium alloy material prepared by the components has higher strength and plasticity, can be quickly dissolved in a solution containing electrolyte, is suitable for plugging tools used in the fracturing process of oil and gas fields, can be automatically dissolved after service, saves subsequent flowback and milling processes, and improves the construction efficiency.
Description
Technical Field
The invention belongs to the field of nonferrous metals, and particularly relates to a functional rapid soluble rare earth magnesium alloy material and a preparation method thereof.
Background
The magnesium alloy is one of the lightest commercial metal structural materials at present, has a series of advantages of low density, high specific strength, high specific rigidity, good electromagnetic shielding capability, machinability, easy recycling and the like, and is widely applied to the fields of aerospace, oceans, automobiles, electronics and the like. On the other hand, the magnesium alloy has lower electrode potential and more active chemical property, is easy to corrode in most solutions and can be applied to specific industrial fields. However, the corrosion rate of magnesium alloy at normal temperature is not high, and the industrial application requirements cannot be met. The alloying method has great significance for improving the corrosion speed of the magnesium alloy.
China has rich low-permeability oil gas resources and great exploration and development potential, and the stable yield and the yield increase of oil gas yield in the future depend on the low-permeability unconventional oil gas resources more. Most of the oil and gas resources are distributed in strata with different depths, and the development of the unconventional oil and gas resources must depend on reservoir transformation process technologies such as hydraulic fracturing. In the hydraulic fracturing technology, fracturing reconstruction is carried out layer by layer after different intervals need to be separated by packing tools (such as fracturing balls and bridge plugs), and the packing tools are discharged back after all intervals are constructed so as to conveniently open a well to 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. Thus, composite materials have been developed, which have a problem of easy blocking of passages because they cannot be completely dissolved, although they have solved the problem of high specific gravity, and are expensive because they rely on imports for production and processing of raw materials.
Disclosure of Invention
The invention aims to: provides a functional fast soluble rare earth magnesium alloy material, ensures that the material has excellent mechanical property and can realize fast dissolution in corresponding solution.
A functional fast soluble rare earth magnesium alloy material, the magnesium alloy composition is Mg a Gd b Y c Zr d Ni e M f N g Wherein M is one or the combination of two elements of Ga and In, and N is one or the combination of more than one of Al, mn, ca, zn, cu, sn, sr, li, la, ce, pr, nd, ge, ag, si and the like.
Wherein formula Mg a Gd b Y c Zr d Ni e M f N g Wherein the weight percentage of b is 0.1-15%, the weight percentage of c is 0.1-10%, d is 0.1-5%, e is 0.1-10%, f is 0.1-10%, g is 0-20%, and a is the balance, a + b + c + d + e + f + g =100.
The preparation method of the functional rapid soluble rare earth magnesium alloy material comprises the following steps:
(1) Pretreatment: weighing the required raw materials according to the weight percentage, and polishing the oxide layer on the surface of the metal by using sand paper.
(2) Smelting and casting: putting the pretreated raw materials into a graphite crucible, heating and melting the raw materials in a resistance furnace, stirring and mixing the raw materials uniformly, and casting to obtain a cast ingot;
(3) Homogenization treatment: keeping the obtained cast ingot at a certain temperature for a period of time;
(4) Hot extrusion: carrying out hot extrusion on the obtained cast ingot at a certain temperature to obtain an alloy bar;
(5) Aging treatment: and carrying out aging treatment on the alloy bar obtained by extrusion at a certain temperature.
Further, in the smelting and casting process of the step (2), pure magnesium is added into a crucible to be molten, and SF is required to be used in the melting process 6 +CO 2 And (3) under the protection of gas, then, raising the temperature of the melt to 700-710 ℃, adding other pure metals and intermediate alloys, stirring and skimming after the melt is completely melted, raising the temperature of the melt to 730-750 ℃, preserving the heat for 10-30min, then, cooling to 700-710 ℃ for casting, wherein a casting mold adopts a water-cooled copper mold.
Further, the homogenization treatment in the step (3) is carried out, the temperature range is 400-530 ℃, and the time is 10-40h.
Further, in the hot extrusion process in the step (4), the extrusion temperature is 350-450 ℃, and the total deformation is 60-90%.
Further, the aging treatment in the step (5) is carried out at the temperature of 160-250 ℃ for 10-200h.
The invention aims to provide a novel functional dissoluble magnesium alloy material which has high strength and good plasticity, can be quickly dissolved and can be widely applied to the field of oil exploitation. Compared with steel and composite materials, the fracturing oil can be completely dissolved, the problem of easy blocking does not exist, the problem of secondary drilling does not exist, the production cost can be reduced, and the fracturing oil is mainly used for manufacturing fracturing downhole tool members such as fracturing balls, ball seats, packers, bridge plugs and the like.
Compared with the prior art, the magnesium alloy material prepared by the method has high mechanical strength and good plasticity, can be quickly dissolved in a salt solution, is suitable for plugging tools used in the fracturing process of oil and gas fields, can be automatically dissolved after the tools are in service, saves subsequent flowback and milling processes, and improves the construction efficiency.
Drawings
FIG. 1 is a typical microstructure morphology of the alloys of examples 1, 2;
FIG. 2 is a graph of the elongation curves of the alloys of examples 1-4;
FIG. 3 is a graph comparing the corrosion rates of the alloys of examples 1-4;
Detailed Description
The following examples further illustrate the invention.
Example 1: mg-10Gd-3Y-0.3Zr-0.2Ni-0.1In alloy
Weighing the required alloy raw materials in proportion, and polishing the surface of the alloy. The alloy is added into a crucible one by one to be melted, the temperature is kept at 750 ℃ for 10min, then the temperature is reduced to 710 ℃ for casting, and a water-cooling copper mold is adopted as a casting mold. Then homogenizing the cast ingot, and keeping the temperature at 520 ℃ for 10 hours. And processing the homogenized cast ingot into a cylinder for extrusion processing, wherein the extrusion temperature is 420 ℃, the extrusion speed is 0.4mm/s, and the extrusion ratio is 16. And (3) after extrusion, carrying out aging treatment on the bar at 225 ℃ for 12h.
The Mg-10Gd-3Y-0.3Zr-0.2Ni-0.1In alloy obtained by the above steps has a tensile strength of 320.6MPa at room temperature, a yield strength of 259.1MPa, an elongation at break as high as 13.4%, and a corrosion rate In 3% KCl solution at room temperature of 37.6Mg/cm 2 At 90 ℃ 3% corrosion rate in KCl solution of 67.8mg/cm 2 The dissolution can be realized by itself.
Example 2: mg-9Gd-3Y-0.1Zr-0.8Ni-0.1In alloy
Weighing the required alloy raw materials in proportion, and polishing the surface of the alloy. The alloy is added into a crucible one by one to be melted, the temperature is kept at 750 ℃ for 10min, then the temperature is reduced to 710 ℃ for casting, and a water-cooling copper mold is adopted as a casting mold. Then homogenizing the cast ingot, and keeping the temperature at 520 ℃ for 10 hours. And processing the homogenized cast ingot into a cylinder for extrusion processing, wherein the extrusion temperature is 420 ℃, the extrusion speed is 0.4mm/s, and the extrusion ratio is 16. And (3) after extrusion, carrying out aging treatment on the bar at 225 ℃ for 12h.
The Mg-9Gd-3Y-0.1Zr-0.8Ni-0.1In alloy obtained by the above steps has a tensile strength of 363.1MPa at room temperature, a yield strength of 289.3MPa, an elongation at break as high as 11.2%, and a corrosion rate of 22.8Mg/cm In 3-percent KCl solution at room temperature 2 (ii)/h, 90 ℃ 3% Corrosion Rate in KCl solution of 41.4mg/cm 2 And h, the dissolution can be automatically realized.
Example 3: mg-10Gd-3Y-0.25Zr-0.4Ni-0.1Ga alloy
Weighing the required alloy raw materials in proportion, and polishing the surface of the alloy. Adding the alloy into a crucible one by one for melting, preserving heat at 750 ℃ for 10min, cooling to 710 ℃ for casting, and adopting a water-cooled copper mould as a casting mould. Then homogenizing the cast ingot, and keeping the temperature at 520 ℃ for 10 hours. And processing the homogenized cast ingot into a cylinder for extrusion processing, wherein the extrusion temperature is 420 ℃, the extrusion speed is 0.4mm/s, and the extrusion ratio is 16. And (3) after extrusion, carrying out aging treatment on the bar at 225 ℃ for 12h.
The Mg-10Gd-3Y-0.25Zr-0.4Ni-0.1Ga alloy obtained by the above steps has a tensile strength at room temperature of 319.9MPa, a yield strength of 255.5MPa, an elongation at break as high as 12.6%, and a corrosion rate in a 3% KCl solution at room temperature of 16.3Mg/cm 2 H,90 ℃ 3% of the corrosion rate in the KCl solution is 32.3mg/cm 2 The dissolution can be realized by itself.
Example 4: mg-9Gd-3Y-0.2Zr-0.6Ni-0.1In-0.3Zn alloy
Weighing the required alloy raw materials in proportion, and polishing the alloy surface. The alloy is added into a crucible one by one to be melted, the temperature is kept at 750 ℃ for 10min, then the temperature is reduced to 710 ℃ for casting, and a water-cooling copper mold is adopted as a casting mold. Then homogenizing the cast ingot, and keeping the temperature at 520 ℃ for 10 hours. And processing the homogenized cast ingot into a cylinder for extrusion processing, wherein the extrusion temperature is 420 ℃, the extrusion speed is 0.4mm/s, and the extrusion ratio is 16. And (3) after extrusion, carrying out aging treatment on the bar at 225 ℃ for 12h.
The Mg-9Gd-3Y-0.2Zr-0.6Ni-0.1In-0.3Zn alloy obtained by the above steps has a tensile strength of 360.9MPa at room temperature, a yield strength of 270.2MPa, an elongation at break as high as 10.1%, and a corrosion rate of 10.2Mg/cm In a KCl solution at room temperature 3% 2 At 90 ℃ 3% corrosion rate in KCl solution of 22.7mg/cm 2 The dissolution can be realized by itself.
Example 5: mg-9Gd-3Y-0.2Zr-0.6Ni-0.1In-0.5Cu alloy
Weighing the required alloy raw materials in proportion, and polishing the surface of the alloy. The alloy is added into a crucible one by one to be melted, the temperature is kept at 750 ℃ for 10min, then the temperature is reduced to 710 ℃ for casting, and a water-cooling copper mold is adopted as a casting mold. Then homogenizing the cast ingot, and keeping the temperature at 520 ℃ for 10 hours. And processing the homogenized cast ingot into a cylinder for extrusion processing, wherein the extrusion temperature is 420 ℃, the extrusion speed is 0.4mm/s, and the extrusion ratio is 16. And (3) after extrusion, carrying out aging treatment on the bar at 225 ℃ for 12h.
The Mg-9Gd-3Y-0.2Zr-0.6Ni-0.1In-0.3Zn alloy obtained by the above steps has a tensile strength of 370.9MPa at room temperature, a yield strength of 282.2MPa, an elongation at break of up to 11.9%, and a corrosion rate of 15.2Mg/cm In a 3% KCl solution at room temperature 2 At 90 ℃ 3% of the corrosion rate in KCl solution of 33.7mg/cm 2 And h, the dissolution can be automatically realized.
The examples are given solely for the purpose of illustrating the invention and are not intended to limit the practice of the invention. Other variants than those described above will be apparent to those skilled in the art and all such modifications are intended to fall within the scope of the appended claims.
Claims (5)
1. A kind ofThe functional fast soluble rare earth magnesium alloy material is characterized in that the magnesium alloy consists of Mg a Gd b Y c Zr d Ni e M f N g And can be quickly dissolved In a salt solution, wherein M is one or the combination of two elements of Ga and In, and N is one or the arbitrary combination of more than one element of Al, mn, ca, zn, cu, sn, sr, li, la, ce, pr, nd, ge, ag and Si; formula Mg a Gd b Y c Zr d Ni e M f N g Wherein the weight percentage of b is 9-15%, the weight percentage of c is 3-10%, the weight percentage of d is 0.2-5%, the weight percentage of e is 0.6-10%, the weight percentage of f is 0.1-10%, the weight percentage of g is 0.3-20%, a is the rest, and a + b + c + d + e + f + g =100;
the functional rapid soluble rare earth magnesium alloy material is prepared by raw material weighing, abrasive paper polishing pretreatment, smelting casting, homogenization treatment, hot extrusion and aging treatment; and the preparation steps are as follows:
(1) Pretreatment: weighing the required raw materials according to the weight percentage, and polishing the oxide layer on the surface of the metal by using sand paper.
(2) Smelting and casting: putting the pretreated raw materials into a graphite crucible, heating and melting the raw materials in a resistance furnace, stirring and mixing the raw materials uniformly, and casting to obtain a cast ingot;
(3) Homogenization treatment: keeping the obtained cast ingot at a certain temperature for a period of time;
(4) Hot extrusion: carrying out hot extrusion on the obtained cast ingot at a certain temperature to obtain an alloy bar;
(5) And (3) aging treatment: and carrying out aging treatment on the alloy bar obtained by extrusion at a certain temperature.
2. The method for preparing the functional rapid soluble rare earth magnesium alloy material according to claim 1, wherein the method comprises the following steps: the smelting and casting process of the step (2) is as follows: adding pure magnesium into a crucible to melt, wherein SF is required to be used in the melting process 6 +CO 2 Gas protection, then raising the temperature of the melt to 700-710 ℃, adding other pure metals andstirring and slagging off the intermediate alloy after the intermediate alloy is completely melted, raising the temperature of the melt to 730-750 ℃, preserving the heat for 10-30min, then cooling to 700-710 ℃ for casting, and adopting a water-cooling copper mould as a casting mould.
3. The method for preparing the functional rapid soluble rare earth magnesium alloy material according to claim 1, wherein the method comprises the following steps: the homogenization treatment in the step (3) is that the temperature range of heat preservation is 520-530 ℃ and the time is 10-40h.
4. The method for preparing the functional rapid soluble rare earth magnesium alloy material according to claim 1, wherein the method comprises the following steps: the hot extrusion process in the step (4) is that the extrusion temperature is 420-450 ℃, and the total deformation is 60-90%.
5. The method for preparing the functional rapid soluble rare earth magnesium alloy material according to claim 1, wherein the method comprises the following steps: the aging treatment in the step (5) is carried out at the temperature of 160-250 ℃ for 10-200h.
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| CN109694976B (en) * | 2019-03-13 | 2020-03-17 | 山东省科学院新材料研究所 | Low-cost soluble magnesium alloy and preparation method and application thereof |
| CN110184518B (en) * | 2019-04-24 | 2020-10-27 | 北京易联结科技发展有限公司 | Rapidly-dissolved high-strength high-elongation magnesium alloy and preparation method thereof |
| CN110106416B (en) * | 2019-05-24 | 2020-03-24 | 山东省科学院新材料研究所 | Ultrahigh-strength dissolvable magnesium alloy and preparation method and application thereof |
| CN110863130A (en) * | 2019-11-11 | 2020-03-06 | 北京科技大学 | High-plasticity quick soluble magnesium alloy material and preparation method thereof |
| CN111041265B (en) * | 2019-11-11 | 2021-07-02 | 北京科技大学 | Preparation of degradable magnesium alloy sliding sleeve fracturing ball and method for controlling degradation rate |
| CN111286657A (en) * | 2020-03-13 | 2020-06-16 | 重庆大学 | High-strength Mg-Gd-Zn-Zr-Ag magnesium alloy and preparation method thereof |
| CN111850367A (en) * | 2020-07-30 | 2020-10-30 | 中国石油化工股份有限公司 | High-plasticity soluble magnesium alloy and preparation method and application thereof |
| CN113667871A (en) * | 2021-08-10 | 2021-11-19 | 郑州轻研合金科技有限公司 | High-ductility soluble magnesium-lithium alloy and preparation method and application thereof |
| 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 |
| CN116043086B (en) * | 2022-12-19 | 2024-04-12 | 湖南稀土金属材料研究院有限责任公司 | Soluble magnesium alloy, preparation method and application thereof, and fracturing product |
| CN116005051A (en) * | 2023-01-16 | 2023-04-25 | 中南大学 | Aluminum alloy capable of being rapidly dissolved in neutral medium and preparation method and application thereof |
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Effective date of registration: 20240712 Address after: 274039 Lanzhou Road, Heze hi tech Zone, Heze, Shandong Province, No. 2166 Patentee after: AMGAIN SHANDONG MAGNESIUM Co.,Ltd. Country or region after: China Address before: 100083 No. 30, Haidian District, Beijing, Xueyuan Road Patentee before: University OF SCIENCE AND TECHNOLOGY BEIJING Country or region before: China |