CN109161769A - A kind of functional quickly solvable rare earth magnesium alloy material and preparation method thereof - Google Patents

A kind of functional quickly solvable rare earth magnesium alloy material and preparation method thereof Download PDF

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CN109161769A
CN109161769A CN201811279001.9A CN201811279001A CN109161769A CN 109161769 A CN109161769 A CN 109161769A CN 201811279001 A CN201811279001 A CN 201811279001A CN 109161769 A CN109161769 A CN 109161769A
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magnesium alloy
rare earth
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weight percent
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CN109161769B (en
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李宏祥
张济山
王健
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University of Science and Technology Beijing USTB
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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
    • C22C23/06—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
    • 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
    • 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
    • C22C23/00—Alloys based on magnesium
    • C22C23/02—Alloys based on magnesium with aluminium as the next major constituent
    • 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
    • C—CHEMISTRY; METALLURGY
    • 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
    • C—CHEMISTRY; METALLURGY
    • 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
    • C22C30/02—Alloys containing less than 50% by weight of each constituent containing copper
    • C—CHEMISTRY; METALLURGY
    • 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
    • C22C30/04—Alloys containing less than 50% by weight of each constituent containing tin or lead
    • C—CHEMISTRY; METALLURGY
    • 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
    • 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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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
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  • Crystallography & Structural Chemistry (AREA)
  • Extrusion Of Metal (AREA)
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Abstract

The invention discloses a kind of functional quickly solvable rare earth magnesium alloy materials and preparation method thereof, belong to non-ferrous metal field.The group of magnesium alloys becomes MgaGdbYcZrdNieMfNgWherein M is the combination of one or both of Ga, In element element, N is any combination one or more kinds of in the elements such as Al, Mn, Ca, Zn, Cu, Sn, Sr, Li, La, Ce, Pr, Nd, Ge, Ag, Si, smelting casting, solution treatment, hot extrusion and ageing treatment obtain subject alloy.Compared with prior art, the magnesium alloy materials prepared using ingredient of the present invention, intensity and plasticity with higher, and quickly dissolution can be realized in the solution containing electrolyte, suitable for capping tools used in processing oil gas field fracturing process, tool can voluntarily dissolve after the completion of military service, save the subsequent row of returning, milling process, improve construction efficiency.

Description

A kind of functional quickly solvable rare earth magnesium alloy material and preparation method thereof
Technical field
The invention belongs to non-ferrous metal fields, and in particular to a kind of functional quickly solvable rare earth magnesium alloy material and its system Preparation Method.
Background technique
Magnesium alloy has low-density, high specific strength, Gao Bigang as now most light one of commercial metal structural material Degree, good electromagnetic shielding capability, machinability and a series of advantage such as be easy to regeneration, aerospace, ocean, The fields such as automobile, electronics are widely applied.On the other hand, magnesium alloy has lower electrode potential, and chemical property is more living It sprinkles, corrosion is easy to happen in most solutions, can be applied to specific industrial circle.But the corrosion rate of magnesium alloy under room temperature It is not high, it is not able to satisfy industrial application demand.By alloyage process, the corrosion rate of magnesium alloy is improved, is had particularly important Meaning.
Chinese Low Permeability Oil/gas is resourceful, has very big exploration-development potential, the stable yields of the following oil and gas production, volume increase These hyposmosis unconventional petroleum resources will be relied more heavily on.These petroleum resources are distributed in the stratum of different depth mostly In, developing these unconventional petroleum resources must be by reservoir reconstructions technologies such as hydraulic fracturings.In hydraulic fracturing technology, It needs successively to carry out fracturing reform after separating using isolating tool (such as pressure break ball, bridge plug) between different intervals, construct to all intervals Isolating tool is returned into discharge again after the completion, to get through the exploitation that hoistway realizes oil, gas.
Currently, common isolating tool is made by steel mostly, exist brill milling is difficult, time-consuming, bore after powder, fragment be not easy The disadvantages of row of returning.Therefore have developed composite material, although solve the problems, such as it is heavy because cannot be completely dissolved, There are problems that easy blocking channel, and raw material production need to rely on import, somewhat expensive with processing.
Summary of the invention
It is an object of the invention to: a kind of functional quickly solvable rare earth magnesium alloy material is provided, guarantees it with excellent Mechanical property, and can be realized in corresponding solution quickly dissolution.
A kind of functional quickly solvable rare earth magnesium alloy material, the group of magnesium alloys become MgaGdbYcZrdNieMfNg, Middle M is the combination of one or both of Ga, In element element, N Al, Mn, Ca, Zn, Cu, Sn, Sr, Li, La, Ce, Pr, One or more kinds of any combination in the elements such as Nd, Ge, Ag, Si.
Wherein formula MgaGdbYcZrdNieMfNgThe weight percent of middle b is 0.1-15%, and the weight percent of c is 0.1- The weight percent of 10%, d are 0.1-5%, and the weight percent of e is 0.1-10%, and the weight percent of f is 0.1-10%, g Weight percent be 0-20%, a is surplus, a+b+c+d+e+f+g=100.
A kind of preparation method of functional quickly solvable rare earth magnesium alloy material as described above, includes the following steps:
(1) it pre-processes: weighing required raw material by weight percentage, and oxidation on metal surface layer is polished off with sand paper.
(2) melting is cast: pretreated raw material being put into graphite crucible, fusing is heated in resistance furnace, and stir It is uniformly mixed, ingot casting is obtained after casting；
(3) gained ingot casting Homogenization Treatments: is kept the temperature into a period of time at a certain temperature；
(4) hot extrusion: gained ingot casting is subjected to hot extrusion at a certain temperature, obtains alloy bar material；
(5) ageing treatment: resulting alloy bar material will be squeezed and carry out ageing treatment at a certain temperature.
Further, pure magnesium, is first added in crucible and melts, need in fusion process by the melting casting process of step (2) Use SF6+CO2Melt temperature is then risen to 700-710 DEG C and other pure metal and intermediate alloy is added, to whole by gas shield It is stirred and skims after fusing, melt temperature is increased to 730-750 DEG C, 10-30min is kept the temperature, is cooled to 700-710 later It DEG C casts, casting die uses water cooled copper mould.
Further, step (3) Homogenization Treatments, holding temperature range are 400-530 DEG C, time 10-40h.
Further, step (4) hot extrusion process, squeezing temperature is 350-450 DEG C, total deformation 60-90%.
Further, step (5) ageing treatment, temperature range are 160-250 DEG C, time 10-200h.
The present invention is intended to provide a kind of novel dissolvable magnesium alloy materials of functionality, the strength of materials is high, and plasticity is good, can be quick Dissolution, can be widely used for field of petroleum exploitation.It compared to steel and composite material, can be completely dissolved, there is no easy blockings to ask Topic, be not present secondary lower brill problem, production cost can be reduced, be used primarily in tool component under fractured well, as pressure break ball, ball seat, In the manufacture such as packer, bridge plug.
Compared with prior art, using magnesium alloy materials produced by the present invention, mechanical strength is high, and plasticity is good, can be molten in salt Quickly dissolution is realized in liquid, is suitable for capping tools used in processing oil gas field fracturing process, tool can be after the completion of military service It voluntarily dissolves, saves the subsequent row of returning, milling process, improve construction efficiency.
Detailed description of the invention
Fig. 1 is the representative microstructure pattern of alloy in embodiment 1,2；
Fig. 2 is the stress strain curve figure of alloy in embodiment 1-4；
Fig. 3 is the comparison between corrosion figure of alloy in embodiment 1-4；
Specific embodiment
Following embodiment will invention is further explained.
Embodiment 1:Mg-10Gd-3Y-0.3Zr-0.2Ni-0.1In alloy
Alloy raw material needed for weighing in proportion polishes alloy surface clean.Alloy is added in crucible one by one and is melted, It is cooled to 710 DEG C after 750 DEG C of heat preservation 10min to cast, casting die uses water cooled copper mould.Then ingot casting is carried out uniform Change processing, holding temperature are 520 DEG C, time 10h.Ingot casting after homogenization is processed into cylindrical body and carries out extrusion process, is squeezed Pressing temperature is 420 DEG C, extrusion speed 0.4mm/s, extrusion ratio 16.Ageing treatment, temperature 225 are carried out to bar after extruding DEG C, time 12h.
The Mg-10Gd-3Y-0.3Zr-0.2Ni-0.1In Alloy At Room Temperature tensile strength obtained through the above steps is 320.6MPa, yield strength 259.1MPa, elongation at break are up to 13.4%, at room temperature, the corrosion speed in 3%KCl solution Rate is 37.6mg/cm2/ h, at 90 DEG C, the corrosion rate in 3%KCl solution is 67.8mg/cm2/ h can voluntarily realize dissolution.
Embodiment 2:Mg-9Gd-3Y-0.1Zr-0.8Ni-0.1In alloy
Alloy raw material needed for weighing in proportion polishes alloy surface clean.Alloy is added in crucible one by one and is melted, It is cooled to 710 DEG C after 750 DEG C of heat preservation 10min to cast, casting die uses water cooled copper mould.Then ingot casting is carried out uniform Change processing, holding temperature are 520 DEG C, time 10h.Ingot casting after homogenization is processed into cylindrical body and carries out extrusion process, is squeezed Pressing temperature is 420 DEG C, extrusion speed 0.4mm/s, extrusion ratio 16.Ageing treatment, temperature 225 are carried out to bar after extruding DEG C, time 12h.
The Mg-9Gd-3Y-0.1Zr-0.8Ni-0.1In Alloy At Room Temperature tensile strength obtained through the above steps is 363.1MPa, yield strength 289.3MPa, elongation at break are up to 11.2%, at room temperature, the corrosion speed in 3%KCl solution Rate is 22.8mg/cm2/ h, at 90 DEG C, the corrosion rate in 3%KCl solution is 41.4mg/cm2/ h can voluntarily realize dissolution.
Embodiment 3:Mg-10Gd-3Y-0.25Zr-0.4Ni-0.1Ga alloy
Alloy raw material needed for weighing in proportion polishes alloy surface clean.Alloy is added in crucible one by one and is melted, It is cooled to 710 DEG C after 750 DEG C of heat preservation 10min to cast, casting die uses water cooled copper mould.Then ingot casting is carried out uniform Change processing, holding temperature are 520 DEG C, time 10h.Ingot casting after homogenization is processed into cylindrical body and carries out extrusion process, is squeezed Pressing temperature is 420 DEG C, extrusion speed 0.4mm/s, extrusion ratio 16.Ageing treatment, temperature 225 are carried out to bar after extruding DEG C, time 12h.
The Mg-10Gd-3Y-0.25Zr-0.4Ni-0.1Ga Alloy At Room Temperature tensile strength obtained through the above steps is 319.9MPa, yield strength 255.5MPa, elongation at break are up to 12.6%, at room temperature, the corrosion speed in 3%KCl solution Rate is 16.3mg/cm2/ h, at 90 DEG C, the corrosion rate in 3%KCl solution is 32.3mg/cm2/ h can voluntarily realize dissolution.
Embodiment 4:Mg-9Gd-3Y-0.2Zr-0.6Ni-0.1In-0.3Zn alloy
Alloy raw material needed for weighing in proportion polishes alloy surface clean.Alloy is added in crucible one by one and is melted, It is cooled to 710 DEG C after 750 DEG C of heat preservation 10min to cast, casting die uses water cooled copper mould.Then ingot casting is carried out uniform Change processing, holding temperature are 520 DEG C, time 10h.Ingot casting after homogenization is processed into cylindrical body and carries out extrusion process, is squeezed Pressing temperature is 420 DEG C, extrusion speed 0.4mm/s, extrusion ratio 16.Ageing treatment, temperature 225 are carried out to bar after extruding DEG C, time 12h.
The Mg-9Gd-3Y-0.2Zr-0.6Ni-0.1In-0.3Zn Alloy At Room Temperature tensile strength obtained through the above steps is 360.9MPa, yield strength 270.2MPa, elongation at break are up to 10.1%, at room temperature, the corrosion speed in 3%KCl solution Rate is 10.2mg/cm2/ h, at 90 DEG C, the corrosion rate in 3%KCl solution is 22.7mg/cm2/ h can voluntarily realize dissolution.
Embodiment 5:Mg-9Gd-3Y-0.2Zr-0.6Ni-0.1In-0.5Cu alloy
Alloy raw material needed for weighing in proportion polishes alloy surface clean.Alloy is added in crucible one by one and is melted, It is cooled to 710 DEG C after 750 DEG C of heat preservation 10min to cast, casting die uses water cooled copper mould.Then ingot casting is carried out uniform Change processing, holding temperature are 520 DEG C, time 10h.Ingot casting after homogenization is processed into cylindrical body and carries out extrusion process, is squeezed Pressing temperature is 420 DEG C, extrusion speed 0.4mm/s, extrusion ratio 16.Ageing treatment, temperature 225 are carried out to bar after extruding DEG C, time 12h.
The Mg-9Gd-3Y-0.2Zr-0.6Ni-0.1In-0.3Zn Alloy At Room Temperature tensile strength obtained through the above steps is 370.9MPa, yield strength 282.2MPa, elongation at break are up to 11.9%, at room temperature, the corrosion speed in 3%KCl solution Rate is 15.2mg/cm2/ h, at 90 DEG C, the corrosion rate in 3%KCl solution is 33.7mg/cm2/ h can voluntarily realize dissolution.
Embodiment of the present invention only citing used in the present invention to clearly illustrate, rather than is to embodiment of the present invention It limits.For those of ordinary skill in the art, other different forms can also be made on the basis of the above description Change, correlation change in the protection scope of the claims in the present invention.

Claims (6)

1. a kind of functional quickly solvable rare earth magnesium alloy material, it is characterised in that the group of magnesium alloys becomes MgaGdbYcZrdNieMfNg, wherein M is the combination of one or both of Ga, In element element, N Al, Mn, Ca, Zn, Cu, One or more kinds of any combination in Sn, Sr, Li, La, Ce, Pr, Nd, Ge, Ag, Si element；Formula MgaGdbYcZrdNieMfNgThe weight percent of middle b is 0.1-15%, and the weight percent of c is 0.1-10%, the weight percent of d Than being 0.1-10% for the weight percent of 0.1-5%, e, the weight percent of f is 0.1-10%, and the weight percent of g is 0- 20%, a are surplus, a+b+c+d+e+f+g=100.
2. a kind of preparation method of functional quickly solvable rare earth magnesium alloy material as described in claim 1, which is characterized in that Preparation step is as follows:
(1) it pre-processes: weighing required raw material by weight percentage, and oxidation on metal surface layer is polished off with sand paper.
(2) melting is cast: pretreated raw material being put into graphite crucible, fusing is heated in resistance furnace, and be stirred Uniformly, ingot casting is obtained after casting；
(3) gained ingot casting Homogenization Treatments: is kept the temperature into a period of time at a certain temperature；
(4) hot extrusion: gained ingot casting is subjected to hot extrusion at a certain temperature, obtains alloy bar material；
(5) ageing treatment: resulting alloy bar material will be squeezed and carry out ageing treatment at a certain temperature.
3. a kind of preparation method of functional quickly solvable rare earth magnesium alloy material as claimed in claim 2, it is characterised in that: Melting casting process described in step (2) is: first pure magnesium being added in crucible and is melted, is needed in fusion process using SF6+CO2Gas Body protection, then rises to 700-710 DEG C for melt temperature and other pure metal and intermediate alloy is added, and is stirred after all fusings It mixes and stirs and skims, melt temperature is increased to 730-750 DEG C, 10-30min is kept the temperature, is cooled to 700-710 DEG C later and casts, Casting die uses water cooled copper mould.
4. a kind of preparation method of functional quickly solvable rare earth magnesium alloy material as claimed in claim 2, it is characterised in that: Homogenization Treatments described in step (3) are that holding temperature range is 400-530 DEG C, time 10-40h.
5. a kind of preparation method of functional quickly solvable rare earth magnesium alloy material as claimed in claim 2, it is characterised in that: Hot extrusion process described in step (4) is that extruding temperature is 350-450 DEG C, total deformation 60-90%.
6. a kind of preparation method of functional quickly solvable rare earth magnesium alloy material as claimed in claim 2, it is characterised in that: Step (5) described ageing treatment is that temperature range is 160-250 DEG C, time 10-200h.
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Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109694976A (en) * 2019-03-13 2019-04-30 山东省科学院新材料研究所 A kind of low cost soluble magnesium alloy and its preparation method and application
CN109797361A (en) * 2019-03-05 2019-05-24 北京科技大学 A kind of preparation method of solvable Mg alloy surface high corrosion resistant coating
CN110106416A (en) * 2019-05-24 2019-08-09 山东省科学院新材料研究所 A kind of superhigh intensity can dissolve magnesium alloy and its preparation method and application
CN110184518A (en) * 2019-04-24 2019-08-30 北京易联结科技发展有限公司 A kind of rapidly-soluble high-strength high-elongation ratio magnesium alloy and preparation method 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
CN111041265A (en) * 2019-11-11 2020-04-21 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
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
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
CN116043086A (en) * 2022-12-19 2023-05-02 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

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CN107723546A (en) * 2017-10-26 2018-02-23 冉兴 The toughening magnesium alloy of running water fast erosion and its manufacture method of component
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CN105950931A (en) * 2016-07-20 2016-09-21 肖旅 High-strength and high-hardness magnesium alloy in controllable reaction with water, and manufacturing method of component thereof
CN106048353A (en) * 2016-08-23 2016-10-26 肖旅 High-plasticity magnesium alloy for controllable reaction with water and manufacture method of magnesium alloy component
CN106119647A (en) * 2016-08-27 2016-11-16 冉兴 High-strength magnesium alloy and the manufacture method of component thereof with water generation controllable reaction
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Cited By (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109797361A (en) * 2019-03-05 2019-05-24 北京科技大学 A kind of preparation method of solvable Mg alloy surface high corrosion resistant coating
CN109694976A (en) * 2019-03-13 2019-04-30 山东省科学院新材料研究所 A kind of low cost soluble magnesium alloy and its preparation method and application
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
CN110184518A (en) * 2019-04-24 2019-08-30 北京易联结科技发展有限公司 A kind of rapidly-soluble high-strength high-elongation ratio magnesium alloy and preparation method thereof
CN110106416A (en) * 2019-05-24 2019-08-09 山东省科学院新材料研究所 A kind of superhigh intensity can dissolve magnesium alloy and its preparation method and application
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
CN111041265A (en) * 2019-11-11 2020-04-21 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
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
CN116043086A (en) * 2022-12-19 2023-05-02 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
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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