CN111172438B - High-strength low-temperature rapid degradation magnesium alloy containing Na and preparation method thereof - Google Patents

High-strength low-temperature rapid degradation magnesium alloy containing Na and preparation method thereof Download PDF

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CN111172438B
CN111172438B CN202010061499.2A CN202010061499A CN111172438B CN 111172438 B CN111172438 B CN 111172438B CN 202010061499 A CN202010061499 A CN 202010061499A CN 111172438 B CN111172438 B CN 111172438B
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magnesium alloy
alloy
temperature
magnesium
strength low
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CN111172438A (en
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张跃忠
胡芳怡
刘宝胜
任晓霞
卫英慧
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Taiyuan University of Science and Technology
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Taiyuan University of Science and Technology
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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
    • 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
    • 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
    • C22C23/06—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
    • E—FIXED CONSTRUCTIONS
    • E21—EARTH DRILLING; MINING
    • E21B—EARTH DRILLING, e.g. DEEP DRILLING; OBTAINING OIL, GAS, WATER, SOLUBLE OR MELTABLE MATERIALS OR A SLURRY OF MINERALS FROM WELLS
    • E21B43/00—Methods or apparatus for obtaining oil, gas, water, soluble or meltable materials or a slurry of minerals from wells
    • E21B43/25—Methods for stimulating production
    • E21B43/26—Methods for stimulating production by forming crevices or fractures

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Geology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Mining & Mineral Resources (AREA)
  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Environmental & Geological Engineering (AREA)
  • Fluid Mechanics (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Extrusion Of Metal (AREA)

Abstract

The invention discloses a high-strength low-temperature rapid degradation magnesium alloy containing Na and a preparation method thereof, wherein the percentage of each element in the alloy is as follows: al: 3.0% -10.0%, Zr: 0.05% -0.3%, Mn: 0.4% -1.2%, Gd: 5.0% -8.0%, Na: 0.5 to 2.0 percent, and the balance of magnesium and other inevitable impurities. Al can enhance the strength of the alloy, and Zr and Mn can refine crystal grains and improve the strength of the alloy. The preparation method is combined with the preparation method of the invention, which can ensure that the material can realize rapid degradation at low temperature and effectively meet the requirement of the plugging material in the oil exploitation process.

Description

High-strength low-temperature rapid degradation magnesium alloy containing Na and preparation method thereof
Technical Field
The invention relates to the field of magnesium alloy materials, in particular to a high-strength low-temperature rapid degradation magnesium alloy containing Na and a preparation method thereof.
Background
With the increase of energy and the development of petroleum, the exploitation and utilization of oil and gas has become the focus of many resource researches. The exploitation of natural gas and oil gas needs to solve the problems of poor circulation, low permeability and the like in the reservoir. The fracturing technology is a core technology, and in the fracturing process, a pressure-holding ball is used as a core of fracturing work and is increasingly widely applied. The pressure-building ball for plugging is a key material during operation, and must be conveyed to a preset position underground through an aboveground tool to perform segmentation, layered plugging and fracturing until the underground operation is finished. The novel blocking ball material is developed, can be automatically decomposed within a certain time after fracturing is finished, and by combining the general use environment of a pressure building ball, the soluble pressure building ball needs to have certain mechanical properties, so that the pressure building ball still can keep complete and not deform in high-pressure fracturing operation, and meanwhile, the material also needs to have a degradation speed at a certain temperature, and the normal production of a reservoir stratum is guaranteed. The requirements of different oil and gas areas on the blocking ball are different, and the pressure-holding ball disclosed by the invention is used for meeting the requirements that the pressure-holding ball is used for exploiting oil and gas in a low-temperature environment of less than 20 ℃ and has good pressure-holding and rapid dissolving capabilities.
Disclosure of Invention
The invention aims to solve the technical problem of providing a high-strength low-temperature rapid degradation magnesium alloy material containing Na aiming at the technical current situation.
The technical scheme adopted by the invention for solving the technical problems is as follows: a high-strength low-temperature fast degradation magnesium alloy containing Na comprises the following components in percentage by weight: al: 3.0% -10.0%, Zr: 0.05% -0.3%, Mn: 0.4% -1.2%, Gd: 5.0% -8.0%, Na: 0.5 to 2.0 percent, and the balance of magnesium and other inevitable impurities.
Al can increase the strength of the magnesium alloy, but too high an amount of Al can embrittle the magnesium alloy. Gd is dissolved in the magnesium matrix in a solid mode, the structure can be refined, the yield strength and the high-temperature tensile strength are improved after the solution treatment, the solubility in the magnesium matrix is 8.0%, and the Gd is added in an amount of 5% -8% comprehensively. Zr and Mn can obviously refine grains and improve strength. Mn can reduce the generation of plastic defects and inhibit the growth of crystal grains. The addition of Na element is beneficial to improving the degradation rate of the alloy at low temperature.
The invention relates to a preparation method of a high-strength low-temperature fast-degradation magnesium alloy containing Na, which comprises the following components in percentage by weight: al: 3.0% -10.0%, Zr: 0.05% -0.3%, Mn: 0.4% -1.2%, Gd: 5.0% -8.0%, Na: 0.5 to 2.0 percent, and the balance of magnesium and other inevitable impurities; the method comprises the following steps:
accurately batching materials according to the component proportion of the Na-containing high-strength low-temperature rapid degradation magnesium alloy, smelting a magnesium ingot and an Mg-Mn alloy at 700-720 ℃, adding pure Al, an Mg-Zr intermediate alloy and an Mg-Gd intermediate alloy after melting, simultaneously introducing inert gas into a furnace for protection, and preserving heat for 30min at 650-700 ℃;
secondly, continuously and slowly heating the furnace to 750-780 ℃, adding Al-Na intermediate alloy, slowly stirring, after melting, keeping the temperature and standing for 20-30min to obtain magnesium alloy melt;
thirdly, pouring the magnesium alloy melt obtained in the second step into a preheated mold at 300-400 ℃, and cooling to obtain a magnesium alloy ingot;
and fourthly, extruding the magnesium alloy ingot at 420 ℃, wherein the extrusion speed is 3 m/min, and the extrusion ratio is 8.
The magnesium alloy prepared by the method has the compressive strength of 324-342 Mpa at 20 ℃ and the corrosion rate of 46 mg/cm in a 3% KCl solution at 20 DEG C2·h~56 mg/cm2H, the compression resistance requirement of the material on the plugging material in the oil exploitation process can be ensured, and meanwhile, the rapid degradation can be realized at a relatively low temperature. The material effectively meets the requirements of different oil and gas areas (especially cold areas) on pressure building balls in the oil and gas exploitation process.
Detailed Description
Case 1
In this embodiment, the magnesium alloy contains 5.0% of Gd, 0.25% of Zr, 0.5% of Mn, 6.0% of Al, and 0.5% of Na.
Firstly, according to the proportion of the invention, the magnesium ingot and the Mg-Mn alloy are smelted together at 700-720 ℃, after the smelting, pure Al, Mg-Zr intermediate alloy and Mg-Gd intermediate alloy are added, meanwhile, inert gas is introduced into the furnace for protection, the temperature is kept for 30min at 650-700 ℃,
and secondly, continuously heating the furnace at the speed of 5 ℃/min until the temperature reaches 750 ℃, adding Al-Na intermediate alloy, slowly stirring, and standing for 20 min after melting.
Thirdly, pouring the obtained magnesium alloy melt into a preheated die at 400 ℃ and cooling to obtain a magnesium alloy ingot.
The compressive strength of the prepared Na-containing high-strength low-temperature rapid degradation magnesium alloy at 20 ℃ is 324Mpa, and the corrosion rate of the prepared Na-containing high-strength low-temperature rapid degradation magnesium alloy at 20 ℃ in a 3% KCl solution is 46 mg/cm2·h。
Case 2
In this embodiment, the magnesium alloy contains 6.0% of Gd, 0.25% of Zr, 1.0% of Mn, 3.0% of Al, and 1.0% of Na.
Firstly, according to the proportion of the invention, the magnesium ingot and the Mg-Mn alloy are smelted together at 700-720 ℃, after the smelting, pure Al, Mg-Zr intermediate alloy and Mg-Gd intermediate alloy are added, meanwhile, inert gas is introduced into the furnace for protection, the temperature is kept for 30min at 650-700 ℃,
and secondly, continuously heating the furnace at the speed of 5 ℃/min until the temperature reaches 760 ℃, adding Al-Na intermediate alloy, slowly stirring, and standing for 20 min after melting.
Thirdly, pouring the obtained magnesium alloy melt into a preheated 300 ℃ mold, and cooling to obtain a magnesium alloy ingot.
Fourthly, extruding at the temperature of 420 ℃, wherein the extruding speed is 3 m/min, and the extruding ratio is 8.
The prepared Na-containing high-strength low-temperature rapid degradation magnesium alloy has the compressive strength of 331Mpa at 20 ℃ and the corrosion rate of 49 mg/cm under the KCl solution with the temperature of 20 ℃ and the concentration of 3 percent2·h。
Case 3
In this embodiment, the magnesium alloy contains 5.5% of Gd, 0.1% of Zr, 1.2% of Mn, 8.0% of Al, and 1.5% of Na.
Firstly, according to the proportion of the invention, the magnesium ingot and the Mg-Mn alloy are smelted together at 700-720 ℃, after the smelting, pure Al, Mg-Zr intermediate alloy and Mg-Gd intermediate alloy are added, meanwhile, inert gas is introduced into the furnace for protection, the temperature is kept for 30min at 650-700 ℃,
and secondly, continuously heating the furnace at the speed of 5 ℃/min until the temperature reaches 750-780 ℃, adding Al-Na intermediate alloy, slowly stirring, and standing for 30min after melting.
Thirdly, pouring the obtained magnesium alloy melt into a preheated mold at 300-400 ℃ and cooling to obtain a magnesium alloy ingot.
Fourthly, extruding at the temperature of 420 ℃, wherein the extruding speed is 3 m/min, and the extruding ratio is 8.
The prepared Na-containing high-strength low-temperature rapid degradation magnesium alloy has the compressive strength of 324Mpa at 20 ℃ and the corrosion rate of 46 mg/cm in a 3% KCl solution at 20 DEG C2·h。
Case 4
In this embodiment, the magnesium alloy contains 5.5% of Gd, 0.3% of Zr, 0.7% of Mn, 10.0% of Al, and 2.0% of Na.
Firstly, according to the proportion of the invention, the magnesium ingot and the Mg-Mn alloy are smelted together at 700-720 ℃, after the smelting, pure Al, Mg-Zr intermediate alloy and Mg-Gd intermediate alloy are added, meanwhile, inert gas is introduced into the furnace for protection, the temperature is kept for 30min at 650-700 ℃,
and secondly, continuously heating the furnace at the speed of 5 ℃/min until the temperature reaches 750 ℃, adding Al-Na intermediate alloy, slowly stirring, and standing for 25 min after melting.
Thirdly, pouring the obtained magnesium alloy melt into a preheated 350 ℃ die, and cooling to obtain a magnesium alloy ingot.
Fourthly, extruding at the temperature of 420 ℃, wherein the extruding speed is 3 m/min, and the extruding ratio is 8.
The prepared Na-containing high-strength low-temperature rapid degradation magnesium alloy has the compression strength of 342Mpa at 20 ℃ and the corrosion rate of 56 mg/cm in a 3% KCl solution at 20 DEG C2·h。

Claims (3)

1. A preparation method of a high-strength low-temperature fast-degradation magnesium alloy containing Na comprises the following components in percentage by weight: 5.5% of Gd, 0.3% of Zr, 0.7% of Mn, 10.0% of Al and 2.0% of Na;
the method comprises the following steps:
accurately batching according to the proportion, smelting a magnesium ingot and Mg-Mn alloy together at 700-720 ℃, adding pure Al, Mg-Zr intermediate alloy and Mg-Gd intermediate alloy after melting, simultaneously introducing inert gas into a furnace for protection, and preserving heat for 30min at 650-700 ℃;
heating the furnace at the speed of 5 ℃/min to 750 ℃, adding Al-Na intermediate alloy, slowly stirring, keeping the temperature for 25 min after the Na element in the Al-Na intermediate alloy is melted, wherein the mass content of the Na element in the Al-Na intermediate alloy is 5%;
thirdly, pouring the obtained magnesium alloy melt into a preheated 350 ℃ die, and cooling to obtain a magnesium alloy ingot;
fourthly, extruding at the temperature of 420 ℃, wherein the extruding speed is 3 m/min, and the extruding ratio is 8.
2. The method for preparing a high-strength low-temperature rapidly degradable magnesium alloy containing Na according to claim 1, wherein the inert gas used is CO2And SF6Mixed gas of (2), CO2And SF6The volume ratio is 200-400: 1.
3. the method for preparing a high-strength low-temperature rapidly degradable magnesium alloy containing Na according to claim 2, wherein CO is2And SF6The volume ratio is 300: 1.
CN202010061499.2A 2020-01-15 2020-01-15 High-strength low-temperature rapid degradation magnesium alloy containing Na and preparation method thereof Active CN111172438B (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2011117630A1 (en) * 2010-03-25 2011-09-29 Magnesium Elektron Limited Magnesium alloy containing heavy rare earths
CN102747261A (en) * 2011-04-19 2012-10-24 株式会社神户制钢所 Magnesium alloy material and engine part
WO2016118444A1 (en) * 2015-01-23 2016-07-28 University Of Florida Research Foundation, Inc. Radiation shielding and mitigating alloys, methods of manufacture thereof and articles comprising the same
CN107523732A (en) * 2017-08-15 2017-12-29 太原科技大学 A kind of magnesium alloy of fast degradation containing Na and preparation method thereof
CN108085548A (en) * 2017-11-28 2018-05-29 袁颖宏 A kind of quick dissolving has functional mechanical characteristic magnesium alloy and its manufacturing method
CN109988955A (en) * 2019-04-22 2019-07-09 重庆科技学院 A kind of high-elongation low temperature fast degradation magnesium alloy and preparation method thereof

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2011117630A1 (en) * 2010-03-25 2011-09-29 Magnesium Elektron Limited Magnesium alloy containing heavy rare earths
CN102747261A (en) * 2011-04-19 2012-10-24 株式会社神户制钢所 Magnesium alloy material and engine part
WO2016118444A1 (en) * 2015-01-23 2016-07-28 University Of Florida Research Foundation, Inc. Radiation shielding and mitigating alloys, methods of manufacture thereof and articles comprising the same
CN107523732A (en) * 2017-08-15 2017-12-29 太原科技大学 A kind of magnesium alloy of fast degradation containing Na and preparation method thereof
CN108085548A (en) * 2017-11-28 2018-05-29 袁颖宏 A kind of quick dissolving has functional mechanical characteristic magnesium alloy and its manufacturing method
CN109988955A (en) * 2019-04-22 2019-07-09 重庆科技学院 A kind of high-elongation low temperature fast degradation magnesium alloy and preparation method thereof

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