CN109694976B - Low-cost soluble magnesium alloy and preparation method and application thereof - Google Patents

Low-cost soluble magnesium alloy and preparation method and application thereof Download PDF

Info

Publication number
CN109694976B
CN109694976B CN201910189609.0A CN201910189609A CN109694976B CN 109694976 B CN109694976 B CN 109694976B CN 201910189609 A CN201910189609 A CN 201910189609A CN 109694976 B CN109694976 B CN 109694976B
Authority
CN
China
Prior art keywords
alloy
magnesium alloy
ingot
extrusion
low
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN201910189609.0A
Other languages
Chinese (zh)
Other versions
CN109694976A (en
Inventor
刘运腾
刘聪
林涛
周吉学
刘洪涛
庄海华
马百常
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Chongqing Yuhua New Materials Technology Co.,Ltd.
Original Assignee
New Material Institute of Shandong Academy of Sciences
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by New Material Institute of Shandong Academy of Sciences filed Critical New Material Institute of Shandong Academy of Sciences
Priority to CN201910189609.0A priority Critical patent/CN109694976B/en
Publication of CN109694976A publication Critical patent/CN109694976A/en
Application granted granted Critical
Publication of CN109694976B publication Critical patent/CN109694976B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C23/00Alloys based on magnesium
    • C22C23/02Alloys based on magnesium with aluminium as the next major constituent
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/02Making non-ferrous alloys by melting
    • C22C1/03Making non-ferrous alloys by melting using master alloys
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C23/00Alloys based on magnesium

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Continuous Casting (AREA)

Abstract

The invention belongs to the technical field of metal materials and processingThe low-cost soluble magnesium alloy can be used for preparing related parts of shale oil and gas exploitation by a multistage sliding sleeve staged fracturing technology. The alloy is Mg-Al-Ca-Mn-Cu-Ni magnesium alloy and consists of the following elements in percentage by mass: 0.20 to 0.50wt% of Al, 0.20 to 1.00 wt% of Ca, 0.30 to 1.10 wt% of Mn, 0.10 to 1.20 wt% of Cu, 0.10 to 0.50wt% of Ni, and the balance of Mg and inevitable impurity elements. The low-cost soluble magnesium alloy prepared by the invention has the tensile strength of more than or equal to 280MPa, the yield strength of more than or equal to 240MPa and the elongation of more than or equal to 14 percent; the dissolution rate in 3% KCl solution at 93 deg.C is 50-60mg cm 2h‑1

Description

Low-cost soluble magnesium alloy and preparation method and application thereof
Technical Field
The invention belongs to the technical field of metal materials and processing, and particularly relates to a low-cost soluble magnesium alloy, a preparation method and application thereof, which can be used for preparing relevant parts of shale oil and gas exploitation by a multistage sliding sleeve staged fracturing technology.
Background
The development of scientific technology has prompted an increasing level of global industrial automation, which has led to a further increase in energy demand. Shale oil and gas has high economic value as one of the important directions of energy field development in the current and future period, and related mining technologies have been successful in the United states and gradually popularized to the world. According to statistics, the shale gas reserves of China are the first in the world, the shale oil reserves are the third in the world, and the future development prospect is wide. However, related mining technologies are still in a starting price stage, and the current mainstream technology is a multi-stage sliding sleeve staged fracturing technology commonly used for horizontal well mining. One key component of the technology is the fracturing tool, including a temporary plugging ball, a ball seat, a bridge plug, a sliding sleeve and the like. The tool has the characteristics of dissolubility, good strength and elongation rate and the like in the fracturing process.
At present, the soluble materials developed at home and abroad aiming at the tools are mostly high polymer materials, composite materials, aluminum alloys and magnesium alloys. The high molecular material has low mechanical property and is not easy to decompose in a high-temperature corrosion medium. The composite material mostly adopts nanoscale metal powder, so that the material cost is greatly increased, and the application and popularization of the composite material are also hindered.
The patent "a pressure-resistant rapidly-degradable cast aluminum alloy and a preparation method thereof" (application No. 201710327729.3) and the patent "a light pressure-resistant rapidly-degradable cast magnesium alloy" (application No. CN201310284659.X) respectively disclose a rapidly-dissolvable cast aluminum alloy and a cast magnesium alloy. However, the inventors found that: the aluminum alloy and magnesium alloy products obtained by the casting process have obvious casting structure characteristics: dendrite structure, coarse grains and different degrees of component segregation; this leads to low mechanical properties of the product and to an inhomogeneous stabilization of the dissolution process.
Disclosure of Invention
Aiming at the problems, the invention provides a low-cost soluble magnesium alloy and a preparation method and application thereof. The soluble magnesium alloy does not contain expensive rare earth elements, has good mechanical property and uniform and stable dissolution rate on the basis of realizing low cost; the alloy is a dissoluble magnesium alloy with good comprehensive performance. The extrusion speed adopted in the preparation process of the soluble magnesium alloy can reach 20 m/min.
The invention adopts the following technical scheme:
in a first aspect of the invention, a low-cost soluble magnesium alloy is provided, and the low-cost soluble magnesium alloy is a Mg-Al-Ca-Mn-Cu-Ni magnesium alloy and consists of the following elements in percentage by mass: 0.20 to 0.50wt% of Al, 0.20 to 1.00 wt% of Ca, 0.30 to 1.10 wt% of Mn, 0.10 to 1.20 wt% of Cu, 0.10 to 0.50wt% of Ni, and the balance of Mg and inevitable impurity elements.
The inevitable impurities in the invention are less than or equal to 0.050%.
In a second aspect of the present invention, there is provided a method for preparing the above-mentioned low-cost soluble magnesium alloy, comprising the steps of: weighing a pure magnesium ingot, a pure aluminum ingot, a Mg-Ca intermediate alloy, a Mg-Mn intermediate alloy, a Mg-Cu intermediate alloy and a Mg-Ni intermediate alloy; introducing protective gas, smelting and casting into an ingot; homogenizing the cast ingot, cutting into blanks with corresponding sizes, and peeling; hot extrusion to obtain a bar; the hot extrusion conditions are as follows: the extrusion temperature is 350-400 ℃, the extrusion ratio is 4-10, and the extrusion speed is 10-20 m/min; the extrusion temperature is preferably 350 ℃.
In a third aspect of the invention, the application of the low-cost soluble magnesium alloy in preparing the soluble parts in the shale oil and gas exploitation process is provided.
The invention achieves the following beneficial results:
(1) the Mg-Al-Ca-Mn-Cu-Ni alloy of the invention refines the grain size of the cast ingot through Mn and Ca, further reduces the segregation of the cast ingot, ensures that Cu and Ni in the material are uniformly distributed, and forms fine and dispersed Mg2Cu and Mg2Ni to achieve the purpose of uniform dissolution. The low-cost soluble magnesium alloy prepared by the invention has the tensile strength of more than or equal to 280MPa, the yield strength of more than or equal to 240MPa and the elongation of more than or equal to 14 percent; the dissolution rate in a 3% KCl solution at 93 ℃ is 50-60mg cm-2h-1
(2) The alloy of the invention weakens the basal plane texture of the magnesium alloy by adding Ca element, thereby improving the elongation of the material. In addition, Ca has the effects of flame retardance and oxidation resistance, and the ignition point of the alloy is improved. Therefore, the consumption of protective gas is reduced in the smelting process; gas protection is not needed in the homogenization treatment process, and the extrusion speed can reach 20m/min in the extrusion process.
(3) In the invention, a small amount of Al element is added into the alloy, so that the strength of the material is improved in a solid solution strengthening mode, and a small amount of high-melting-point (Mg, Al) can be formed2Ca and Al8Mn5The second phase of (2) improves the strength of the material by means of dispersion strengthening.
(4) The soluble magnesium alloy can be rapidly extruded under the conditions of 350-400 ℃ high temperature and the extrusion ratio less than 10 to obtain the soluble magnesium alloy with good mechanical property. The deformation caused by introducing the protective gas and the small extrusion ratio can reduce the deformation resistance in the processing process, improve the forming rate and reduce the equipment loss on one hand; on the other hand, a small-tonnage device can be adopted to process a large-size product, and the investment of fixed assets such as equipment and the like is reduced.
(5) The soluble magnesium alloy only adds a small amount of expensive Ni element, thus the cost of the alloy is increased a little; meanwhile, the material has high processing rate and low cost, so the application prospect is better.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate exemplary embodiments of the invention and together with the description serve to explain the invention and not to limit the invention.
FIG. 1 is a microstructure of a magnesium alloy prepared in test example group 1.
FIG. 2 is a microstructure of a magnesium alloy prepared in test example group 6.
Detailed Description
It is to be understood that the following detailed description is exemplary and is intended to provide further explanation of the invention as claimed. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the invention. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of the stated features, steps, operations, and/or combinations thereof, unless the context clearly indicates otherwise.
In view of the problems in the background art, the invention provides, in a first aspect, a low-cost soluble magnesium alloy, which is a Mg-Al-Ca-Mn-Cu-Ni magnesium alloy, and consists of the following elements in percentage by mass: 0.20 to 0.50wt% of Al, 0.20 to 1.00 wt% of Ca, 0.30 to 1.10 wt% of Mn, 0.10 to 1.20 wt% of Cu, 0.10 to 0.50wt% of Ni, and the balance of Mg and inevitable impurity elements.
Further, the low-cost soluble magnesium alloy consists of the following elements in percentage by mass: 0.30 to 0.50wt% of Al, 0.80 to 1.00 wt% of Ca, 0.30 to 0.70 wt% of Mn, 0.30 to 0.90 wt% of Cu, 0.20 to 0.40 wt% of Ni, and the balance of Mg and inevitable impurity elements.
Further, the low-cost soluble magnesium alloy consists of the following elements in percentage by mass: 0.50wt% of Al, 0.90 wt% of Ca, 0.55 wt% of Mn, 0.40 wt% of Cu, 0.30 wt% of Ni, and the balance of Mg and inevitable impurity elements.
Because of active chemical properties of the magnesium alloy, oxidation combustion is easy to occur in the melting and casting processes under the condition of no protection, the ignition temperature of the alloy can be improved by proper alloying, and the cost and the accident risk in the melting and casting processes are reduced; in addition, the magnesium alloy belongs to a close-packed hexagonal metal structure, a room-temperature slip system is less, hot forming processing is needed, high alloying can increase material cost, and the forming performance is reduced, and defects such as oxidation, cracks and the like are easy to occur in the extrusion process. Therefore, the selection and content control of alloying elements have a significant influence on the processing cost of the material and the product quality, mechanical properties and dissolution rate. The magnesium alloy achieves the purposes of low cost, easy forming, moderate strength, elongation and dissolubility by optimizing the alloy elements and the content thereof.
Al is the most economical element for improving the strength of the wrought magnesium alloy. The Ca element can obviously improve the ignition temperature of the magnesium alloy and refine the ingot casting structure. Mn element can also refine the grain structure of the magnesium alloy ingot. In addition, Al and Ca can form a high melting point (Mg, Al) with Mg2A Ca phase; al and Mn elements may also form high melting point Al8Mn5And (4) phase(s). The strength of the magnesium alloy is improved and better elongation is kept through micro-alloying of Al, Ca and Mn.
Cu and Ni are conventionally considered as impurity elements, which increase the corrosion rate of magnesium alloys. According to the invention, by controlling the contents of Cu and Ni elements, fine Mg2Cu and Mg2Ni phases are obtained in the magnesium alloy structure, so that the soluble magnesium alloy can be prepared.
In a second aspect of the present invention, there is provided a method for preparing the above-mentioned low-cost soluble magnesium alloy, comprising the steps of: weighing a pure magnesium ingot, a pure aluminum ingot, a Mg-Ca intermediate alloy, a Mg-Mn intermediate alloy, a Mg-Cu intermediate alloy and a Mg-Ni intermediate alloy; introducing protective gas, smelting and casting into an ingot; homogenizing the cast ingot, cutting into blanks with corresponding sizes, and peeling; hot extrusion to obtain a bar; the hot extrusion conditions are as follows: the extrusion temperature is 350-400 ℃, the extrusion ratio is 4-10, and the extrusion speed is 10-20 m/min; the extrusion temperature is preferably 350 ℃. The method has the advantages of small extrusion ratio, high extrusion speed and reduced equipment loss.
Further, the hot extrusion conditions are: the extrusion temperature is 350 ℃, the extrusion ratio is 8, and the extrusion speed is 20 m/min. The soluble magnesium alloy prepared under the hot extrusion condition has the best performances such as solubility, tensile strength, elongation percentage and the like. The invention can prepare the bar with larger size by adopting the lower extrusion ratio, and can reduce the tonnage of the required extruder equipment.
Further, the step of melting and casting into an ingot comprises: weighing a pure magnesium ingot, a pure aluminum ingot, an Mg-Ca intermediate alloy, an Mg-Mn intermediate alloy, an Mg-Cu intermediate alloy and an Mg-Ni intermediate alloy according to a ratio, introducing protective gas, smelting at 720-740 ℃, preserving heat for 40-60 min, stirring for 5-10 min, refining for 20-30 min, heating to 740-760 ℃ after refining, standing for 30-40 min, and casting into ingots at 720-740 ℃; preferably, the smelting is carried out at 730 ℃, the heat preservation is carried out for 60min, the stirring is carried out for 10min, the refining is carried out for 20min, the temperature is raised to 760 ℃ after the refining, the standing is carried out for 40min, and the casting ingot is cast at 720 ℃.
Further, the shielding gas used is CO2And SF6Mixed gas of (2), CO2And SF6The volume ratio is 200-400: 1; preferably, CO2And SF6The volume ratio is 300: 1. The mixed gas has the most obvious effect of preventing the oxidation in the preparation process of the alloy.
Further, homogenizing at 480-520 ℃ for 1-4 h, cooling by air, cutting into corresponding blanks, and peeling; preferably, the homogenization treatment is carried out at 500 ℃ for a holding time of 2 h. The invention adopts higher homogenization temperature, on one hand, the invention can promote the micro-alloy to be dissolved into the magnesium alloy matrix as soon as possible, and the heat treatment cost is reduced; on the other hand, the homogenization heat preservation time can be shortened, and the cast structure can be prevented from coarsening.
In a third aspect of the invention, the application of the low-cost soluble magnesium alloy in preparing the soluble parts in the shale oil and gas exploitation process is provided.
Further, the low-cost soluble magnesium alloy is applied to the preparation of relevant parts of shale oil and gas exploitation by adopting a multistage sliding sleeve staged fracturing technology. The soluble magnesium alloy has the advantages of high dissolution rate, high tensile strength and the like, and has wide application prospect in preparation of relevant parts of shale oil and gas exploitation by adopting a multistage sliding sleeve staged fracturing technology.
In order to make the technical solution of the present invention more clearly understood by those skilled in the art, the technical solution of the present invention will be described in detail below with reference to specific examples and comparative examples.
Example 1A Low cost soluble magnesium alloy
The low-cost soluble magnesium alloy is Mg-Al-Ca-Mn-Cu-Ni magnesium alloy and consists of the following elements in percentage by mass: 0.50wt% of Al, 0.90 wt% of Ca, 0.55 wt% of Mn, 0.40 wt% of Cu, 0.30 wt% of Ni, and the balance of Mg and inevitable impurity elements.
Example 2A Low cost soluble magnesium alloy
The low-cost soluble magnesium alloy is Mg-Al-Ca-Mn-Cu-Ni magnesium alloy and consists of the following elements in percentage by mass: 0.40 wt% of Al, 0.50wt% of Ca, 0.45 wt% of Mn, 0.90 wt% of Cu, 0.10 wt% of Ni, and the balance of Mg and inevitable impurity elements.
Example 3A Low cost soluble magnesium alloy
The low-cost soluble magnesium alloy is Mg-Al-Ca-Mn-Cu-Ni magnesium alloy and consists of the following elements in percentage by mass: 0.30 wt% of Al, 1.00 wt% of Ca, 0.90 wt% of Mn, 1.0 wt% of Cu, 0.50wt% of Ni, and the balance of Mg and inevitable impurity elements.
Example 4A Low cost soluble magnesium alloy
The low-cost soluble magnesium alloy is Mg-Al-Ca-Mn-Cu-Ni magnesium alloy and consists of the following elements in percentage by mass: 0.40 wt% of Al, 1.00 wt% of Ca, 1.00 wt% of Mn, 1.2 wt% of Cu, 0.50wt% of Ni, and the balance of Mg and inevitable impurity elements.
Example 5 preparation method of low-cost soluble magnesium alloy
The raw materials are as follows: pure magnesium ingot, pure aluminum ingot, Mg-25% Ca intermediate alloy, Mg-10% Mn intermediate alloy, Mg-30% Cu intermediate alloy, Mg-25% Ni intermediate alloy.
Weighing raw materials according to a ratio, wherein the raw materials adopt a pure magnesium ingot, a pure aluminum ingot, Mg-25% Ca intermediate alloy and Mg-10% Mn intermediate alloy; in CO2+SF6Smelting at 720 ℃ under the protection of mixed gas (volume ratio of 300:1), preserving heat for 60min, stirring for 10min, refining for 20min, heating to 740 ℃ after refining, standing for 30min, and casting into ingots at 720 ℃.
Homogenizing the cast ingot at 520 deg.C for 2h, cooling by air cooling, cutting into corresponding blanks, and peeling.
And extruding the blank obtained in the last step into a bar by an extruder under the conditions of extrusion temperature of 350 ℃, extrusion ratio of 5 and extrusion speed of 20m/min, thus obtaining the bar.
Example 6 preparation method of low-cost soluble magnesium alloy
The raw materials are as follows: pure magnesium ingot, pure aluminum ingot, Mg-25% Ca intermediate alloy, Mg-10% Mn intermediate alloy, Mg-30% Cu intermediate alloy, Mg-25% Ni intermediate alloy.
Weighing raw materials according to a ratio, wherein the raw materials comprise pure magnesium ingots, pure aluminum ingots, pure tin ingots, Mg-25% Ca intermediate alloy and Mg-10% Mn intermediate alloy; in CO2+SF6Smelting at 740 ℃ under the protection of mixed gas (volume ratio of 400:1), preserving heat for 40min, stirring for 5min, refining for 30min, raising temperature to 760 ℃ after refining, standing for 40min, and casting into ingots at 740 ℃.
Homogenizing the cast ingot at 500 deg.C for 2h, cooling by air cooling, cutting into corresponding blanks, and peeling.
Extruding the blank obtained in the last step into a bar by an extruder under the conditions of extrusion temperature of 400 ℃, extrusion ratio of 8 and extrusion speed of 20 m/min.
Example 7 preparation method of low-cost soluble magnesium alloy
The raw materials are as follows: pure magnesium ingot, pure aluminum ingot, Mg-25% Ca intermediate alloy, Mg-10% Mn intermediate alloy, Mg-30% Cu intermediate alloy, Mg-25% Ni intermediate alloy.
Weighing raw materials according to a ratio, wherein the raw materials comprise pure magnesium ingots, pure aluminum ingots, pure tin ingots, Mg-25% Ca intermediate alloy and Mg-10% Mn intermediate alloy; in CO2+SF6Smelting at 720 ℃ under the protection of mixed gas (volume ratio of 400:1), preserving heat for 40min, stirring for 5min, refining for 30min, heating to 750 ℃ after refining, standing for 30min, and casting into ingots at 730 ℃.
Homogenizing the cast ingot at 510 deg.C for 1h, cooling by air cooling, cutting into corresponding blanks, and peeling.
Extruding the blank obtained in the last step into a bar by an extruder under the conditions of extrusion temperature of 390 ℃, extrusion ratio of 10 and extrusion speed of 10 m/min.
Embodiment 8 preparation method of low-cost soluble magnesium alloy
The raw materials are as follows: pure magnesium ingot, pure aluminum ingot, Mg-25% Ca intermediate alloy, Mg-10% Mn intermediate alloy, Mg-30% Cu intermediate alloy, Mg-25% Ni intermediate alloy.
Weighing raw materials according to a ratio, wherein the raw materials comprise pure magnesium ingots, pure aluminum ingots, pure tin ingots, Mg-25% Ca intermediate alloy and Mg-10% Mn intermediate alloy; in CO2+SF6Smelting at 720 ℃ under the protection of mixed gas (volume ratio of 300:1), preserving heat for 40min, stirring for 10min, refining for 30min, heating to 740 ℃ after refining, standing for 30min, and casting into ingots at 720 ℃.
Homogenizing the cast ingot at 500 deg.C for 2h, cooling by air cooling, cutting into corresponding blanks, and peeling.
Extruding the blank obtained in the last step into a bar by an extruder under the conditions of extrusion temperature of 380 ℃, extrusion ratio of 10 and extrusion speed of 5 m/min.
Comparative example 1
The comparative alloy is an as-cast AZ91D magnesium alloy, and the chemical composition of the alloy is as follows: mg-9.0 wt% Al-0.80 wt% Zn-0.3 wt% Mn-0.025 wt% Cu, and alloy ingredients (raw materials are pure magnesium ingot, pure aluminum ingot, pure zinc ingot, Mg-10% Mn intermediate alloy and Mg-30% Cu intermediate alloy).
Comparative example 2:
the difference from the embodiment 1 is that the Mg-Al-Ca-Mn-Cu-Ni alloy elements have the following mass percentages: 0.70wt% of Al, 1.20 wt% of Ca, 1.00 wt% of Mn, 1.5 wt% of Cu, 1.50 wt% of Ni and the balance of Mg and inevitable impurity elements.
Comparative example 3:
the difference from the embodiment 1 is that the Mg-Al-Ca-Mn-Cu-Ni alloy elements have the following mass percentages: 0.30wt% of Al, 0.20 wt% of Ca, 0.10 wt% of Mn, 0.05 wt% of Cu, 0.05 wt% of Ni and the balance of Mg and inevitable impurity elements.
Comparative example 4
The difference from example 7 was that a rod was extruded at an extrusion temperature of 450 ℃ and an extrusion ratio of 10 at an extrusion speed of 10 m/min.
Comparative example 5
The difference from example 5 was that the extrusion ratio was 40, and the bar was extruded at an extrusion speed of 10 m/min.
Comparative example 6
The difference from example 5 was that the extrusion ratio was 80 and the extrusion speed was 10m/min, and a rod was extruded.
Test examples
Group 1: example 1 an alloy was prepared as in example 5;
group 2: example 2 an alloy was prepared as in example 6;
group 3: example 3 an alloy was prepared as in example 7;
group 4: example 4 an alloy was prepared as in example 8;
group 5: the alloy of comparative example 1 was prepared as in example 5;
group 6: the alloy of comparative example 2 was prepared as in example 5;
group 7: comparative example 3 the alloy was prepared according to the method of example 5;
group 8: example 1 the alloy was prepared according to the method of comparative example 4;
group 9: example 1 the alloy was prepared according to the method of comparative example 5;
group 10: example 1 the alloy was prepared according to the method of comparative example 6;
measuring the mechanical property and solubility of each group of alloy;
the mechanical property testing method is executed according to GB T228.1-2010.
The dissolution property test conditions are as follows: will be provided with
Figure BDA0001993988340000072
The sample (2) was placed in a 3% KCl aqueous solution at 93 ℃ and the weight dissolved per hour was measured. The dissolution rate was: weight dissolved/(sample surface area × time).
TABLE 1 magnesium alloy room-temperature mechanical properties and high-temperature dissolution rates
Figure BDA0001993988340000071
Figure BDA0001993988340000081
Comparing the room temperature mechanical properties and the high temperature dissolution rates of the magnesium alloys of the examples and the comparative examples, it can be seen that: the room temperature mechanical property of the low-cost dissoluble magnesium alloy prepared by the invention is obviously superior to that of the comparative alloy, and the dissolution rate of the alloy of the invention in a KCl solution with the temperature of 93 ℃ and the concentration of 3 percent is obviously superior to that of the comparative alloy.
From the microstructure morphology of the alloys of test example group 1 and test example group 6, it can be seen that: the grain size of the material prepared by the invention is uniform and fine; and the second phase is more dispersed (as shown in fig. 1, 2). Therefore, the room-temperature mechanical property of the alloy is obviously better than that of the comparative alloy.
By comparing test example groups 1, 9 and 10, it can be seen that: the mechanical properties of the material are further enhanced as the extrusion ratio is increased. The invention can achieve better performance by adopting smaller extrusion ratio, and is beneficial to the popularization and application of the alloy and the preparation method.
In conclusion, the low-cost dissolvable magnesium alloy can meet the performance requirements of different parts related to the multistage sliding sleeve staged fracturing technology in the shale oil and gas exploitation process.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.

Claims (14)

1. The low-cost soluble magnesium alloy is characterized by being Mg-Al-Ca-Mn-Cu-Ni magnesium alloy and comprising the following elements in percentage by mass: 0.20 to 0.50wt% of Al, 0.20 to 1.00 wt% of Ca, 0.30 to 1.10 wt% of Mn, 0.10 to 1.20 wt% of Cu, 0.10 to 0.50wt% of Ni, and the balance of Mg and inevitable impurity elements.
2. The low-cost soluble magnesium alloy according to claim 1, consisting of the following elements in mass percent: 0.30 to 0.50wt% of Al, 0.80 to 1.00 wt% of Ca, 0.30 to 0.70 wt% of Mn, 0.30 to 0.90 wt% of Cu, 0.20 to 0.40 wt% of Ni, and the balance of Mg and inevitable impurity elements.
3. The low-cost soluble magnesium alloy according to claim 1, consisting of the following elements in mass percent: 0.50wt% of Al, 0.90 wt% of Ca, 0.55 wt% of Mn, 0.40 wt% of Cu, 0.30 wt% of Ni, and the balance of Mg and inevitable impurity elements.
4. The method for preparing the low-cost soluble magnesium alloy according to any one of claims 1 to 3, comprising the following steps: weighing a pure magnesium ingot, a pure aluminum ingot, a Mg-Ca intermediate alloy, a Mg-Mn intermediate alloy, a Mg-Cu intermediate alloy and a Mg-Ni intermediate alloy; introducing protective gas, smelting and casting into an ingot; homogenizing the cast ingot, cutting into blanks with corresponding sizes, and peeling; hot extrusion to obtain a bar; the hot extrusion conditions are as follows: the extrusion temperature is 350-400 ℃, the extrusion ratio is 4-10, and the extrusion speed is 10-20 m/min.
5. The method of claim 4, wherein the extrusion temperature is 350 ℃.
6. The production method according to claim 4, wherein the hot extrusion conditions are: the extrusion temperature is 350 ℃, the extrusion ratio is 8, and the extrusion speed is 20 m/min.
7. The method of claim 4, wherein said step of melting and casting into an ingot comprises: weighing a pure magnesium ingot, a pure aluminum ingot, an Mg-Ca intermediate alloy, an Mg-Mn intermediate alloy, an Mg-Cu intermediate alloy and an Mg-Ni intermediate alloy according to a ratio, introducing protective gas, smelting at 720-740 ℃, preserving heat for 40-60 min, stirring for 5-10 min, refining for 20-30 min, heating to 740-760 ℃ after refining, standing for 30-40 min, and casting into an ingot at 720-740 ℃.
8. The preparation method of claim 7, wherein the smelting is carried out at 730 ℃, the temperature is kept for 60min, the stirring is carried out for 10min, the refining is carried out for 20min, the temperature is raised to 760 ℃ after the refining, the standing is carried out for 40min, and the mixture is cast into an ingot at 720 ℃.
9. The process according to claim 4, wherein the protective gas used is CO2And SF6Mixed gas of (2), CO2And SF6The volume ratio is 200-400: 1.
10. The method of claim 9, wherein the CO is2And SF6The volume ratio is 300: 1.
11. The preparation method according to claim 4, wherein the homogenization treatment is carried out at 480-520 ℃ for 1-4 h, and the cooling method is air cooling, and then the raw materials are cut into corresponding blanks and peeled.
12. The method of claim 11, wherein the homogenization treatment is carried out at 500 ℃ for 2 hours.
13. The use of the low-cost soluble magnesium alloy of any one of claims 1 to 3 in the preparation of soluble components in shale oil and gas exploitation.
14. The use according to claim 13, in the preparation of parts related to shale oil and gas exploitation using a multistage sliding sleeve staged fracturing technique.
CN201910189609.0A 2019-03-13 2019-03-13 Low-cost soluble magnesium alloy and preparation method and application thereof Active CN109694976B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201910189609.0A CN109694976B (en) 2019-03-13 2019-03-13 Low-cost soluble magnesium alloy and preparation method and application thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201910189609.0A CN109694976B (en) 2019-03-13 2019-03-13 Low-cost soluble magnesium alloy and preparation method and application thereof

Publications (2)

Publication Number Publication Date
CN109694976A CN109694976A (en) 2019-04-30
CN109694976B true CN109694976B (en) 2020-03-17

Family

ID=66233860

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201910189609.0A Active CN109694976B (en) 2019-03-13 2019-03-13 Low-cost soluble magnesium alloy and preparation method and application thereof

Country Status (1)

Country Link
CN (1) CN109694976B (en)

Families Citing this family (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110284033B (en) * 2019-08-05 2020-11-24 深圳市爱斯特新材料科技有限公司 High-strength Mg-Zn-Al-based microalloyed magnesium alloy and preparation method thereof
CN110923531B (en) * 2019-11-14 2022-02-01 大同高镁科技有限公司 Low-cost high-plasticity soluble magnesium alloy material and preparation method thereof
CN111041309B (en) * 2019-12-08 2020-10-16 江苏奇纳新材料科技有限公司 Soluble magnesium-based alloy and preparation method 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
US20230392235A1 (en) * 2022-06-03 2023-12-07 Cnpc Usa Corp Dissolvable magnesium alloy
CN115466890B (en) * 2022-09-19 2023-12-01 重庆科技学院 High-strength and high-toughness Cu-containing magnesium alloy material capable of being rapidly degraded and preparation method thereof
CN116179914B (en) * 2023-02-13 2024-06-18 哈尔滨工业大学 Room-temperature high-plasticity soluble magnesium alloy and preparation method thereof

Family Cites Families (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20150005626A (en) * 2012-04-19 2015-01-14 고꾸리쯔다이가꾸호오진 구마모또 다이가꾸 Magnesium alloy and method for producing same
CN103343271B (en) * 2013-07-08 2015-07-01 中南大学 Light and pressure-proof fast-decomposed cast magnesium alloy
CN104004950B (en) * 2014-06-05 2016-06-29 宁波高新区融创新材料科技有限公司 Ease of solubility magnesium alloy materials and manufacture method thereof and application
CN107267827B (en) * 2017-05-26 2018-12-28 广西庆达汽车零部件有限公司 A kind of high-strength magnesium aluminium alloy
CN107385245B (en) * 2017-06-09 2019-06-18 西安理工大学 Based on the oil-gas mining manufacturing method of soluble alloy pressure break ball
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
CN109266927A (en) * 2018-09-11 2019-01-25 山东省科学院新材料研究所 It is a kind of can high-speed extrusion high-performance wrought magnesium alloy and preparation method thereof
CN109161769B (en) * 2018-10-30 2022-11-22 北京科技大学 Functional rapidly-soluble rare earth magnesium alloy material and preparation method thereof

Also Published As

Publication number Publication date
CN109694976A (en) 2019-04-30

Similar Documents

Publication Publication Date Title
CN109694976B (en) Low-cost soluble magnesium alloy and preparation method and application thereof
EP3650567B1 (en) High-strength and high-toughness magnesium alloy and preparation method thereof
EP3650561B1 (en) Plastic wrought magnesium alloy and preparation method thereof
CN105154734B (en) It is a kind of can high-speed extrusion wrought magnesium alloy and preparation method thereof
CN110129644B (en) Heat-resistant soluble magnesium alloy and preparation method and application thereof
CN110184518B (en) Rapidly-dissolved high-strength high-elongation magnesium alloy and preparation method thereof
CN108251721B (en) High-strength degradable aluminum alloy and preparation method and application thereof
CN110106416B (en) Ultrahigh-strength dissolvable magnesium alloy and preparation method and application thereof
CN104032195B (en) Efficiently-extrudable low-cost high-performance heat-conducting magnesium alloy and preparation method thereof
CN109988955B (en) High-elongation low-temperature rapid degradation magnesium alloy and preparation method thereof
CN109930045B (en) High-strength-toughness heat-resistant Mg-Gd alloy suitable for gravity casting and preparation method thereof
CN111876636B (en) Dissoluble aluminum alloy material, preparation method thereof and fracturing ball
CN115323232B (en) Controllable dissolved magnesium alloy wire and preparation method thereof
CN112921223A (en) Fe-containing soluble magnesium alloy and preparation method thereof
CN115852217A (en) High-strength easily-extruded aluminum alloy and section extrusion method thereof
CN110468317B (en) Magnesium alloy with excellent room temperature plasticity and preparation method thereof
CN109680194B (en) Preparation method of high-strength extruded section of Mg-Zn-Sn-Mn alloy
CN111607728A (en) Low-cost wrought magnesium alloy reinforced by light rare earth elements Ce and Sm and preparation method thereof
CN113403515A (en) Mg-Gd alloy with low Gd content and preparation and heat treatment method thereof
CN111172440B (en) Low-cost rapid-corrosion magnesium alloy and preparation method thereof
CN109371301B (en) Room-temperature high-plasticity magnesium alloy and preparation method thereof
CN113005347B (en) High-plasticity Mg-Al-Ca magnesium alloy and preparation method thereof
CN113897567A (en) Homogenization thermomechanical treatment method for rapidly refining and homogenizing cast aluminum-lithium alloy
CN114262825A (en) Aluminum alloy, and processing method and application thereof
CN103334038B (en) A kind of alkaline earth magnesium alloy plate treatment process

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant
TR01 Transfer of patent right

Effective date of registration: 20220323

Address after: 400800 No. 2 Jinsheng Road, Pingshan Industrial Park, Wansheng Economic Development Zone, Qijiang District, Chongqing

Patentee after: Chongqing Yuhua New Materials Technology Co.,Ltd.

Address before: 250014 No. 19, ASTRI Road, Lixia District, Shandong, Ji'nan

Patentee before: NEW MATERIAL INSTITUTE OF SHANDONG ACADEMY OF SCIENCES

TR01 Transfer of patent right