US20220220590A1 - Fast-dissolved high-plasticity soluble magnesium alloy material and preparation method thereof - Google Patents
Fast-dissolved high-plasticity soluble magnesium alloy material and preparation method thereof Download PDFInfo
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- US20220220590A1 US20220220590A1 US17/565,504 US202117565504A US2022220590A1 US 20220220590 A1 US20220220590 A1 US 20220220590A1 US 202117565504 A US202117565504 A US 202117565504A US 2022220590 A1 US2022220590 A1 US 2022220590A1
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- 239000000956 alloy Substances 0.000 title claims abstract description 80
- 229910000861 Mg alloy Inorganic materials 0.000 title claims abstract description 63
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 238000007670 refining Methods 0.000 claims abstract description 121
- 238000003723 Smelting Methods 0.000 claims abstract description 29
- 230000032683 aging Effects 0.000 claims abstract description 29
- 238000001192 hot extrusion Methods 0.000 claims abstract description 29
- 239000011777 magnesium Substances 0.000 claims abstract description 28
- 238000005266 casting Methods 0.000 claims abstract description 27
- 239000002994 raw material Substances 0.000 claims description 47
- 239000003795 chemical substances by application Substances 0.000 claims description 44
- 229910052751 metal Inorganic materials 0.000 claims description 36
- 239000002184 metal Substances 0.000 claims description 36
- 238000003756 stirring Methods 0.000 claims description 30
- 238000000034 method Methods 0.000 claims description 26
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 21
- 150000002739 metals Chemical class 0.000 claims description 20
- 238000005507 spraying Methods 0.000 claims description 20
- 229910045601 alloy Inorganic materials 0.000 claims description 18
- 238000002844 melting Methods 0.000 claims description 18
- 230000008018 melting Effects 0.000 claims description 18
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims description 16
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 16
- 238000001125 extrusion Methods 0.000 claims description 16
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 10
- 238000009749 continuous casting Methods 0.000 claims description 10
- 239000010439 graphite Substances 0.000 claims description 10
- 229910002804 graphite Inorganic materials 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 10
- 238000005303 weighing Methods 0.000 claims description 10
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 8
- 239000000440 bentonite Substances 0.000 claims description 8
- 229910000278 bentonite Inorganic materials 0.000 claims description 8
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims description 8
- 239000011575 calcium Substances 0.000 claims description 8
- 229910052791 calcium Inorganic materials 0.000 claims description 8
- 239000000498 cooling water Substances 0.000 claims description 8
- 229910001629 magnesium chloride Inorganic materials 0.000 claims description 8
- ORUIBWPALBXDOA-UHFFFAOYSA-L magnesium fluoride Chemical compound [F-].[F-].[Mg+2] ORUIBWPALBXDOA-UHFFFAOYSA-L 0.000 claims description 8
- 229910001635 magnesium fluoride Inorganic materials 0.000 claims description 8
- 239000000395 magnesium oxide Substances 0.000 claims description 8
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 8
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 8
- 238000010309 melting process Methods 0.000 claims description 8
- 239000001103 potassium chloride Substances 0.000 claims description 8
- 235000011164 potassium chloride Nutrition 0.000 claims description 8
- 239000011780 sodium chloride Substances 0.000 claims description 8
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 abstract description 13
- 229910052749 magnesium Inorganic materials 0.000 abstract description 13
- 238000012360 testing method Methods 0.000 abstract description 10
- 239000000463 material Substances 0.000 abstract description 4
- 239000012266 salt solution Substances 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 34
- 230000001276 controlling effect Effects 0.000 description 16
- 238000004090 dissolution Methods 0.000 description 5
- 239000012535 impurity Substances 0.000 description 5
- 238000010276 construction Methods 0.000 description 4
- 230000007797 corrosion Effects 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 238000012856 packing Methods 0.000 description 3
- 238000005553 drilling Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000002198 insoluble material Substances 0.000 description 2
- 238000003801 milling Methods 0.000 description 2
- 229910000733 Li alloy Inorganic materials 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000001186 cumulative effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 239000012634 fragment Substances 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000001989 lithium alloy Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000004580 weight loss Effects 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C23/00—Alloys based on magnesium
- C22C23/02—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
- 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
Definitions
- the present disclosure relates to the technical field of magnesium alloy materials, and particularly relates to a fast-dissolved high-plasticity soluble magnesium alloy material and a preparation method thereof.
- the tools prepared from the insoluble materials have the defects in use that they have difficulty in drilling and milling, consume a lot of time, make powder/fragments after drilling difficult to flow back, and the like, and these defects seriously affect the construction progress, efficiency and safety. Therefore, a plugging tool prepared from composite materials has been developed internationally. Although the material reduces the problems that are likely to occur during construction, it still has the problem of easy jamming because it cannot be completely dissolved, and raw materials are produced and processed depending on imports, so that it is very high in cost, and severely restricted by foreign countries.
- a magnesium alloy has low density, high specific strength, high specific rigidity, and low electrode potential, is relatively active in chemical property, and is prone to corrosion in most solutions. According to its characteristics, magnesium alloy materials can be used to prepare fracturing and packing tools applied in the field of oil and gas exploitation. However, the existing magnesium alloy materials have a plurality of problems such as low corrosion rate or low strength or poor plasticity, cannot meet the actual needs of oil and gas exploitation tools, and are relatively high in production cost. It is necessary to provide a novel magnesium alloy material with relatively high plasticity and a good corrosion rate to meet the needs of industrial production.
- the present disclosure provides a fast-dissolved high-plasticity soluble magnesium alloy material and a preparation method thereof.
- a fast-dissolved high-plasticity soluble magnesium alloy material includes the following elements by mass percentage:
- the fast-dissolved high-plasticity soluble magnesium alloy material includes the following elements by mass percentage:
- the fast-dissolved high-plasticity soluble magnesium alloy material includes the following elements by mass percentage:
- the present disclosure further provides a preparation method for the fast-dissolved high-plasticity soluble magnesium alloy material, including the following steps:
- hot extrusion performing hot extrusion on the obtained ingot at a certain temperature to obtain the soluble magnesium alloy material
- aging treatment performing aging treatment on the extruded alloy material at a certain temperature.
- a melting temperature is 700-900° C.
- SF6+CO2 mixed gas needs to be used for protection in a melting process
- a refining temperature is 700-730° C.
- SF6+CO2 mixed gas needs to be used for protection in a refining process.
- cooling water needs to be continuously supplied to the crystallizer, and a drawing casting speed of the alloy is 10-30 cm/min.
- a heat-preserving temperature is in a range of 380-420° C. for 5-50 h.
- an extrusion temperature is 350-370° C.
- an extrusion ratio is in a range of 3-30.
- a temperature is in a range of 260-300° C. for 10-100 h.
- a weight of the refining agent charged in the first time accounts for 20-30% of a weight of the raw material metal
- a weight of the refining agent charged in the second time accounts for 10-15% that of the raw material metal
- the refining agent includes magnesium chloride, sodium chloride, potassium chloride, magnesium fluoride, magnesium oxide and calcium-based bentonite, and a feed ratio among them is 30-40:4-8:25-36:7-10:8-10:5-6.
- the present disclosure has the advantages that the soluble magnesium material produced by the present disclosure is high in mechanical strength, good in plasticity and capable of being fast dissolved in a salt solution, and exhibits very excellent tensile strength and plastic extension strength and obvious percentage elongation after fracture during performance testing, proving that the soluble magnesium of the present disclosure has good plasticity;
- the fracturing tools processed from this material have sufficient strength to ensure smooth downhole construction, and can be autonomously dissolved in an electrolyte solution after service is completed, eliminating a subsequent flowback, and milling process and improving construction efficiency.
- FIG. 1 is a mechanical property testing graph of the present disclosure.
- the present disclosure provides a fast-dissolved high-plasticity soluble magnesium alloy material and a preparation method thereof to solve the problems in the above background.
- a fast-dissolved high-plasticity soluble magnesium alloy material includes the following elements by mass percentage:
- the fast-dissolved high-plasticity soluble magnesium alloy material includes the following elements by mass percentage:
- the fast-dissolved high-plasticity soluble magnesium alloy material includes the following elements by mass percentage:
- the present disclosure further provides a preparation method for the fast-dissolved high-plasticity soluble magnesium alloy material, including the following steps:
- hot extrusion performing hot extrusion on the obtained ingot at a certain temperature to obtain the soluble magnesium alloy material
- aging treatment performing aging treatment on the extruded alloy material at a certain temperature.
- a melting temperature is 700-900° C.
- SF6+CO2 mixed gas needs to be used for protection in a melting process
- a refining temperature is 700-730° C.
- SF6+CO2 mixed gas needs to be used for protection in a refining process.
- cooling water needs to be continuously supplied to the crystallizer, and a drawing casting speed of the alloy is 10-30 cm/min.
- a heat-preserving temperature is in a range of 380-420° C. for 5-50 h.
- an extrusion temperature is 350-370° C.
- an extrusion ratio is in a range of 3-30.
- a temperature is in a range of 260-300° C. for 10-100 h.
- a weight of the refining agent charged in the first time accounts for 20-30% of a weight of the raw material metal
- a weight of the refining agent charged in the second time accounts for 10-15% that of the raw material metal
- the refining agent includes magnesium chloride, sodium chloride, potassium chloride, magnesium fluoride, magnesium oxide and calcium-based bentonite, and a feed ratio among them is 30-40:4-8:25-36:7-10:8-10:5-6.
- the soluble magnesium alloy material is prepared and includes the following elements by mass percentage:
- hot extrusion performing hot extrusion on the obtained ingot at a certain temperature to obtain the soluble magnesium alloy material
- aging treatment performing aging treatment on the extruded alloy material at a certain temperature.
- a melting temperature is 700° C.
- SF6+CO2 mixed gas needs to be used for protection in a melting process
- a refining temperature is 700° C.
- SF6+CO2 mixed gas needs to be used for protection in a refining process
- cooling water needs to be continuously supplied to the crystallizer, and a drawing casting speed of the alloy is 10 cm/min.
- a heat-preserving temperature is 380° C. for 5 h.
- an extrusion temperature is 350° C.
- an extrusion ratio is 3.
- a temperature is 260° C. for 10 h.
- a weight of the refining agent charged in the first time accounts for 20% of a weight of the raw material metal
- a weight of the refining agent charged in the second time accounts for 10% that of the raw material metal
- the refining agent includes magnesium chloride, sodium chloride, potassium chloride, magnesium fluoride, magnesium oxide and calcium-based bentonite, and a feed ratio among them is 30:4:25:7:8:5.
- the soluble magnesium alloy material is prepared and includes the following elements by mass percentage:
- hot extrusion performing hot extrusion on the obtained ingot at a certain temperature to obtain the soluble magnesium alloy material
- aging treatment performing aging treatment on the extruded alloy material at a certain temperature.
- a melting temperature is 900° C.
- SF6+CO2 mixed gas needs to be used for protection in a melting process
- a refining temperature is 730° C.
- SF6+CO2 mixed gas needs to be used for protection in a refining process.
- cooling water needs to be continuously supplied to the crystallizer, and a drawing casting speed of the alloy is 30 cm/min.
- a heat-preserving temperature is 420° C. for 50 h.
- an extrusion temperature is 370° C.
- an extrusion ratio is 30.
- a temperature is 300° C. for 100 h.
- a weight of the refining agent charged in the first time accounts for 30% of a weight of the raw material metal
- a weight of the refining agent charged in the second time accounts for 15% that of the raw material metal
- the refining agent includes magnesium chloride, sodium chloride, potassium chloride, magnesium fluoride, magnesium oxide and calcium-based bentonite, and a feed ratio among them is 40:8:36:10:10:6.
- the soluble magnesium alloy material is prepared and includes the following elements by mass percentage:
- the present disclosure further provides a preparation method for the fast-dissolved high-plasticity soluble magnesium alloy material, including the following steps:
- hot extrusion performing hot extrusion on the obtained ingot at a certain temperature to obtain the soluble magnesium alloy material
- aging treatment performing aging treatment on the extruded alloy material at a certain temperature.
- a melting temperature is 720° C.
- SF6+CO2 mixed gas needs to be used for protection in a melting process
- a refining temperature is 710° C.
- SF6+CO2 mixed gas needs to be used for protection in a refining process.
- cooling water needs to be continuously supplied to the crystallizer, and a drawing casting speed of the alloy is 15 cm/min.
- a heat-preserving temperature is 390° C. for 10 h.
- an extrusion temperature is 360° C.
- an extrusion ratio is 7.
- a temperature is 280° C. for 20 h.
- a weight of the refining agent charged in the first time accounts for 22% of a weight of the raw material metal
- a weight of the refining agent charged in the second time accounts for 12% that of the raw material metal
- the refining agent includes magnesium chloride, sodium chloride, potassium chloride, magnesium fluoride, magnesium oxide and calcium-based bentonite, and a feed ratio among them is 32:5:27:8:8:5.
- the soluble magnesium alloy material is prepared and includes the following elements by mass percentage:
- hot extrusion performing hot extrusion on the obtained ingot at a certain temperature to obtain the soluble magnesium alloy material
- aging treatment performing aging treatment on the extruded alloy material at a certain temperature.
- a melting temperature is 800° C.
- SF6+CO2 mixed gas needs to be used for protection in a melting process
- a refining temperature is 725° C.
- SF6+CO2 mixed gas needs to be used for protection in a refining process.
- cooling water needs to be continuously supplied to the crystallizer, and a drawing casting speed of the alloy is 25 cm/min.
- a heat-preserving temperature is 410° C. for 45 h.
- an extrusion temperature is 365° C.
- an extrusion ratio is 25.
- a temperature is 290° C. for 85 h.
- a weight of the refining agent charged in the first time accounts for 28% of a weight of the raw material metal
- a weight of the refining agent charged in the second time accounts for 14% that of the raw material metal
- the refining agent includes magnesium chloride, sodium chloride, potassium chloride, magnesium fluoride, magnesium oxide and calcium-based bentonite, and a feed ratio among them is 37:7:32:9:9:6.
- the soluble magnesium alloy material is prepared and includes the following elements by mass percentage:
- hot extrusion performing hot extrusion on the obtained ingot at a certain temperature to obtain the soluble magnesium alloy material
- aging treatment performing aging treatment on the extruded alloy material at a certain temperature.
- a melting temperature is 730° C.
- SF6+CO2 mixed gas needs to be used for protection in a melting process
- a refining temperature is 720° C.
- SF6+CO2 mixed gas needs to be used for protection in a refining process.
- cooling water needs to be continuously supplied to the crystallizer, and a drawing casting speed of the alloy is 20 cm/min.
- a heat-preserving temperature is 390° C. for 30 h.
- an extrusion temperature is 360° C., and an extrusion ratio is 20.
- a temperature is 280° C. for 50 h.
- a weight of the refining agent charged in the first time accounts for 26% of a weight of the raw material metal
- a weight of the refining agent charged in the second time accounts for 12% that of the raw material metal
- the refining agent includes magnesium chloride, sodium chloride, potassium chloride, magnesium fluoride, magnesium oxide and calcium-based bentonite, and a feed ratio among them is 35:6:30:8:9:6.
- the soluble magnesium alloy material in Example 5 is prepared into soluble magnesium test blocks with a length of 25.4 mm, a width of 20.30 mm, a height of 15.2 mm and a weight of 11.555 g, and a soluble magnesium alloy material in the prior art is prepared into soluble magnesium comparison blocks with a length of 25.4 mm, a width of 20.30 mm, a height of 15.2 mm and a weight of 11.555 g; and the soluble magnesium test block and the soluble magnesium comparison block are tested, and
- a dissolution rate of the soluble magnesium comparison block in the prior art is 50 mg/cm 2 /hr, and this shows that the dissolution rate of the soluble magnesium alloy material of the present application is high, and the dissolution rate of the present disclosure is significantly increased.
- the soluble magnesium alloy material of the present disclosure has various good mechanical properties, and compared with the soluble magnesium in the prior art, the present disclosure has a significant property improvement, with a significant property improvement.
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Abstract
Description
- The present disclosure relates to the technical field of magnesium alloy materials, and particularly relates to a fast-dissolved high-plasticity soluble magnesium alloy material and a preparation method thereof.
- In recent years, a large number of unconventional oil and gas resources that are difficult to exploit have been found in China, and these unconventional oil and gas resources are exploited depending on reservoir reconstruction process technologies such as hydraulic fracturing. In a hydraulic fracturing technology, between different layer sections, packing tools (such as fracturing balls and bridge plugs) need to be used to perform separation and then perform fracturing reconstruction layer by layer, so as to realize oil and gas exploitation. At present, commonly used packing tools are mostly prepared from insoluble materials (steel, lithium alloys, polymer materials, etc.). The tools prepared from the insoluble materials have the defects in use that they have difficulty in drilling and milling, consume a lot of time, make powder/fragments after drilling difficult to flow back, and the like, and these defects seriously affect the construction progress, efficiency and safety. Therefore, a plugging tool prepared from composite materials has been developed internationally. Although the material reduces the problems that are likely to occur during construction, it still has the problem of easy jamming because it cannot be completely dissolved, and raw materials are produced and processed depending on imports, so that it is very high in cost, and severely restricted by foreign countries.
- A magnesium alloy has low density, high specific strength, high specific rigidity, and low electrode potential, is relatively active in chemical property, and is prone to corrosion in most solutions. According to its characteristics, magnesium alloy materials can be used to prepare fracturing and packing tools applied in the field of oil and gas exploitation. However, the existing magnesium alloy materials have a plurality of problems such as low corrosion rate or low strength or poor plasticity, cannot meet the actual needs of oil and gas exploitation tools, and are relatively high in production cost. It is necessary to provide a novel magnesium alloy material with relatively high plasticity and a good corrosion rate to meet the needs of industrial production.
- The present disclosure provides a fast-dissolved high-plasticity soluble magnesium alloy material and a preparation method thereof.
- According to the scheme of the present disclosure:
- a fast-dissolved high-plasticity soluble magnesium alloy material includes the following elements by mass percentage:
- 9.2-11.5% of Al;
- 0.8-6% of Zn;
- 0.06-0.4% of Ni;
- 0.01-0.08% of Au;
- 0.14-0.35% of Sb;
- 0.2-1.5% of Cr;
- 0.05-0.3% of Cu;
- 2.1-3.5% of Sn;
- 0.1-0.28% of Fe;
- 0.05-0.18% of Mn; and
- the balance Mg.
- As a preferred technical solution, the fast-dissolved high-plasticity soluble magnesium alloy material includes the following elements by mass percentage:
- 9.3-9.5% of Al;
- 0.8-2.6% of Zn;
- 0.15-0.22% of Ni;
- 0.025-0.04% of Au;
- 0.25-0.28% of Sb;
- 0.8-1.2% of Cr;
- 0.15-0.25% of Cu;
- 2.4-2.8% of Sn;
- 0.15-0.23% of Fe;
- 0.1-0.15% of Mn; and
- the balance Mg.
- As a preferred technical solution, the fast-dissolved high-plasticity soluble magnesium alloy material includes the following elements by mass percentage:
- 9.4% of Al;
- 1.6% of Zn;
- 0.18% of Ni;
- 0.03% of Au;
- 0.26% of Sb;
- 1% of Cr;
- 0.2% of Cu;
- 2.6% of Sn;
- 0.18% of Fe;
- 0.11% of Mn; and
- the balance Mg.
- The present disclosure further provides a preparation method for the fast-dissolved high-plasticity soluble magnesium alloy material, including the following steps:
- 1) making preparations: removing oxidized surfaces of various metals required, and then respectively weighing the raw material metals according to ratios of raw materials;
- 2) smelting: putting the prepared raw materials into a graphite crucible, heating and smelting, stirring after melting, and controlling a temperature to be stable;
- 3) refining: spraying a refining agent into a melted solution to perform first-time refining, performing slagging-off operation after the first-time refining, stirring by controlling a pressure in a refining furnace, then standing to perform second-time slagging-off operation, then spraying the refining agent into the solution for the second time to perform second-time refining, performing slagging-off after the second-time refining, and stirring uniformly;
- 4) casting: introducing the magnesium alloy solution into a crystallizer to carry out semi-continuous casting of an alloy;
- 5) homogenizing treatment: keeping temperature of obtained ingots at a certain temperature for a period of time;
- 6) hot extrusion: performing hot extrusion on the obtained ingot at a certain temperature to obtain the soluble magnesium alloy material; and
- 7) aging treatment: performing aging treatment on the extruded alloy material at a certain temperature.
- As the preferred technical solution, in a smelting process of step 2), a melting temperature is 700-900° C., and SF6+CO2 mixed gas needs to be used for protection in a melting process, and in step 3), a refining temperature is 700-730° C., and SF6+CO2 mixed gas needs to be used for protection in a refining process.
- As the preferred technical solution, in a casting process of step 4), cooling water needs to be continuously supplied to the crystallizer, and a drawing casting speed of the alloy is 10-30 cm/min.
- As the preferred technical solution, in homogenizing treatment of step 5), a heat-preserving temperature is in a range of 380-420° C. for 5-50 h.
- As the preferred technical solution, in a hot extrusion process of step 6), an extrusion temperature is 350-370° C., and an extrusion ratio is in a range of 3-30.
- As the preferred technical solution, in aging treatment of step 7), a temperature is in a range of 260-300° C. for 10-100 h.
- As the preferred technical solution, a weight of the refining agent charged in the first time accounts for 20-30% of a weight of the raw material metal, a weight of the refining agent charged in the second time accounts for 10-15% that of the raw material metal, the refining agent includes magnesium chloride, sodium chloride, potassium chloride, magnesium fluoride, magnesium oxide and calcium-based bentonite, and a feed ratio among them is 30-40:4-8:25-36:7-10:8-10:5-6.
- By adopting the above-mentioned technical solution, according to the fast-dissolved high-plasticity soluble magnesium alloy material and the preparation method thereof, 1) making preparations: removing the oxidized surfaces of the various metals required, and then respectively weighing the raw material metals according to the ratios of the raw materials; 2) smelting: putting the prepared raw materials into the graphite crucible, heating and smelting, stirring after melting, and controlling the temperature to be stable; 3) refining: spraying the refining agent into the melted solution to perform first-time refining, performing slagging-off operation after the first-time refining, stirring by controlling the pressure in the refining furnace, then standing to perform second-time slagging-off operation, then spraying the refining agent into the solution for the second time to perform second-time refining, performing slagging-off after the second-time refining, and stirring uniformly; 4) casting: introducing the magnesium alloy solution into the crystallizer to carry out semi-continuous casting of the alloy; 5) homogenizing treatment: keeping temperature of the obtained ingots at a certain temperature for a period of time; 6) hot extrusion: performing hot extrusion on the obtained ingot at a certain temperature to obtain the soluble magnesium alloy material; and 7) aging treatment: performing aging treatment on the extruded alloy material at a certain temperature.
- The present disclosure has the advantages that the soluble magnesium material produced by the present disclosure is high in mechanical strength, good in plasticity and capable of being fast dissolved in a salt solution, and exhibits very excellent tensile strength and plastic extension strength and obvious percentage elongation after fracture during performance testing, proving that the soluble magnesium of the present disclosure has good plasticity;
- it is suitable for processing fracturing tools used in the fracturing process of oil and gas fields, and the fracturing tools processed from this material have sufficient strength to ensure smooth downhole construction, and can be autonomously dissolved in an electrolyte solution after service is completed, eliminating a subsequent flowback, and milling process and improving construction efficiency.
-
FIG. 1 is a mechanical property testing graph of the present disclosure. - In order to overcome the above defects, the present disclosure provides a fast-dissolved high-plasticity soluble magnesium alloy material and a preparation method thereof to solve the problems in the above background.
- A fast-dissolved high-plasticity soluble magnesium alloy material includes the following elements by mass percentage:
- 9.2-11.5% of Al;
- 0.8-6% of Zn;
- 0.06-0.4% of Ni;
- 0.01-0.08% of Au;
- 0.14-0.35% of Sb;
- 0.2-1.5% of Cr;
- 0.05-0.3% of Cu;
- 2.1-3.5% of Sn;
- 0.1-0.28% of Fe;
- 0.05-0.18% of Mn; and
- the balance Mg.
- The fast-dissolved high-plasticity soluble magnesium alloy material includes the following elements by mass percentage:
- 9.3-9.5% of Al;
- 0.8-2.6% of Zn;
- 0.15-0.22% of Ni;
- 0.025-0.04% of Au;
- 0.25-0.28% of Sb;
- 0.8-1.2% of Cr;
- 0.15-0.25% of Cu;
- 2.4-2.8% of Sn;
- 0.15-0.23% of Fe;
- 0.1-0.15% of Mn; and
- the balance Mg.
- The fast-dissolved high-plasticity soluble magnesium alloy material includes the following elements by mass percentage:
- 9.4% of Al;
- 1.6% of Zn;
- 0.18% of Ni;
- 0.03% of Au;
- 0.26% of Sb;
- 1% of Cr;
- 0.2% of Cu;
- 2.6% of Sn;
- 0.18% of Fe;
- 0.11% of Mn; and
- the balance Mg.
- The present disclosure further provides a preparation method for the fast-dissolved high-plasticity soluble magnesium alloy material, including the following steps:
- 1) making preparations: removing oxidized surfaces of various metals required, and then respectively weighing the raw material metals according to ratios of raw materials;
- 2) smelting: putting the prepared raw materials into a graphite crucible, heating and smelting, stirring after melting, and controlling a temperature to be stable;
- 3) refining: spraying a refining agent into a melted solution to perform first-time refining, performing slagging-off operation after the first-time refining, stirring by controlling a pressure in a refining furnace, then standing to perform second-time slagging-off operation, then spraying the refining agent into the solution for the second time to perform second-time refining, performing slagging-off after the second-time refining, and stirring uniformly;
- 4) casting: introducing the magnesium alloy solution into a crystallizer to carry out semi-continuous casting of an alloy;
- 5) homogenizing treatment: keeping temperature of obtained ingots at a certain temperature for a period of time;
- 6) hot extrusion: performing hot extrusion on the obtained ingot at a certain temperature to obtain the soluble magnesium alloy material; and
- 7) aging treatment: performing aging treatment on the extruded alloy material at a certain temperature.
- In a smelting process of step 2), a melting temperature is 700-900° C., and SF6+CO2 mixed gas needs to be used for protection in a melting process, and in step 3), a refining temperature is 700-730° C., and SF6+CO2 mixed gas needs to be used for protection in a refining process.
- In a casting process of step 4), cooling water needs to be continuously supplied to the crystallizer, and a drawing casting speed of the alloy is 10-30 cm/min.
- In homogenizing treatment of step 5), a heat-preserving temperature is in a range of 380-420° C. for 5-50 h.
- In a hot extrusion process of step 6), an extrusion temperature is 350-370° C., and an extrusion ratio is in a range of 3-30.
- In aging treatment of step 7), a temperature is in a range of 260-300° C. for 10-100 h.
- A weight of the refining agent charged in the first time accounts for 20-30% of a weight of the raw material metal, a weight of the refining agent charged in the second time accounts for 10-15% that of the raw material metal, the refining agent includes magnesium chloride, sodium chloride, potassium chloride, magnesium fluoride, magnesium oxide and calcium-based bentonite, and a feed ratio among them is 30-40:4-8:25-36:7-10:8-10:5-6.
- In order to make the technical means, creative features, purposes, and effects achieved by the present disclosure be readily understood, the present disclosure will be further described with reference to specific examples.
- The soluble magnesium alloy material is prepared and includes the following elements by mass percentage:
- 9.2% of Al;
- 0.8% of Zn;
- 0.06% of Ni;
- 0.01% of Au;
- 0.14% of Sb;
- 0.2% of Cr;
- 0.05% of Cu;
- 2.1% of Sn;
- 0.1% of Fe;
- 0.05% of Mn; and
- the balance Mg and inevitable impurities, and the mass percentage sum of the elements is 100%.
- 1) Making preparations: removing oxidized surfaces of the above-mentioned metals required, and then respectively weighing the raw material metals according to ratios of raw materials;
- 2) smelting: putting the prepared raw materials into a graphite crucible, heating and smelting, stirring after melting, and controlling a temperature to be stable;
- 3) refining: spraying a refining agent into a melted solution to perform first-time refining, performing slagging-off operation after the first-time refining, stirring by controlling a pressure in a refining furnace, then standing to perform second-time slagging-off operation, then spraying the refining agent into the solution for the second time to perform second-time refining, performing slagging-off after the second-time refining, and stirring uniformly;
- 4) casting: introducing the magnesium alloy solution into a crystallizer to carry out semi-continuous casting of an alloy;
- 5) homogenizing treatment: keeping temperature of obtained ingots at a certain temperature for a period of time;
- 6) hot extrusion: performing hot extrusion on the obtained ingot at a certain temperature to obtain the soluble magnesium alloy material; and
- 7) aging treatment: performing aging treatment on the extruded alloy material at a certain temperature.
- In a smelting process of step 2), a melting temperature is 700° C., and SF6+CO2 mixed gas needs to be used for protection in a melting process, and in step 3), a refining temperature is 700° C., and SF6+CO2 mixed gas needs to be used for protection in a refining process.
- In a casting process of step 4), cooling water needs to be continuously supplied to the crystallizer, and a drawing casting speed of the alloy is 10 cm/min.
- In homogenizing treatment of step 5), a heat-preserving temperature is 380° C. for 5 h.
- In a hot extrusion process of step 6), an extrusion temperature is 350° C., and an extrusion ratio is 3.
- In aging treatment of step 7), a temperature is 260° C. for 10 h.
- A weight of the refining agent charged in the first time accounts for 20% of a weight of the raw material metal, a weight of the refining agent charged in the second time accounts for 10% that of the raw material metal, the refining agent includes magnesium chloride, sodium chloride, potassium chloride, magnesium fluoride, magnesium oxide and calcium-based bentonite, and a feed ratio among them is 30:4:25:7:8:5.
- The soluble magnesium alloy material is prepared and includes the following elements by mass percentage:
- 11.5% of Al;
- 6% of Zn;
- 0.4% of Ni;
- 0.08% of Au;
- 0.35% of Sb;
- 1.5% of Cr;
- 0.3% of Cu;
- 3.5% of Sn;
- 0.28% of Fe;
- 0.18% of Mn; and
- the balance Mg and inevitable impurities, and the mass percentage sum of the elements is 100%.
- 1) Making preparations: removing oxidized surfaces of various metals required, and then respectively weighing the raw material metals according to ratios of raw materials;
- 2) smelting: putting the prepared raw materials into a graphite crucible, heating and smelting, stirring after melting, and controlling a temperature to be stable;
- 3) refining: spraying a refining agent into a melted solution to perform first-time refining, performing slagging-off operation after the first-time refining, stirring by controlling a pressure in a refining furnace, then standing to perform second-time slagging-off operation, then spraying the refining agent into the solution for the second time to perform second-time refining, performing slagging-off after the second-time refining, and stirring uniformly;
- 4) casting: introducing the magnesium alloy solution into a crystallizer to carry out semi-continuous casting of an alloy;
- 5) homogenizing treatment: keeping temperature of obtained ingots at a certain temperature for a period of time;
- 6) hot extrusion: performing hot extrusion on the obtained ingot at a certain temperature to obtain the soluble magnesium alloy material; and
- 7) aging treatment: performing aging treatment on the extruded alloy material at a certain temperature.
- In a smelting process of step 2), a melting temperature is 900° C., and SF6+CO2 mixed gas needs to be used for protection in a melting process, and in step 3), a refining temperature is 730° C., and SF6+CO2 mixed gas needs to be used for protection in a refining process.
- In a casting process of step 4), cooling water needs to be continuously supplied to the crystallizer, and a drawing casting speed of the alloy is 30 cm/min.
- In homogenizing treatment of step 5), a heat-preserving temperature is 420° C. for 50 h.
- In a hot extrusion process of step 6), an extrusion temperature is 370° C., and an extrusion ratio is 30.
- In aging treatment of step 7), a temperature is 300° C. for 100 h.
- A weight of the refining agent charged in the first time accounts for 30% of a weight of the raw material metal, a weight of the refining agent charged in the second time accounts for 15% that of the raw material metal, the refining agent includes magnesium chloride, sodium chloride, potassium chloride, magnesium fluoride, magnesium oxide and calcium-based bentonite, and a feed ratio among them is 40:8:36:10:10:6.
- The soluble magnesium alloy material is prepared and includes the following elements by mass percentage:
- 9.3% of Al;
- 0.8% of Zn;
- 0.15% of Ni;
- 0.025% of Au;
- 0.25% of Sb;
- 0.8% of Cr;
- 0.15% of Cu;
- 2.4% of Sn;
- 0.15% of Fe;
- 0.1% of Mn; and
- the balance Mg and inevitable impurities, and the mass percentage sum of the elements is 100%.
- The present disclosure further provides a preparation method for the fast-dissolved high-plasticity soluble magnesium alloy material, including the following steps:
- 1) making preparations: removing oxidized surfaces of various metals required, and then respectively weighing the raw material metals according to ratios of raw materials;
- 2) smelting: putting the prepared raw materials into a graphite crucible, heating and smelting, stirring after melting, and controlling a temperature to be stable;
- 3) refining: spraying a refining agent into a melted solution to perform first-time refining, performing slagging-off operation after the first-time refining, stirring by controlling a pressure in a refining furnace, then standing to perform second-time slagging-off operation, then spraying the refining agent into the solution for the second time to perform second-time refining, performing slagging-off after the second-time refining, and stirring uniformly;
- 4) casting: introducing the magnesium alloy solution into a crystallizer to carry out semi-continuous casting of an alloy;
- 5) homogenizing treatment: keeping temperature of obtained ingots at a certain temperature for a period of time;
- 6) hot extrusion: performing hot extrusion on the obtained ingot at a certain temperature to obtain the soluble magnesium alloy material; and
- 7) aging treatment: performing aging treatment on the extruded alloy material at a certain temperature.
- In a smelting process of step 2), a melting temperature is 720° C., and SF6+CO2 mixed gas needs to be used for protection in a melting process, and in step 3), a refining temperature is 710° C., and SF6+CO2 mixed gas needs to be used for protection in a refining process.
- In a casting process of step 4), cooling water needs to be continuously supplied to the crystallizer, and a drawing casting speed of the alloy is 15 cm/min.
- In homogenizing treatment of step 5), a heat-preserving temperature is 390° C. for 10 h.
- In a hot extrusion process of step 6), an extrusion temperature is 360° C., and an extrusion ratio is 7.
- In aging treatment of step 7), a temperature is 280° C. for 20 h.
- A weight of the refining agent charged in the first time accounts for 22% of a weight of the raw material metal, a weight of the refining agent charged in the second time accounts for 12% that of the raw material metal, the refining agent includes magnesium chloride, sodium chloride, potassium chloride, magnesium fluoride, magnesium oxide and calcium-based bentonite, and a feed ratio among them is 32:5:27:8:8:5.
- The soluble magnesium alloy material is prepared and includes the following elements by mass percentage:
- 9.5% of Al;
- 2.6% of Zn;
- 0.22% of Ni;
- 0.04% of Au;
- 0.28% of Sb;
- 1.2% of Cr;
- 0.25% of Cu;
- 2.8% of Sn;
- 0.23% of Fe;
- 0.15% of Mn; and
- the balance Mg and inevitable impurities, and the mass percentage sum of the elements is 100%.
- 1) Making preparations: removing oxidized surfaces of various metals required, and then respectively weighing the raw material metals according to ratios of raw materials;
- 2) smelting: putting the prepared raw materials into a graphite crucible, heating and smelting, stirring after melting, and controlling a temperature to be stable;
- 3) refining: spraying a refining agent into a melted solution to perform first-time refining, performing slagging-off operation after the first-time refining, stirring by controlling a pressure in a refining furnace, then standing to perform second-time slagging-off operation, then spraying the refining agent into the solution for the second time to perform second-time refining, performing slagging-off after the second-time refining, and stirring uniformly;
- 4) casting: introducing the magnesium alloy solution into a crystallizer to carry out semi-continuous casting of an alloy;
- 5) homogenizing treatment: keeping temperature of obtained ingots at a certain temperature for a period of time;
- 6) hot extrusion: performing hot extrusion on the obtained ingot at a certain temperature to obtain the soluble magnesium alloy material; and
- 7) aging treatment: performing aging treatment on the extruded alloy material at a certain temperature.
- In a smelting process of step 2), a melting temperature is 800° C., and SF6+CO2 mixed gas needs to be used for protection in a melting process, and in step 3), a refining temperature is 725° C., and SF6+CO2 mixed gas needs to be used for protection in a refining process.
- In a casting process of step 4), cooling water needs to be continuously supplied to the crystallizer, and a drawing casting speed of the alloy is 25 cm/min.
- In homogenizing treatment of step 5), a heat-preserving temperature is 410° C. for 45 h.
- In a hot extrusion process of step 6), an extrusion temperature is 365° C., and an extrusion ratio is 25.
- In aging treatment of step 7), a temperature is 290° C. for 85 h.
- A weight of the refining agent charged in the first time accounts for 28% of a weight of the raw material metal, a weight of the refining agent charged in the second time accounts for 14% that of the raw material metal, the refining agent includes magnesium chloride, sodium chloride, potassium chloride, magnesium fluoride, magnesium oxide and calcium-based bentonite, and a feed ratio among them is 37:7:32:9:9:6.
- The soluble magnesium alloy material is prepared and includes the following elements by mass percentage:
- 9.4% of Al;
- 1.6% of Zn;
- 0.18% of Ni;
- 0.03% of Au;
- 0.26% of Sb;
- 1% of Cr;
- 0.2% of Cu;
- 2.6% of Sn;
- 0.18% of Fe;
- 0.11% of Mn; and
- the balance Mg and inevitable impurities, and the mass percentage sum of the elements is 100%.
- 1) Making preparations: removing oxidized surfaces of various metals required, and then respectively weighing the raw material metals according to ratios of raw materials;
- 2) smelting: putting the prepared raw materials into a graphite crucible, heating and smelting, stirring after melting, and controlling a temperature to be stable;
- 3) refining: spraying a refining agent into a melted solution to perform first-time refining, performing slagging-off operation after the first-time refining, stirring by controlling a pressure in a refining furnace, then standing to perform second-time slagging-off operation, then spraying the refining agent into the solution for the second time to perform second-time refining, performing slagging-off after the second-time refining, and stirring uniformly;
- 4) casting: introducing the magnesium alloy solution into a crystallizer to carry out semi-continuous casting of an alloy;
- 5) homogenizing treatment: keeping temperature of obtained ingots at a certain temperature for a period of time;
- 6) hot extrusion: performing hot extrusion on the obtained ingot at a certain temperature to obtain the soluble magnesium alloy material; and
- 7) aging treatment: performing aging treatment on the extruded alloy material at a certain temperature.
- In a smelting process of step 2), a melting temperature is 730° C., and SF6+CO2 mixed gas needs to be used for protection in a melting process, and in step 3), a refining temperature is 720° C., and SF6+CO2 mixed gas needs to be used for protection in a refining process.
- In a casting process of step 4), cooling water needs to be continuously supplied to the crystallizer, and a drawing casting speed of the alloy is 20 cm/min.
- In homogenizing treatment of step 5), a heat-preserving temperature is 390° C. for 30 h.
- In a hot extrusion process of step 6), an extrusion temperature is 360° C., and an extrusion ratio is 20.
- In aging treatment of step 7), a temperature is 280° C. for 50 h.
- A weight of the refining agent charged in the first time accounts for 26% of a weight of the raw material metal, a weight of the refining agent charged in the second time accounts for 12% that of the raw material metal, the refining agent includes magnesium chloride, sodium chloride, potassium chloride, magnesium fluoride, magnesium oxide and calcium-based bentonite, and a feed ratio among them is 35:6:30:8:9:6.
- The soluble magnesium alloy material in Example 5 is prepared into soluble magnesium test blocks with a length of 25.4 mm, a width of 20.30 mm, a height of 15.2 mm and a weight of 11.555 g, and a soluble magnesium alloy material in the prior art is prepared into soluble magnesium comparison blocks with a length of 25.4 mm, a width of 20.30 mm, a height of 15.2 mm and a weight of 11.555 g; and the soluble magnesium test block and the soluble magnesium comparison block are tested, and
- data of the soluble magnesium test block are shown in Table 1 as follows:
-
Start End Interval Cumulative Length Width Height Weight Loss Temperature Liquid Dissolution rate time time time time (mm) (mm) (mm) (g) weight (g) (° C.) concentration (mg/cm2/hr) 25.40 20.30 15.20 11.555 10:05 11:05 1 1 25.12 20.12 15.06 10.586 0.969 93 3% KCL 40.03 11:07 12:07 1 2 24.00 19.02 13.96 8.829 1.757 93 3% KCL 74.03 12:09 13:09 1 3 22.96 17.84 12.82 7.088 1.741 93 3% KCL 82.35 13:12 14:15 1 4 21.86 16.64 11.96 5.644 1.444 93 3% KCL 77.41 14:17 15:17 1 5 20.60 15.52 10.16 4.323 1.321 93 3% KCL 80.14 Remark: dissolution rate (77-82 mg/cm2/hr); - However, a dissolution rate of the soluble magnesium comparison block in the prior art is 50 mg/cm2/hr, and this shows that the dissolution rate of the soluble magnesium alloy material of the present application is high, and the dissolution rate of the present disclosure is significantly increased.
- A mechanical test is carried out on Sample 7 of a soluble magnesium bar prepared from the soluble magnesium alloy material in Example 4 and Sample 2 of a soluble magnesium bar prepared from the soluble magnesium alloy material in Example 5, test time: 337.866669 s; a test speed: 5 mm/min; Table 2 below and
FIG. 1 are obtained; -
Regulated Percentage plastic elongation Tensile extension after Sample strength strength fracture Unit number KSI KSI % Sample 7 1 18.9050 15.2951 44.24 Sample 8 2 18.9779 15.4748 45.2 - From the mechanical property testing of
FIG. 1 and Table 2, it can be seen that the soluble magnesium alloy material of the present disclosure has various good mechanical properties, and compared with the soluble magnesium in the prior art, the present disclosure has a significant property improvement, with a significant property improvement. - The basic principles, principal features, and advantages of the present disclosure are displayed and described above. It should be understood by those skilled in the art that the present disclosure is not limited by the examples described above, merely the principles of the present disclosure are described in the above-mentioned examples and the description, and various changes and improvements may be made for the present disclosure without departing from the spirit and scope of the present disclosure, and these changes and improvements fall into a protection range claimed by the present disclosure. The protection range claimed by the present disclosure is defined by the appended claims and equivalents thereof.
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