CN115053003A - Rapidly-dissolved high-plasticity soluble magnesium alloy material and preparation method thereof - Google Patents
Rapidly-dissolved high-plasticity soluble magnesium alloy material and preparation method thereof Download PDFInfo
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- 239000000956 alloy Substances 0.000 title claims abstract description 75
- 229910000861 Mg alloy Inorganic materials 0.000 title claims abstract description 58
- 238000002360 preparation method Methods 0.000 title abstract description 11
- 238000007670 refining Methods 0.000 claims abstract description 124
- 238000003723 Smelting Methods 0.000 claims abstract description 29
- 230000032683 aging Effects 0.000 claims abstract description 27
- 238000001192 hot extrusion Methods 0.000 claims abstract description 27
- 238000005266 casting Methods 0.000 claims abstract description 26
- 239000003795 chemical substances by application Substances 0.000 claims description 45
- 239000002994 raw material Substances 0.000 claims description 44
- 229910052751 metal Inorganic materials 0.000 claims description 35
- 239000002184 metal Substances 0.000 claims description 35
- 238000000034 method Methods 0.000 claims description 33
- 238000003756 stirring Methods 0.000 claims description 27
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims description 26
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 26
- 238000001125 extrusion Methods 0.000 claims description 25
- 230000008569 process Effects 0.000 claims description 24
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 22
- 229910045601 alloy Inorganic materials 0.000 claims description 18
- 150000002739 metals Chemical class 0.000 claims description 18
- 239000002893 slag Substances 0.000 claims description 18
- 238000005507 spraying Methods 0.000 claims description 18
- 238000002844 melting Methods 0.000 claims description 16
- 230000008018 melting Effects 0.000 claims description 16
- 229910000281 calcium bentonite Inorganic materials 0.000 claims description 15
- 229910001629 magnesium chloride Inorganic materials 0.000 claims description 13
- 239000000395 magnesium oxide Substances 0.000 claims description 13
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 13
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 13
- 239000011780 sodium chloride Substances 0.000 claims description 13
- ORUIBWPALBXDOA-UHFFFAOYSA-L magnesium fluoride Chemical compound [F-].[F-].[Mg+2] ORUIBWPALBXDOA-UHFFFAOYSA-L 0.000 claims description 11
- 229910001635 magnesium fluoride Inorganic materials 0.000 claims description 11
- 239000001103 potassium chloride Substances 0.000 claims description 11
- 235000011164 potassium chloride Nutrition 0.000 claims description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 9
- 238000009749 continuous casting Methods 0.000 claims description 9
- 239000010439 graphite Substances 0.000 claims description 9
- 229910002804 graphite Inorganic materials 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 9
- 238000005303 weighing Methods 0.000 claims description 9
- 239000000498 cooling water Substances 0.000 claims description 8
- 238000010309 melting process Methods 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 5
- 230000003647 oxidation Effects 0.000 claims description 5
- 238000007254 oxidation reaction Methods 0.000 claims description 5
- 238000000265 homogenisation Methods 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 25
- 239000011777 magnesium Substances 0.000 description 22
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 11
- 229910052749 magnesium Inorganic materials 0.000 description 11
- 238000012360 testing method Methods 0.000 description 7
- 239000012535 impurity Substances 0.000 description 5
- 238000004321 preservation Methods 0.000 description 5
- 238000010276 construction Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- NROKBHXJSPEDAR-UHFFFAOYSA-M potassium fluoride Chemical compound [F-].[K+] NROKBHXJSPEDAR-UHFFFAOYSA-M 0.000 description 4
- 230000007797 corrosion Effects 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 238000004090 dissolution Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000005553 drilling Methods 0.000 description 2
- 239000002198 insoluble material Substances 0.000 description 2
- 238000003801 milling Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012856 packing Methods 0.000 description 2
- 239000011698 potassium fluoride Substances 0.000 description 2
- 235000003270 potassium fluoride Nutrition 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 238000002474 experimental method Methods 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
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C23/00—Alloys based on magnesium
- C22C23/02—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
- 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
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/06—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of magnesium or alloys based thereon
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Powder Metallurgy (AREA)
- Extrusion Of Metal (AREA)
Abstract
The invention discloses a high-plasticity soluble magnesium alloy material capable of being rapidly dissolved and a preparation method thereof, 1) preparation, 2) smelting, 3) refining, 4) casting, 5) homogenization treatment, 6) hot extrusion, and 7) aging treatment.
Description
The invention relates to the technical field of magnesium alloy materials, in particular to a rapidly-dissolved high-plasticity soluble magnesium alloy material and a preparation method thereof.
In recent years, China has found a large number of unconventional oil and gas resources which are difficult to be exploited, and the development of the unconventional oil and gas resources must rely on reservoir transformation process technologies such as hydraulic fracturing. In the hydraulic fracturing technology, different intervals need to be separated by packing tools (such as fracturing balls and bridge plugs) and then fractured and reformed layer by layer, so that oil and gas exploitation is realized. Currently, most of the common packing tools are made of insoluble materials (steel, stainless steel, etc.),Lithium ion source 
Alloy, high polymer materials and the like), and tools made of insoluble materials have the defects of difficult drilling and milling, long time consumption, difficult flowback of powder/fragments after drilling and the like in use, thereby seriously influencing the construction progress, efficiency and safety. Therefore, the plugging tool prepared from the composite material is developed internationally, although the material reduces the problems which are easy to generate in construction, the problem of easy blockage still exists because the material cannot be completely dissolved, and the production and processing of raw materials depend on import, so that the cost is high, and the plugging tool is severely restricted abroad.
The magnesium alloy has low density, high specific strength, high specific rigidity, lower electrode potential, more active chemical property and easy corrosion in most solutions. According to the characteristics, the magnesium alloy material can be used for preparing a fracturing packer tool applied to the field of oil and gas exploitation. However, the existing magnesium alloy material has various problems of low corrosion rate, low strength, poor plasticity and the like, can not meet the actual requirements of oil and gas exploitation tools, has higher production cost, and needs to provide a novel magnesium alloy material which has higher plasticity and good corrosion rate so as to meet the requirements of industrial production.
Disclosure of Invention
The invention provides a high-plasticity soluble magnesium alloy material capable of being rapidly dissolved and a preparation method thereof.
The scheme of the invention is as follows:
a fast-dissolving high-plasticity soluble magnesium alloy material comprises the following elements in percentage by mass:
the balance being Mg.
The preferable technical scheme comprises the following elements in percentage by mass:
the balance being Mg.
The preferable technical scheme comprises the following elements in percentage by mass:
the balance being Mg.
The invention also provides a preparation method of the rapidly-dissolved high-plasticity soluble magnesium alloy material, which comprises the following steps:
1) preparing, removing the oxidized surfaces of various metals, and then weighing the raw material metals according to the raw material proportion;
2) smelting, namely putting prepared raw materials into a graphite crucible, heating and smelting, stirring after melting, and controlling the temperature to be stable;
3) refining, spraying a refining agent into the melted solution, carrying out primary refining, carrying out slag skimming operation after the primary refining, controlling the pressure in the refining furnace to stir, then standing, carrying out secondary slag skimming operation, then spraying a secondary refining agent into the solution, carrying out secondary refining, skimming after the secondary refining, and uniformly stirring;
4) casting, namely introducing the magnesium alloy solution into a crystallizer to perform semi-continuous casting of the alloy;
5) homogenizing, and keeping the temperature of the obtained cast ingot at a certain temperature for a period of time;
6) hot extrusion: carrying out hot extrusion on the obtained cast ingot at a certain temperature to obtain a soluble magnesium alloy material;
7) aging treatment: and (3) carrying out aging treatment on the alloy material obtained by extrusion at a certain temperature.
As a preferable technical scheme, in the smelting process in the step 2), the melting temperature is 700-900 ℃, mixed gas of SF6+ CO2 is used for protection in the melting process, in the step 3), the refining temperature is 700-730 ℃, and mixed gas of SF6+ CO2 is used for protection in the refining process.
As a preferable technical scheme, in the casting process of the step 4), cooling water is not continuously fed into a crystallizer, and the alloy drawing casting speed is 10-30 cm/min.
As a preferable technical scheme, the step 5) is carried out with homogenization treatment, the temperature range is 380-420 ℃, and the time is 5-50 h.
As a preferable technical scheme, the step 6) hot extrusion process has the extrusion temperature of 350-370 ℃ and the extrusion ratio range of 3-30.
As a preferable technical scheme, the aging treatment in the step 7) is carried out at the temperature of 260 ℃ to 300 ℃ for 10-100 h.
Preferably, the weight of the refining agent which is put in for the first time accounts for 20-30% of the weight of the raw material metal, the weight of the refining agent which is put in for the second time accounts for 10-15% of the weight of the raw material metal, the refining agent comprises magnesium chloride, sodium chloride, potassium chloride, magnesium fluoride, magnesium oxide and calcium bentonite, and the feeding ratio of the magnesium chloride to the sodium chloride to the potassium chloride to the magnesium fluoride to the magnesium oxide to the calcium bentonite is 30-40: 4-8: 25-36: 7-10: 8-10: 5-6.
The technical scheme is adopted, the high-plasticity soluble magnesium alloy material capable of being rapidly dissolved and the preparation method thereof comprise the steps of 1) preparing, removing the oxidized surfaces of various metals, and then weighing the raw metals according to the raw material proportion; 2) smelting, namely putting prepared raw materials into a graphite crucible, heating and smelting, stirring after melting, and controlling the temperature to be stable; 3) refining, spraying a refining agent into the melted solution, carrying out primary refining, carrying out slag skimming operation after the primary refining, controlling the pressure in the refining furnace to stir, then standing, carrying out secondary slag skimming operation, then spraying a secondary refining agent into the solution, carrying out secondary refining, skimming after the secondary refining, and uniformly stirring; 4) casting, namely introducing the magnesium alloy solution into a crystallizer to perform semi-continuous casting of the alloy; 5) homogenizing, and keeping the temperature of the obtained cast ingot at a certain temperature for a period of time; 6) hot extrusion: carrying out hot extrusion on the obtained cast ingot at a certain temperature to obtain a soluble magnesium alloy material; 7) aging treatment: and carrying out aging treatment on the alloy material obtained by extrusion at a certain temperature.
The invention has the advantages that: the soluble magnesium material produced by the invention has high mechanical strength and good plasticity, is quickly dissolved in a salt solution, shows very excellent tensile strength and plastic elongation strength in a performance test, has obvious elongation after fracture, and proves that the soluble magnesium has good plasticity capability;
the fracturing tool processed by the material has enough strength, can ensure smooth underground construction, can be automatically dissolved in electrolyte solution after being used, saves subsequent flowback and milling procedures, and improves the construction efficiency.
FIG. 1 is a mechanical property test chart of the present invention;
in order to make up for the defects, the invention provides a high-plasticity soluble magnesium alloy material capable of being rapidly dissolved and a preparation method thereof so as to solve the problems in the background technology.
A fast-dissolving high-plasticity soluble magnesium alloy material comprises the following elements in percentage by mass:
the balance being Mg.
Comprises the following elements in percentage by mass:
the balance being Mg.
Comprises the following elements in percentage by mass:
the balance being Mg.
The invention also provides a preparation method of the rapidly-dissolved high-plasticity soluble magnesium alloy material, which comprises the following steps:
1) preparing, removing the oxidation surfaces of various metals, and then weighing the raw material metals according to the raw material proportion;
2) smelting, namely putting prepared raw materials into a graphite crucible, heating and smelting, stirring after melting, and controlling the temperature to be stable;
3) refining, spraying a refining agent into the melted solution, carrying out primary refining, carrying out slag skimming operation after the primary refining, controlling the pressure in the refining furnace to stir, then standing, carrying out secondary slag skimming operation, then spraying a secondary refining agent into the solution, carrying out secondary refining, skimming after the secondary refining, and uniformly stirring;
4) casting, namely introducing the magnesium alloy solution into a crystallizer to perform semi-continuous casting of the alloy;
5) homogenizing, and keeping the temperature of the obtained cast ingot at a certain temperature for a period of time;
6) hot extrusion: carrying out hot extrusion on the obtained cast ingot at a certain temperature to obtain a soluble magnesium alloy material;
7) and (3) aging treatment: and (3) carrying out aging treatment on the alloy material obtained by extrusion at a certain temperature.
In the smelting process of the step 2), the melting temperature is 700-900 ℃, the mixed gas of SF6+ CO2 is used for protection in the melting process, the refining process in the step 3) is 700-730 ℃, and the mixed gas of SF6+ CO2 is used for protection in the refining process.
In the casting process of the step 4), cooling water is continuously fed into the crystallizer, and the alloy drawing casting speed is 10-30 cm/min.
Step 5), homogenizing, wherein the temperature range is 380-420 ℃, and the time is 5-50 h.
Step 6) hot extrusion process, wherein the extrusion temperature is 350-370 ℃, and the extrusion ratio range is 3-30.
Step 7) aging treatment, wherein the temperature range is 260-300 ℃, and the time is 10-100 h.
The weight of the refining agent added for the first time accounts for 20-30% of the weight of the raw material metal, the weight of the refining agent added for the second time accounts for 10-15% of the weight of the raw material metal, the refining agent comprises magnesium chloride, sodium chloride, potassium chloride, magnesium fluoride, magnesium oxide and calcium bentonite, and the adding ratio of the refining agent to the calcium bentonite is 30-40: 4-8: 25-36: 7-10: 8-10: 5-6.
In order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the invention is further described with the specific embodiments.
Example 1:
the soluble magnesium alloy material is prepared from the following elements in percentage by mass:
the balance of Mg and inevitable impurities, and the sum of the mass percentages of the element components is 100 percent.
1) Preparing, removing the oxidized surfaces of the various required metals, and then respectively weighing the raw material metals according to the raw material proportion;
2) smelting, namely putting prepared raw materials into a graphite crucible, heating and smelting, stirring after melting, and controlling the temperature to be stable;
3) refining, spraying a refining agent into the melted solution, carrying out primary refining, carrying out slag skimming operation after the primary refining, controlling the pressure in the refining furnace to stir, then standing, carrying out secondary slag skimming operation, then spraying a secondary refining agent into the solution, carrying out secondary refining, skimming after the secondary refining, and uniformly stirring;
4) casting, namely introducing the magnesium alloy solution into a crystallizer to perform semi-continuous casting of the alloy;
5) homogenizing, and keeping the temperature of the obtained cast ingot at a certain temperature for a period of time;
6) hot extrusion: carrying out hot extrusion on the obtained cast ingot at a certain temperature to obtain a soluble magnesium alloy material;
7) aging treatment: and carrying out aging treatment on the alloy material obtained by extrusion at a certain temperature.
In the smelting process of the step 2), the melting temperature is 700 ℃, mixed gas of SF6+ CO2 is used for protection in the melting process, the refining temperature in the step 3) is 700 ℃, and mixed gas of SF6+ CO2 is used for protection in the refining process.
In the casting process of the step 4), cooling water is continuously fed into the crystallizer, and the alloy drawing casting speed is 10 cm/min.
Step 5), homogenizing, wherein the temperature range of the heat preservation is 380 ℃, and the time is 5 h.
And 6) hot extrusion, wherein the extrusion temperature is 350 ℃, and the extrusion ratio range is 3.
And 7) aging treatment, wherein the temperature range is 260 ℃, and the time is 10 h.
The weight of the refining agent which is put into the refining furnace for the first time accounts for 20 percent of the weight of the raw material metal, the weight of the refining agent which is put into the refining furnace for the second time accounts for 10 percent of the weight of the raw material metal, the refining agent comprises magnesium chloride, sodium chloride, potassium chloride, magnesium fluoride, magnesium oxide and calcium bentonite, and the feeding ratio of the magnesium chloride, the sodium chloride, the potassium chloride, the magnesium fluoride, the magnesium oxide and the calcium bentonite is 30: 4: 25: 7:8:5.
Example 2:
the soluble magnesium alloy material is prepared from the following elements in percentage by mass:
the balance of Mg and inevitable impurities, and the sum of the mass percentages of the element components is 100 percent.
1) Preparing, removing the oxidation surfaces of various metals, and then weighing the raw material metals according to the raw material proportion;
2) smelting, namely putting prepared raw materials into a graphite crucible, heating and smelting, stirring after melting, and controlling the temperature to be stable;
3) refining, spraying a refining agent into the melted solution, carrying out primary refining, carrying out slag skimming operation after the primary refining, controlling the pressure in the refining furnace to stir, then standing, carrying out secondary slag skimming operation, then spraying a secondary refining agent into the solution, carrying out secondary refining, skimming after the secondary refining, and uniformly stirring;
4) casting, namely introducing the magnesium alloy solution into a crystallizer to perform semi-continuous casting of the alloy;
5) homogenizing, and keeping the temperature of the obtained cast ingot at a certain temperature for a period of time;
6) hot extrusion: carrying out hot extrusion on the obtained cast ingot at a certain temperature to obtain a soluble magnesium alloy material;
7) aging treatment: and carrying out aging treatment on the alloy material obtained by extrusion at a certain temperature.
In the smelting process of the step 2), the melting temperature is 900 ℃, the melting process needs to be protected by mixed gas of SF6 and CO2, the refining process in the step 3) needs 730 ℃, and the refining process needs to be protected by mixed gas of SF6 and CO 2.
In the casting process of the step 4), cooling water is continuously fed into the crystallizer, and the alloy drawing casting speed is 30 cm/min.
Step 5), homogenizing, wherein the temperature range of heat preservation is 420 ℃, and the time is 50 h.
And 6) hot extrusion, wherein the extrusion temperature is 370 ℃, and the extrusion ratio range is 30.
And 7) aging treatment, wherein the temperature range is 300 ℃, and the time is 100 h.
The weight of the refining agent which is put into the refining furnace for the first time accounts for 30 percent of the weight of the raw material metal, the weight of the refining agent which is put into the refining furnace for the second time accounts for 15 percent of the weight of the raw material metal, the refining agent comprises magnesium chloride, sodium chloride, potassium chloride, magnesium fluoride, magnesium oxide and calcium bentonite, and the feeding ratio of the magnesium chloride to the sodium chloride to the potassium fluoride to the magnesium oxide to the calcium bentonite is 40: 8: 36: 10:10:6.
Example 3:
the soluble magnesium alloy material is prepared from the following elements in percentage by mass:
the balance of Mg and inevitable impurities, and the sum of the mass percentages of the element components is 100 percent.
The invention also provides a preparation method of the rapidly-dissolved high-plasticity soluble magnesium alloy material, which comprises the following steps:
1) preparing, removing the oxidized surfaces of various metals, and then weighing the raw material metals according to the raw material proportion;
2) smelting, namely putting prepared raw materials into a graphite crucible, heating and smelting, stirring after melting, and controlling the temperature to be stable;
3) refining, spraying a refining agent into the melted solution, carrying out primary refining, carrying out slag skimming operation after the primary refining, controlling the pressure in the refining furnace to stir, then standing, carrying out secondary slag skimming operation, then spraying a secondary refining agent into the solution, carrying out secondary refining, skimming after the secondary refining, and uniformly stirring;
4) casting, namely introducing the magnesium alloy solution into a crystallizer to perform semi-continuous casting of the alloy;
5) homogenizing, and keeping the temperature of the obtained cast ingot at a certain temperature for a period of time;
6) hot extrusion: carrying out hot extrusion on the obtained cast ingot at a certain temperature to obtain a soluble magnesium alloy material;
7) aging treatment: and (3) carrying out aging treatment on the alloy material obtained by extrusion at a certain temperature.
In the smelting process of the step 2), the smelting temperature is 720 ℃, mixed gas of SF6+ CO2 is used for protection in the smelting process, the refining process in the step 3) is 710 ℃, and mixed gas of SF6+ CO2 is used for protection in the refining process.
In the casting process of the step 4), cooling water is continuously fed into the crystallizer, and the alloy drawing casting speed is 15 cm/min.
Step 5) homogenizing, wherein the temperature range of heat preservation is 390, and the time is 10 h.
And 6) hot extrusion, wherein the extrusion temperature is 360 ℃, and the extrusion ratio range is 7.
And 7) aging treatment, wherein the temperature range is 280 ℃ and the time is 20 h.
The weight of the refining agent which is put into the refining furnace for the first time accounts for 22 percent of the weight of the raw material metal, the weight of the refining agent which is put into the refining furnace for the second time accounts for 12 percent of the weight of the raw material metal, the refining agent comprises magnesium chloride, sodium chloride, potassium chloride, magnesium fluoride, magnesium oxide and calcium bentonite, and the feeding ratio of the magnesium chloride to the sodium chloride to the potassium fluoride to the magnesium oxide to the calcium bentonite is 32: 5: 27: 8:8:5.
Example 4
The soluble magnesium alloy material is prepared from the following elements in percentage by mass:
the balance of Mg and inevitable impurities, and the sum of the mass percentages of the element components is 100 percent.
1) Preparing, removing the oxidation surfaces of various metals, and then weighing the raw material metals according to the raw material proportion;
2) smelting, namely putting prepared raw materials into a graphite crucible, heating and smelting, stirring after melting, and controlling the temperature to be stable;
3) refining, spraying a refining agent into the melted solution, carrying out primary refining, carrying out slag skimming operation after the primary refining, controlling the pressure in the refining furnace to stir, then standing, carrying out secondary slag skimming operation, then spraying a secondary refining agent into the solution, carrying out secondary refining, skimming after the secondary refining, and uniformly stirring;
4) casting, namely introducing the magnesium alloy solution into a crystallizer to perform semi-continuous casting of the alloy;
5) homogenizing, and keeping the temperature of the obtained cast ingot at a certain temperature for a period of time;
6) hot extrusion: carrying out hot extrusion on the obtained cast ingot at a certain temperature to obtain a soluble magnesium alloy material;
7) aging treatment: and carrying out aging treatment on the alloy material obtained by extrusion at a certain temperature.
In the smelting process of the step 2), the melting temperature is 800 ℃, the melting process needs to be protected by mixed gas of SF6 and CO2, the refining in the step 3) needs 725 ℃, and the refining process needs to be protected by mixed gas of SF6 and CO 2.
In the casting process of the step 4), cooling water is continuously fed into the crystallizer, and the alloy drawing casting speed is 25 cm/min.
And 5) homogenizing, wherein the temperature range of the heat preservation is 410 ℃, and the time is 45 h.
And 6) hot extrusion, wherein the extrusion temperature is 365 ℃, and the extrusion ratio range is 25.
And 7) aging treatment, wherein the temperature range is 290 ℃, and the time is 85 h.
The weight of the refining agent added for the first time accounts for 28% of the weight of the raw material metal, the weight of the refining agent added for the second time accounts for 14% of the weight of the raw material metal, the refining agent comprises magnesium chloride, sodium chloride, potassium chloride, magnesium fluoride, magnesium oxide and calcium bentonite, and the addition ratio of the refining agent to the raw material metal is 37: 7: 32: 9:9:6.
Example 5
The soluble magnesium alloy material is prepared from the following elements in percentage by mass:
the balance of Mg and inevitable impurities, and the sum of the mass percentages of the element components is 100 percent.
1) Preparing, removing the oxidation surfaces of various metals, and then weighing the raw material metals according to the raw material proportion;
2) smelting, namely putting prepared raw materials into a graphite crucible, heating and smelting, stirring after melting, and controlling the temperature to be stable;
3) refining, spraying a refining agent into the melted solution, carrying out primary refining, carrying out slag skimming operation after the primary refining, controlling the pressure in the refining furnace to stir, then standing, carrying out secondary slag skimming operation, then spraying a secondary refining agent into the solution, carrying out secondary refining, skimming after the secondary refining, and uniformly stirring;
4) casting, namely introducing the magnesium alloy solution into a crystallizer to perform semi-continuous casting of the alloy;
5) homogenizing, and keeping the temperature of the obtained cast ingot at a certain temperature for a period of time;
6) hot extrusion: carrying out hot extrusion on the obtained cast ingot at a certain temperature to obtain a soluble magnesium alloy material;
7) aging treatment: and (3) carrying out aging treatment on the alloy material obtained by extrusion at a certain temperature.
In the smelting process of the step 2), the melting temperature is 730 ℃, the melting process needs to be protected by mixed gas of SF6 and CO2, the refining in the step 3) is 720 ℃, and the refining process needs to be protected by mixed gas of SF6 and CO 2.
In the casting process of the step 4), cooling water is continuously fed into the crystallizer, and the alloy drawing casting speed is 20 cm/min.
And 5) homogenizing, wherein the temperature range of heat preservation is 390 ℃, and the time is 30 h.
And 6) hot extrusion, wherein the extrusion temperature is 360 ℃, and the extrusion ratio range is 20.
And 7) aging treatment, wherein the temperature range is 280 ℃, and the time is 50 h.
The weight of the refining agent which is put into the refining furnace for the first time accounts for 26 percent of the weight of the raw material metal, the weight of the refining agent which is put into the refining furnace for the second time accounts for 12 percent of the weight of the raw material metal, the refining agent comprises magnesium chloride, sodium chloride, potassium chloride, magnesium fluoride, magnesium oxide and calcium bentonite, and the feeding ratio of the magnesium chloride, the sodium chloride, the potassium chloride, the magnesium fluoride, the magnesium oxide and the calcium bentonite is 35: 6: 30: 8:9:6.
Example 6:
soluble magnesium alloy materials in example 5 are prepared into soluble magnesium test blocks with the length of 25.4mm, the width of 20.30mm, the height of 15.2mm and the weight of 11.555g, and soluble magnesium comparative blocks with the length of 25.4mm, the width of 20.30mm, the height of 15.2mm and the weight of 11.555g are respectively prepared from soluble magnesium alloy materials in the prior art; the soluble magnesium test block was tested against a soluble magnesium control block,
data of the soluble magnesium test block table 1 is as follows:
whereas the dissolution rate of the soluble magnesium comparative block of the prior artThe rate is 50mg/cm 2 The dissolution rate of the soluble magnesium alloy material is high, and the dissolution rate of the soluble magnesium alloy material is obviously improved.
A mechanical experiment was performed on the soluble magnesium alloy material of example 4 in the form of the soluble magnesium bar 7 and the soluble magnesium alloy material of example 5 in the form of the soluble magnesium bar 2, and the test times were as follows:337.866669s(ii) a Test speed:5 mm/min; the following table 2 and fig. 1 are obtained;
| sample number | Tensile strength | Specifying plastic elongation strength | Elongation after fracture | |
| Unit of | KSI | | ％ | |
| Form | ||||
| 7 | 1 | 18.9050 | 15.2951 | 44.24 |
| Form 8 | 2 | 18.9779 | 15.4748 | 45.2 |
Through the mechanical property tests in fig. 1 and table 2, it can be known that the soluble magnesium alloy material of the present invention has good various mechanical properties, and compared with the soluble magnesium in the prior art, the soluble magnesium alloy material of the present invention has significantly improved properties and significant performance progress.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are given by way of illustration of the principles of the present invention, but that various changes and modifications may be made without departing from the spirit and scope of the invention, and such changes and modifications are within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (10)
- The rapidly-dissolved high-plasticity soluble magnesium alloy material is characterized by comprising the following elements in percentage by mass:
- the rapidly dissolving, highly plastic soluble magnesium alloy material according to claim 1, comprising the following elements in mass percent:
- the rapidly dissolving, highly plastic soluble magnesium alloy material according to claim 1 or 2, comprising the following elements in mass percent:
- a method for producing a rapidly dissolving highly plastic soluble magnesium alloy material as defined in claims 1 to 3, characterized by comprising the steps of:1) preparing, removing the oxidation surfaces of various metals, and then weighing the raw material metals according to the raw material proportion;2) smelting, namely putting prepared raw materials into a graphite crucible, heating and smelting, stirring after melting, and controlling the temperature to be stable;3) refining, spraying a refining agent into the melted solution, carrying out primary refining, carrying out slag skimming operation after the primary refining, controlling the pressure in the refining furnace to stir, standing, carrying out secondary slag skimming operation, then spraying the refining agent into the solution for the second time, carrying out secondary refining, skimming after the secondary refining, and uniformly stirring;4) casting, namely introducing the magnesium alloy solution into a crystallizer to perform semi-continuous casting of the alloy;5) homogenizing, and keeping the temperature of the obtained cast ingot at a certain temperature for a period of time;6) hot extrusion: carrying out hot extrusion on the obtained cast ingot at a certain temperature to obtain a soluble magnesium alloy material;7) aging treatment: and (3) carrying out aging treatment on the alloy material obtained by extrusion at a certain temperature.
- The method for preparing the rapidly-dissolving high-plasticity soluble magnesium alloy material according to claim 4, wherein the method comprises the following steps: in the smelting process in the step 2), the melting temperature is 700-900 ℃, the SF6+ CO2 mixed gas is used for protection in the melting process, the refining in the step 3) is 700-730 ℃, and the SF6+ CO2 mixed gas is used for protection in the refining process.
- The method for preparing the rapidly-dissolving high-plasticity soluble magnesium alloy material according to claim 4, wherein the method comprises the following steps: in the casting process of the step 4), cooling water is continuously fed into the crystallizer, and the alloy drawing casting speed is 10-30 cm/min.
- The method for preparing the rapidly-dissolving high-plasticity soluble magnesium alloy material according to claim 4, wherein the method comprises the following steps: step 5) homogenizing treatment, wherein the temperature range is 380-420 ℃, and the time is 5-50 h.
- The method for producing a rapidly dissolving, highly plastic, soluble magnesium alloy material according to claim 4, wherein: step 6) hot extrusion process, wherein the extrusion temperature is 350-370 ℃, and the extrusion ratio range is 3-30.
- The method for producing a rapidly dissolving, highly plastic, soluble magnesium alloy material according to claim 4, wherein: step 7) aging treatment, wherein the temperature range is 260-300 ℃, and the time is 10-100 h.
- The method for preparing the rapidly-dissolving high-plasticity soluble magnesium alloy material according to claim 4, wherein the method comprises the following steps: the weight of the refining agent added for the first time accounts for 20-30% of the weight of the raw material metal, the weight of the refining agent added for the second time accounts for 10-15% of the weight of the raw material metal, the refining agent comprises magnesium chloride, sodium chloride, potassium chloride, magnesium fluoride, magnesium oxide and calcium bentonite, and the adding ratio of the refining agent to the calcium bentonite is 30-40: 4-8: 25-36: 7-10: 8-10: 5-6.
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| US11473179B2 (en) * | 2019-11-29 | 2022-10-18 | Fujian Meifu Technology Co., Ltd. | Method for preparing high-strength, dissolvable magnesium alloy material |
| CN112030049A (en) * | 2020-07-14 | 2020-12-04 | 中国石油天然气股份有限公司 | Controllable dissolution magnesium alloy material and preparation method thereof |
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| US20190048448A1 (en) * | 2014-04-18 | 2019-02-14 | Terves Inc. | Galvanically-Active In Situ Formed Particles for Controlled Rate Dissolving Tools |
| CN105950930A (en) * | 2016-06-24 | 2016-09-21 | 中国石油集团川庆钻探工程有限公司长庆井下技术作业公司 | Soluble extrusion magnesium alloy and preparation method thereof |
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