CN102071439A - Method for directly preparing Mg-Zn-Zr alloy through electrolyzing molten salts - Google Patents
Method for directly preparing Mg-Zn-Zr alloy through electrolyzing molten salts Download PDFInfo
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Abstract
The invention provides a method for directly preparing Mg-Zn-Zr alloy through electrolyzing molten salts, which comprises the following steps that: the following ingredients are finely ground and uniformly mixed in percentage by weight: 30 percent to 45 percent of anhydrous MgCl2, 45 percent to 55 percent of KCl, 5 percent to 8 percent of KF, 5.3 percent to 15 percent of K2ZrF6, 2 percent to 4 percent of ZrO2 and 1 percent to 2 percent of anhydrous ZnCl2, and the materials are heated and melted in an electrobath; and insert metal molybdenum is used as a cathode and graphite is used as an anode, a method that the cathode is downwards sunk is adopted at the electrolysis temperature between 510 DEG C to 630 DEG C, the polar distance being 4cm, the cathode current dentistry being 3 to 12 A/cm<2> and the bath voltage being 5.7 to 8.2 V are adopted, the electrolysis for 2 to 4 hours is carried out, and Mg-Zn-Zr alloy is deposited in the molten salt electrobath near the cathode. The alloy obtained by using the method provided by the invention has uniform ingredients, the heat energy consumption is obviously reduced, the electrolysis temperature is between 510 DEG C and 630 DEG C and is lower than the melting point of magnesium and is much lower than the melting point of zirconium, the production flow process is shortened, the melting cost is reduced, and the economic benefits are very obvious.
Description
Technical field
What the present invention relates to is a kind of method of electrometallurgy.Be the method that a kind of fused salt electrolysis directly prepares the Mg-Zn-Zr alloy specifically.
Background technology
Magnesium alloy is called as " green alloy ", have that density is little, specific tenacity and specific rigidity height, thermal conductivity are good, mechanical property and advantages such as chemical property is good, recyclable utilization, make it very big application arranged, and its consumption have the trend that increases considerably in fields such as space flight, automobile, notebook computer, military affairs.Magnesium alloy by whether containing zirconium, can being divided into contains the zirconium magnesium alloy and does not contain the zirconium magnesium alloy.
The grain-size of Mg-Zn binary alloy is thick, forms micropore easily, and mechanical property is low, seldom uses industrial.Zr is the most effective grain refining element in the Mg-Zn alloy, and the velocity of diffusion that can slow down alloying element, stops grain growth, and Mg-Zn-Zr is that alloy is to use more forging and wrought magnesium alloys.Add 0.6%～0.8% Zr in the Mg-Zn alloy, its grain-size can be reduced to 0.65～6.50 μ m, the effect that has maximum crystal grain thinning and improve mechanical property.So containing the zirconium magnesium alloy has obtained increasingly extensive application.
The production method of Mg-Zn-Zr alloy adopts the method for mixing more at present, is to adopt high purity zinc, magnesium and magnesium zirconium master alloy to form mixing by a certain percentage under molten state.This method Production Flow Chart is long, complex process, and power consumption is high, the easy segregation of alloying constituent, production cost height.Will obtain the second best in quality Mg-Zn-Zr alloy at present mainly is by the vacuum smelting method preparation, and this method will strengthen the melting cost of Mg-Zn-Zr alloy, also its equipment proposed higher requirement.
What propose in the prior art is equipped with alloy to mixing legal system, for example number of patent application is in 200710046148.9 the patent " Mg-Zn-Zr wrought magnesium alloys preparation method ", disclose and a kind ofly under the protection of gas, heated with pure magnesium, after treating that magnesium melts fully, add technical pure Zn, the Mg-Zr master alloy, treat to stir after alloy melts fully, make alloying constituent even, add refining agent after the insulation and carry out refining, refining finishes and is incubated once more, casts then, and the ingot casting that casting is good carries out homogenizing to be handled, on extrusion machine, carry out viscous deformation, after the extruding extrusion ingot is placed on the thermal treatment of annealing in the heat treatment furnace; Number of patent application is 200810236147.5, name be called disclose in " a kind of Mg-Zn-Zr-Nd magnesium alloy and preparation method thereof " a kind of by adjusting Zn, Zr content and adding trace rare-earth element Nd, adopt resistance furnace or reverberatory furnace to carry out melting, directly prepare ingot casting with high strength and corrosion resistance.
Summary of the invention
The purpose of this invention is to provide the method that a kind of technology is simple, the uniform fused salt electrolysis of Mg-Zn-Zr alloying constituent that can cut down the consumption of energy, prepare directly prepares the Mg-Zn-Zr alloy.
The object of the present invention is achieved like this:
With KCl, K
2ZrF
6Under 600 ℃ temperature, carried out drying 72 hours, anhydrous MgCl
2, anhydrous ZnCl
2, KF carried out vacuum-drying 24 hours under 130 ℃ of temperature; With anhydrous MgCl
2, KCl, KF, K
2ZrF
6, ZrO
2With anhydrous ZnCl
2Be 30%-45%, 45%-55%, 5-8%, 5.3-15%, 2-4%, 1-2% by mass percentage, after porphyrize mixes, in electrolyzer, heat and dissolve; With inert metal molybdenum (Mo) is negative electrode, and graphite is anode, under electrolysis temperature 510-630 ℃, takes cathode method, and pole span is 4cm, and cathode current density is 3-12A/cm
2, bath voltage 5.7-8.2V, the electrolysis through 2-4 hour deposits the Mg-Zn-Zr alloy at fused-salt bath near negative electrode.
Theoretical foundation of the present invention is for passing through control Mg
2+, Zn
2+, Zr
4+Concentration and cathode current density, can prepare the magnesium zinc zirconium alloy of different components.And adopt low eutectic MgCl
2-KCl fused salt is an ionogen, can electrolysis under lower temperature.
The outstanding substantive distinguishing features and the significance progress of technical solution of the present invention mainly is embodied in: it is that raw material directly prepares the Mg-Zn-Zr alloy that the present invention adopts metallic compound, and alloying constituent is even; Significantly reduced the heat energy consumption, electrolysis temperature 510-630 ℃, be lower than the fusing point (650 ℃) of magnesium, well below the fusing point (1852 ℃) of zirconium; Shortened Production Flow Chart, reduced the melting cost, economic benefit is very remarkable.
Description of drawings
Fig. 1 a and Fig. 1 b are respectively the X-ray diffraction analysis (XRD) of the alloy sample of embodiment 7 and 6 preparations, and XRD analysis shows that alloy is by Mg phase, Mg
7Zn
3Phase, Zr phase composite.
Fig. 2 a-Fig. 2 d is that the scanning electron microscope (SEM) (spot scan) and the subsidiary energy spectrometer (EDS) (corresponding points) of the alloy sample of embodiment 6 preparations analyzed.Compound and simple substance zirconium by EDS analysis revealed magnesium zinc all are distributed in the crystal boundary place.
Fig. 3 a-Fig. 3 d is that the scanning electron microscope (SEM) (spot scan) and the subsidiary energy spectrometer (EDS) (corresponding points) of the alloy sample of embodiment 5 preparations analyzed.
Fig. 4 is scanning electron microscope (SEM) photo and face scanning (EPMA) photo of the alloy sample of embodiment 5 preparations.As seen face distributes, and zirconium does not have segregation phenomena in the alloy that this method obtains.
Fig. 5 is scanning electron microscope (SEM) photo of the alloy sample of preparation.From the SEM photo as can be seen, different Zr content Mg-Zn-Zr alloys as can be seen, along with the increase degree of grain refinement of zr element content strengthens.(a:Mg-31Zn * 100 stereoscan photographs; B:Mg-11Zn-0.1Zn * 100 stereoscan photographs; C:Mg-13Zn--0.2Zr * 100 stereoscan photographs; D:Mg-18Zn-1.3Zr * 100 stereoscan photographs)
Embodiment
Enumerate below the present invention done description in more detail:
Embodiment 1: with KCl, K
2ZrF
6Under 600 ℃ temperature, carried out drying 72 hours, anhydrous MgCl
2, anhydrous ZnCl
2, KF carried out vacuum-drying 24 hours under 130 ℃ of temperature; With MgCl
2+ KCl+KF+K
2ZrF
6+ ZrO
2+ ZnCl
2Be electrolyte system, the mass percent of each composition is respectively 34.2%, 51.4%, 5.7%, 5.3%, 2.3%, 1.1%, is negative electrode with inert metal molybdenum (Mo), graphite is anode, under 510 ℃ of the electrolysis temperatures, takes cathode method, pole span is 4cm, and cathode current density is 6A/cm
2, anodic current density 0.5A/cm
2, bath voltage 6.1-7.2V, the electrolysis through 2 hours deposits the Mg-Zn-Zr alloy at fused-salt bath near negative electrode, and the content of magnesium, zinc, zirconium is respectively: 32.7%, 66.1%, 1.2%.
Embodiment 2: with KCl, K
2ZrF
6Under 600 ℃ temperature, carried out drying 72 hours, anhydrous MgCl
2, anhydrous ZnCl
2, KF carried out vacuum-drying 24 hours under 130 ℃ of temperature; With MgCl
2+ KCl+KF+K
2ZrF
6+ ZrO
2+ ZnCl
2Be electrolyte system, the mass percent of each composition is respectively 34.2%, 51.4%, 5.7%, 5.3%, 2.3%, 1.1%, is negative electrode with inert metal molybdenum (Mo), graphite is anode, under 540 ℃ of the electrolysis temperatures, takes cathode method, pole span is 4cm, and cathode current density is 3A/cm
2, anodic current density 0.5A/cm
2, bath voltage 5.1-6.2V, the electrolysis through 2 hours deposits the Mg-Zn-Zr alloy at fused-salt bath near negative electrode, and the content of magnesium, zinc, zirconium is respectively: 45.9%, 53.1%, 1.0%.
Embodiment 3: with KCl, K
2ZrF
6Under 600 ℃ temperature, carried out drying 72 hours, anhydrous MgCl
2, anhydrous ZnCl
2, KF carried out vacuum-drying 24 hours under 130 ℃ of temperature; With MgCl
2+ KCl+KF+K
2ZrF
6+ ZrO
2+ ZnCl
2Be electrolyte system, the mass percent of each composition is respectively 34.2%, 51.4%, 5.7%, 5.3%, 2.3%, 1.1%, is negative electrode with inert metal molybdenum (Mo), graphite is anode, under 570 ℃ of the electrolysis temperatures, takes cathode method, pole span is 4cm, and cathode current density is 6A/cm
2, anodic current density 0.5A/cm
2, bath voltage 6.1-7.2V, the electrolysis through 2 hours deposits the Mg-Zn-Zr alloy at fused-salt bath near negative electrode, and the content of magnesium, zinc, zirconium is respectively: 82.4%, 16.7%, 0.9%.
Embodiment 4: with KCl, K
2ZrF
6Under 600 ℃ temperature, carried out drying 72 hours, anhydrous MgCl
2, anhydrous ZnCl
2, KF carried out vacuum-drying 24 hours under 130 ℃ of temperature; With MgCl
2+ KCl+KF+K
2ZrF
6+ ZrO
2+ ZnCl
2Be electrolyte system, the mass percent of each composition is respectively 34.2%, 51.4%, 5.7%, 5.3%, 2.3%, 1.1%, is negative electrode with inert metal molybdenum (Mo), graphite is anode, under 570 ℃ of the electrolysis temperatures, takes cathode method, pole span is 4cm, and cathode current density is 12A/cm
2, anodic current density 0.5A/cm
2, bath voltage 7.2-8.2V, the electrolysis through 2 hours deposits the Mg-Zn-Zr alloy at fused-salt bath near negative electrode, and the content of magnesium, zinc, zirconium is respectively: 52.2%, 47.4%, 0.4%.
Embodiment 5: with KCl, K
2ZrF
6Under 600 ℃ temperature, carried out drying 72 hours, anhydrous MgCl
2, anhydrous ZnCl
2, KF carried out vacuum-drying 24 hours under 130 ℃ of temperature; With MgCl
2+ KCl+KF+K
2ZrF
6+ ZrO
2+ ZnCl
2Be electrolyte system, the mass percent of each composition is respectively 34.2%, 51.4%, 5.7%, 5.3%, 2.3%, 1.1%, is negative electrode with inert metal molybdenum (Mo), graphite is anode, under 600 ℃ of the electrolysis temperatures, takes cathode method, pole span is 4cm, and cathode current density is 9A/cm
2, anodic current density 0.5A/cm
2, bath voltage 6.4-7.5V, the electrolysis through 2 hours deposits the Mg-Zn-Zr alloy at fused-salt bath near negative electrode, and the content of magnesium, zinc, zirconium is respectively: 88.9%, 11.0%, 0.1%.
Embodiment 6: with KCl, K
2ZrF
6Under 600 ℃ temperature, carried out drying 72 hours, anhydrous MgCl
2, anhydrous ZnCl
2, KF carried out vacuum-drying 24 hours under 130 ℃ of temperature; With MgCl
2+ KCl+KF+K
2ZrF
6+ ZrO
2+ ZnCl
2Be electrolyte system, the mass percent of each composition is respectively 34.2%, 51.4%, 5.7%, 5.3%, 2.3%, 1.1%, is negative electrode with inert metal molybdenum (Mo), graphite is anode, under 600 ℃ of the electrolysis temperatures, takes cathode method, pole span is 4cm, and cathode current density is 12A/cm
2, anodic current density 0.5A/cm
2, bath voltage 7.1-8.2V, the electrolysis through 4 hours deposits the Mg-Zn-Zr alloy at fused-salt bath near negative electrode, and the content of magnesium, zinc, zirconium is respectively: 80.3%, 18.4%, 1.3%.
Embodiment 7: with KCl, K
2ZrF
6Under 600 ℃ temperature, carried out drying 72 hours, anhydrous MgCl
2, anhydrous ZnCl
2, KF carried out vacuum-drying 24 hours under 130 ℃ of temperature; With MgCl
2+ KCl+KF+K
2ZrF
6+ ZrO
2+ ZnCl
2Be electrolyte system, the mass percent of each composition is respectively 34.2%, 51.4%, 5.7%, 5.3%, 2.3%, 1.1%, is negative electrode with inert metal molybdenum (Mo), graphite is anode, under 630 ℃ of the electrolysis temperatures, takes cathode method, pole span is 4cm, and cathode current density is 6A/cm
2, anodic current density 0.5A/cm
2, bath voltage 5.3-6.6V, the electrolysis through 2 hours deposits the Mg-Zn-Zr alloy at fused-salt bath near negative electrode, and the content of magnesium, zinc, zirconium is respectively: 75.9%, 23.9%, 0.2%.
Claims (8)
1. a fused salt electrolysis directly prepares the method for Mg-Zn-Zr alloy, it is characterized in that: with KCl, K
2ZrF
6Under 600 ℃ temperature, carried out drying 72 hours, anhydrous MgCl
2, anhydrous ZnCl
2, KF carried out vacuum-drying 24 hours under 130 ℃ of temperature; With anhydrous MgCl
2, KCl, KF, K
2ZrF
6, ZrO
2With anhydrous ZnCl
2Be 30%-45%, 45%-55%, 5-8%, 5.3-15%, 2-4%, 1-2% by mass percentage, after porphyrize mixes, in electrolyzer, heat and dissolve; With the inert metal molybdenum is negative electrode, and graphite is anode, under electrolysis temperature 510-630 ℃, takes cathode method, and pole span is 4cm, and cathode current density is 3-12A/cm
2, bath voltage 5.7-8.2V, the electrolysis through 2-4 hour deposits the Mg-Zn-Zr alloy at fused-salt bath near negative electrode.
2. fused salt electrolysis according to claim 1 directly prepares the method for Mg-Zn-Zr alloy, it is characterized in that: MgCl
2, KCl, KF, K
2ZrF
6, ZrO
2With anhydrous ZnCl
2Mass percent be respectively 34.2%, 51.4%, 5.7%, 5.3%, 2.3%, 1.1%, 510 ℃ of electrolysis temperatures, cathode current density is 6A/cm
2, anodic current density 0.5A/cm
2, bath voltage 6.1-7.2V, the electrolysis through 2 hours deposits the Mg-Zn-Zr alloy at fused-salt bath near negative electrode, and the content of magnesium, zinc, zirconium is respectively: 32.7%, 66.1%, 1.2%.
3. fused salt electrolysis according to claim 1 directly prepares the method for Mg-Zn-Zr alloy, it is characterized in that: MgCl
2, KCl, KF, K
2ZrF
6, ZrO
2With anhydrous ZnCl
2Mass percent be respectively 34.2%, 51.4%, 5.7%, 5.3%, 2.3%, 1.1%, 540 ℃ of electrolysis temperatures, cathode current density is 3A/cm
2, anodic current density 0.5A/cm
2, bath voltage 5.1-6.2V, the electrolysis through 2 hours deposits the Mg-Zn-Zr alloy at fused-salt bath near negative electrode, and the content of magnesium, zinc, zirconium is respectively: 45.9%, 53.1%, 1.0%.
4. fused salt electrolysis according to claim 1 directly prepares the method for Mg-Zn-Zr alloy, it is characterized in that: MgCl
2, KCl, KF, K
2ZrF
6, ZrO
2With anhydrous ZnCl
2Mass percent be respectively 34.2%, 51.4%, 5.7%, 5.3%, 2.3%, 1.1%, 570 ℃ of electrolysis temperatures take cathode method, cathode current density is 6A/cm
2, anodic current density 0.5A/cm
2, bath voltage 6.1-7.2V, the electrolysis through 2 hours deposits the Mg-Zn-Zr alloy at fused-salt bath near negative electrode, and the content of magnesium, zinc, zirconium is respectively: 82.4%, 16.7%, 0.9%.
5. fused salt electrolysis according to claim 1 directly prepares the method for Mg-Zn-Zr alloy, it is characterized in that: MgCl
2, KCl, KF, K
2ZrF
6, ZrO
2With anhydrous ZnCl
2Mass percent be respectively 34.2%, 51.4%, 5.7%, 5.3%, 2.3%, 1.1%, 570 ℃ of electrolysis temperatures, cathode current density is 12A/cm
2, anodic current density 0.5A/cm
2, bath voltage 7.2-8.2V, the electrolysis through 2 hours deposits the Mg-Zn-Zr alloy at fused-salt bath near negative electrode, and the content of magnesium, zinc, zirconium is respectively: 52.2%, 47.4%, 0.4%.
6. fused salt electrolysis according to claim 1 directly prepares the method for Mg-Zn-Zr alloy, it is characterized in that: MgCl
2, KCl, KF, K
2ZrF
6, ZrO
2With anhydrous ZnCl
2Mass percent be respectively 34.2%, 51.4%, 5.7%, 5.3%, 2.3%, 1.1%, 600 ℃ of electrolysis temperatures, cathode current density is 9A/cm
2, anodic current density 0.5A/cm
2, bath voltage 6.4-7.5V, the electrolysis through 2 hours deposits the Mg-Zn-Zr alloy at fused-salt bath near negative electrode, and the content of magnesium, zinc, zirconium is respectively: 88.9%, 11.0%, 0.1%.
7. fused salt electrolysis according to claim 1 directly prepares the method for Mg-Zn-Zr alloy, it is characterized in that: MgCl
2, KCl, KF, K
2ZrF
6, ZrO
2With anhydrous ZnCl
2Mass percent be respectively 34.2%, 51.4%, 5.7%, 5.3%, 2.3%, 1.1%, 600 ℃ of electrolysis temperatures, cathode current density is 12A/cm
2, anodic current density 0.5A/cm
2, bath voltage 7.1-8.2V, the electrolysis through 4 hours deposits the Mg-Zn-Zr alloy at fused-salt bath near negative electrode, and the content of magnesium, zinc, zirconium is respectively: 80.3%, 18.4%, 1.3%.
8. fused salt electrolysis according to claim 1 directly prepares the method for Mg-Zn-Zr alloy, it is characterized in that: MgCl
2, KCl, KF, K
2ZrF
6, ZrO
2With anhydrous ZnCl
2Mass percent be respectively 34.2%, 51.4%, 5.7%, 5.3%, 2.3%, 1.1%, 630 ℃ of electrolysis temperatures, cathode current density is 6A/cm
2, anodic current density 0.5A/cm
2, bath voltage 5.3-6.6V, the electrolysis through 2 hours deposits the Mg-Zn-Zr alloy at fused-salt bath near negative electrode, and the content of magnesium, zinc, zirconium is respectively: 75.9%, 23.9%, 0.2%.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103320819A (en) * | 2013-07-03 | 2013-09-25 | 哈尔滨工程大学 | Method for preparing alloy with high zinc content through direct electrolysis |
| WO2015131344A1 (en) * | 2014-03-05 | 2015-09-11 | 中国科学院青海盐湖研究所 | Method for preparing magnesium-zinc intermediate alloy by fused salt electrolysis process |
| CN110846687A (en) * | 2019-11-22 | 2020-02-28 | 龙南龙钇重稀土科技股份有限公司 | Mg-Zn-Zr intermediate alloy and preparation method thereof |
| CN113005481A (en) * | 2021-01-29 | 2021-06-22 | 河南大学 | Method for preparing biomedical zinc-zirconium or magnesium-zinc-zirconium alloy through electro-deoxidation |
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| US4533442A (en) * | 1984-07-31 | 1985-08-06 | Amax Inc. | Lithium metal/alloy recovery from multi-component molten salt |
| CN101358359A (en) * | 2008-08-27 | 2009-02-04 | 哈尔滨工程大学 | Method for directly preparing Mg-Zr alloy by MgCl2, K2ZrF6 and ZrO2 electrolysis |
| CN101440508A (en) * | 2008-12-12 | 2009-05-27 | 北京科技大学 | Preparation of reactive metal based alloy |
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2011
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|---|---|---|---|---|
| US4533442A (en) * | 1984-07-31 | 1985-08-06 | Amax Inc. | Lithium metal/alloy recovery from multi-component molten salt |
| CN101358359A (en) * | 2008-08-27 | 2009-02-04 | 哈尔滨工程大学 | Method for directly preparing Mg-Zr alloy by MgCl2, K2ZrF6 and ZrO2 electrolysis |
| CN101440508A (en) * | 2008-12-12 | 2009-05-27 | 北京科技大学 | Preparation of reactive metal based alloy |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103320819A (en) * | 2013-07-03 | 2013-09-25 | 哈尔滨工程大学 | Method for preparing alloy with high zinc content through direct electrolysis |
| WO2015131344A1 (en) * | 2014-03-05 | 2015-09-11 | 中国科学院青海盐湖研究所 | Method for preparing magnesium-zinc intermediate alloy by fused salt electrolysis process |
| CN110846687A (en) * | 2019-11-22 | 2020-02-28 | 龙南龙钇重稀土科技股份有限公司 | Mg-Zn-Zr intermediate alloy and preparation method thereof |
| WO2021098116A1 (en) * | 2019-11-22 | 2021-05-27 | 龙南龙钇重稀土科技股份有限公司 | Mg-zn-zr intermediate alloy and preparation method therefor |
| CN113005481A (en) * | 2021-01-29 | 2021-06-22 | 河南大学 | Method for preparing biomedical zinc-zirconium or magnesium-zinc-zirconium alloy through electro-deoxidation |
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Application publication date: 20110525 |