CN105274372A - Method for preparing aluminum-zirconium alloy - Google Patents
Method for preparing aluminum-zirconium alloy Download PDFInfo
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- CN105274372A CN105274372A CN201510888586.4A CN201510888586A CN105274372A CN 105274372 A CN105274372 A CN 105274372A CN 201510888586 A CN201510888586 A CN 201510888586A CN 105274372 A CN105274372 A CN 105274372A
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Abstract
The invention relates to a method for preparing aluminum-zirconium alloy. Kalzium metal is adopted as a composite reducing agent, high-purity zirconium dioxide is used as a raw material, cryolite, potassium fluozirconate and sodium chloride serve as covering agents, and the aluminum-zirconium alloy which is low in content of impurity elements, high in zirconium content and even in distribution of zirconium in alloy can be prepared through the raw material component control and high-temperature reducing technology. Through detection, the zirconium content of the aluminum-zirconium alloy prepared through the method can reach 4-7 wt%, Al and Zr are larger than or equal to 99 wt%, and part of zirconium in the alloy exists in the mode of a small-size Al3Zr compound; deformation processing recrystallization behaviors can be restrained, the grain size and shape are controlled, and thus the hardenability, breaking tenacity and stress corrosion resistance of the aluminum-zirconium alloy are improved. The overall preparation process is free of pollution and low in cost, the covering agents and the zirconium dioxide can be recycled, and the technology is simple and easy to implement.
Description
Technical field
The present invention relates to field of alloy preparation technology, particularly relate to a kind of preparation method of aluminium zirconium alloy.
Background technology
In the industrial production, the zirconium of trace adds and applies in ultralight aluminum base alloy, and its effect one is refinement as-cast grain, two Al forming even dispersion when being homogenizing cast ingot
3zr, suppresses deformation processing recrystallization behavior, controls grain size and shape, thus improves the hardening capacity, fracture toughness property, anti-stress corrosion performance etc. of aluminium alloy.Conventional Al-Zr alloy preparation method is mainly the method for mixing, raw material is metal sponge zirconium powder and electrolytic aluminum, carry out melting and being incubated enough time in general furnace, after adopting machinery, electromagnetism or hand mixing, be cast in mould, the aluminium zirconium hardener utilizing this method to produce exist raw materials cost high, stir after trace impurity content is high in alloy, the difficult chance aluminium of zirconium combines, the problem of component segregation, have a strong impact on its use properties.
Summary of the invention
Technical problem to be solved by this invention is: provide that a kind of foreign matter content is low, zirconium content is high and the preparation method of the aluminium zirconium alloy that zirconium is evenly distributed in the alloy.
In order to solve the problems of the technologies described above, one of the technical solution used in the present invention is: a kind of preparation method of aluminium zirconium alloy, comprising:
Kalzium metal is positioned over crucible bottom, then zirconium dioxide is mixed with sodium aluminum fluoride, potassium chlorate fluozirconate, sodium-chlor, and being covered in kalzium metal top, each composition weight proportioning is: zirconium dioxide: sodium aluminum fluoride: potassium chlorate fluozirconate: sodium-chlor: kalzium metal=20 ~ 28: 35 ~ 55: 45 ~ 60: 30 ~ 50: 80 ~ 130;
Heating crucible makes its temperature reach 960 DEG C ~ 1150 DEG C, reaction 90min ~ 120min, generates aluminium zirconium alloy liquid;
Aluminium zirconium alloy liquid is poured into die casting, makes aluminium zirconium alloy ingot.
Further, the composition weight proportioning of described kalzium metal is: aluminium: calcium=15 ~ 35: 5 ~ 9.
Further, material purity >=99.8% of aluminium and calcium.
Further, described zirconium dioxide is the powder of fineness >=500 order, purity >=99.5%.
Further, described crucible is plumbago crucible.
Another technical scheme that the present invention adopts is: a kind of preparation method of aluminium zirconium alloy, comprising:
First be aluminium by weight proportion: calcium=25: 7, the kalzium metal of material purity >=99.8% of aluminium and calcium is positioned over bottom plumbago crucible, again by purity >=99.5%, fineness >=500 object zirconium dioxide powder and sodium aluminum fluoride, potassium chlorate fluozirconate, sodium-chlor mixes, each composition weight proportioning is: zirconium dioxide: sodium aluminum fluoride: potassium chlorate fluozirconate: sodium-chlor: kalzium metal=24: 45: 53: 40: 105, then heated graphite crucible makes its temperature reach 990 DEG C, reaction 105min, generate aluminium zirconium alloy liquid, finally aluminium zirconium alloy liquid is poured into die casting, make aluminium zirconium alloy ingot.
Beneficial effect of the present invention is: employing high-purity zirconium dioxide is raw material, controlled and high temperature reduction technique by material composition, prepare impurity content low (Al+Zr>=99wt%), zirconium content high (can 4 ~ 7wt% be reached) and the aluminium zirconium hardener be evenly distributed, and zirconium in the alloy part with small size Al
3zr compound form exists, and can suppress deformation processing recrystallization behavior, controls grain size and shape, thus the hardening capacity of raising aluminium zirconium alloy, fracture toughness property and anti-stress corrosion performance.Whole preparation process is pollution-free, and cost is low, and insulating covering agent and zirconium dioxide can reuse, simple for process.
Embodiment
By describing technology contents of the present invention in detail, being realized object and effect, be explained below in conjunction with embodiment.
The design of most critical of the present invention is: employing kalzium metal is reductive agent, high-purity zirconium dioxide is raw material, sodium aluminum fluoride, potassium chlorate fluozirconate and sodium-chlor are insulating covering agent, controlled and high temperature reduction technique by material composition, prepare that impurity content is low, zirconium content is high and the aluminium zirconium hardener that zirconium is evenly distributed in the alloy.
The invention provides a kind of preparation method of aluminium zirconium alloy, comprising:
Kalzium metal is positioned over crucible bottom, then zirconium dioxide is mixed with sodium aluminum fluoride, potassium chlorate fluozirconate, sodium-chlor, and being covered in kalzium metal top, each composition weight proportioning is: zirconium dioxide: sodium aluminum fluoride: potassium chlorate fluozirconate: sodium-chlor: kalzium metal=20 ~ 28: 35 ~ 55: 45 ~ 60: 30 ~ 50: 80 ~ 130;
Heating crucible makes its temperature reach 960 DEG C ~ 1150 DEG C, reaction 90min ~ 120min, generates aluminium zirconium alloy liquid;
Aluminium zirconium alloy liquid is poured into die casting, makes aluminium zirconium alloy ingot.
Further, the composition weight proportioning of described kalzium metal is: aluminium: calcium=15 ~ 35: 5 ~ 9.
Further, material purity >=99.8% of aluminium and calcium.
Further, described zirconium dioxide is the powder of fineness >=500 order, purity >=99.5%.
Further, described crucible is plumbago crucible.
Reaction mechanism of the present invention is as follows:
Under 960-1150 DEG C of hot conditions, also there is following reduction reaction: 2Al-Ca+2ZrO on zirconium dioxide surface in the melting of reductive agent kalzium metal
2=2Al-Zr+2CaO+O
2reaction process is pollution-free, use insulating covering agent potassium chlorate fluozirconate, sodium-chlor, sodium aluminum fluoride to combine according to a certain ratio, the calciothermic reduction reactivity of boosting zirconium dioxide surface can be played under high temperature, thus prepare the aluminium zirconium alloy that impurity content is low, zirconium content is high and be evenly distributed, and zirconium is in the alloy partly with small size Al
3zr compound form exists, and can suppress deformation processing recrystallization behavior, controls grain size and shape, thus the hardening capacity of raising aluminium zirconium alloy, fracture toughness property and anti-stress corrosion performance etc.Under 960 ~ 1150 DEG C of high temperature, insulating covering agent and aluminium zirconium alloy are all in a liquid state, and because insulating covering agent density is less than aluminium zirconium alloy liquid, can directly be separated with aluminium zirconium alloy liquid and reuse, and improve raw material availability, reduce production cost.
Embodiment 1
First be aluminium by weight proportion: calcium=25: 7, the kalzium metal of material purity >=99.8% of aluminium and calcium is positioned over bottom plumbago crucible, again by purity >=99.5%, fineness >=500 object zirconium dioxide powder and sodium aluminum fluoride, potassium chlorate fluozirconate, sodium-chlor mixes, each composition weight proportioning is: zirconium dioxide: sodium aluminum fluoride: potassium chlorate fluozirconate: sodium-chlor: kalzium metal=24: 45: 53: 40: 105, then heated graphite crucible makes its temperature reach 990 DEG C, reaction 105min, generate aluminium zirconium alloy liquid, finally aluminium zirconium alloy liquid is poured into die casting, make aluminium zirconium alloy ingot.
After testing, in the aluminium zirconium alloy prepared, zirconium content is 7.0wt%, Al+Zr=99.8wt%, and zirconium is in the alloy partly with small size Al
3zr compound form even dispersion.
Embodiment 2
First be aluminium by weight proportion: calcium=7: 1, the kalzium metal of material purity >=99.8% of aluminium and calcium is positioned over bottom plumbago crucible, again by purity >=99.5%, fineness >=500 object zirconium dioxide powder and sodium aluminum fluoride, potassium chlorate fluozirconate, sodium-chlor mixes, each composition weight proportioning is: zirconium dioxide: sodium aluminum fluoride: potassium chlorate fluozirconate: sodium-chlor: kalzium metal=20: 35: 45: 30: 80, then heated graphite crucible makes its temperature reach 960 DEG C, reaction 105min, generate aluminium zirconium alloy liquid, finally aluminium zirconium alloy liquid is poured into die casting, make aluminium zirconium alloy ingot.
After testing, in the aluminium zirconium alloy prepared, zirconium content is 5.1wt%, Al+Zr=99.1wt%, and zirconium is in the alloy partly with small size Al
3zr compound form even dispersion.
Embodiment 3
First be aluminium by weight proportion: calcium=5: 3, the kalzium metal of material purity >=99.8% of aluminium and calcium is positioned over bottom plumbago crucible, again by purity >=99.5%, fineness >=500 object zirconium dioxide powder and sodium aluminum fluoride, potassium chlorate fluozirconate, sodium-chlor mixes, each composition weight proportioning is: zirconium dioxide: sodium aluminum fluoride: potassium chlorate fluozirconate: sodium-chlor: kalzium metal=28: 55: 60: 50: 130, then heated graphite crucible makes its temperature reach 1150 DEG C, reaction 105min, generate aluminium zirconium alloy liquid, finally aluminium zirconium alloy liquid is poured into die casting, make aluminium zirconium alloy ingot.
After testing, in the aluminium zirconium alloy prepared, zirconium content is 6.3wt%, Al+Zr=99.3wt%, and zirconium is in the alloy partly with small size Al
3zr compound form even dispersion.
Comparative example 1
First be aluminium by weight proportion: calcium=25: 7, the kalzium metal of material purity >=99.8% of aluminium and calcium is positioned over bottom plumbago crucible, again by purity >=99.5%, fineness >=500 object zirconium dioxide powder and sodium aluminum fluoride, potassium chlorate fluozirconate, sodium-chlor mixes, each composition weight proportioning is: zirconium dioxide: sodium aluminum fluoride: potassium chlorate fluozirconate: sodium-chlor: kalzium metal=24: 20: 20: 15: 105, then heated graphite crucible makes its temperature reach 990 DEG C, reaction 105min, generate aluminium zirconium alloy liquid, finally aluminium zirconium alloy liquid is poured into die casting, make aluminium zirconium alloy ingot.
After testing, in the aluminium zirconium alloy prepared, zirconium content is 0.6wt%, Al+Zr=79wt%.
Comparative example 2
First be aluminium by weight proportion: calcium=25: 7, the kalzium metal of material purity >=99.8% of aluminium and calcium is positioned over bottom plumbago crucible, again by purity >=99.5%, fineness >=500 object zirconium dioxide powder and sodium aluminum fluoride, potassium chlorate fluozirconate, sodium-chlor mixes, each composition weight proportioning is: zirconium dioxide: sodium aluminum fluoride: potassium chlorate fluozirconate: sodium-chlor: kalzium metal=24: 45: 53: 40: 105, then heated graphite crucible makes its temperature reach 750 DEG C, reaction 105min, generate aluminium zirconium alloy liquid, finally aluminium zirconium alloy liquid is poured into die casting, make aluminium zirconium alloy ingot.
After testing, in the aluminium zirconium alloy prepared, zirconium content is 0.4wt%, Al+Zr=48wt%.
In sum, the preparation method of aluminium zirconium alloy provided by the invention is simple, pollution-free, and cost is low, the aluminium zirconium alloy prepared can reach 4wt%-7wt%, Al+Zr>=99wt% containing zirconium amount, zirconium in the alloy part with small size Al
3zr compound form exists, and effectively can improve the hardening capacity of aluminium zirconium alloy, fracture toughness property and anti-stress corrosion performance, insulating covering agent and raw material zirconium dioxide can reuse, and raw material availability is high, and production cost is low.
The foregoing is only embodiments of the invention; not thereby the scope of the claims of the present invention is limited; every equivalents utilizing description of the present invention to do, or be directly or indirectly used in relevant technical field, be all in like manner included in scope of patent protection of the present invention.
Claims (6)
1. a preparation method for aluminium zirconium alloy, is characterized in that, comprising:
Kalzium metal is positioned over crucible bottom, then zirconium dioxide is mixed with sodium aluminum fluoride, potassium chlorate fluozirconate, sodium-chlor, and being covered in kalzium metal top, each composition weight proportioning is: zirconium dioxide: sodium aluminum fluoride: potassium chlorate fluozirconate: sodium-chlor: kalzium metal=20 ~ 28: 35 ~ 55: 45 ~ 60: 30 ~ 50: 80 ~ 130;
Heating crucible makes its temperature reach 960 DEG C ~ 1150 DEG C, reaction 90min ~ 120min, generates aluminium zirconium alloy liquid;
Aluminium zirconium alloy liquid is poured into die casting, makes aluminium zirconium alloy ingot.
2. the preparation method of aluminium zirconium alloy according to claim 1, is characterized in that: the composition weight proportioning of described kalzium metal is: aluminium: calcium=15 ~ 35: 5 ~ 9.
3. aluminium zirconium alloy Preparation Method according to claim 2, is characterized in that: material purity >=99.8% of aluminium and calcium.
4. aluminium zirconium alloy Preparation Method according to claim 1, is characterized in that: described zirconium dioxide is the powder of fineness >=500 order, purity >=99.5%.
5. aluminium zirconium alloy Preparation Method according to claim 1, is characterized in that: described crucible is plumbago crucible.
6. a preparation method for aluminium zirconium alloy, is characterized in that, comprising:
First be aluminium by weight proportion: calcium=25: 7, the kalzium metal of material purity >=99.8% of aluminium and calcium is positioned over bottom plumbago crucible, again by purity >=99.5%, fineness >=500 object zirconium dioxide powder and sodium aluminum fluoride, potassium chlorate fluozirconate, sodium-chlor mixes, each composition weight proportioning is: zirconium dioxide: sodium aluminum fluoride: potassium chlorate fluozirconate: sodium-chlor: kalzium metal=24: 45: 53: 40: 105, then heated graphite crucible makes its temperature reach 990 DEG C, reaction 105min, generate aluminium zirconium alloy liquid, finally aluminium zirconium alloy liquid is poured into die casting, make aluminium zirconium alloy ingot.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1544388A (en) * | 2003-11-20 | 2004-11-10 | 北京科技大学 | Aluminium and / or zirconium carbon system air permeable brick |
| CN101233083A (en) * | 2005-08-25 | 2008-07-30 | 赢创德固赛有限责任公司 | Stabilised aluminium zirconium mixed oxide powder |
| CN102701736A (en) * | 2012-06-21 | 2012-10-03 | 上海海事大学 | Corrosion-resistant ceramic matrix composite in TiAlZr/ZrO2 deep sea hydrothermal fluid area and preparation method thereof |
| CN104388713A (en) * | 2014-10-31 | 2015-03-04 | 三祥新材股份有限公司 | Preparation method of aluminum-zirconium alloy |
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- 2015-12-07 CN CN201510888586.4A patent/CN105274372A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1544388A (en) * | 2003-11-20 | 2004-11-10 | 北京科技大学 | Aluminium and / or zirconium carbon system air permeable brick |
| CN101233083A (en) * | 2005-08-25 | 2008-07-30 | 赢创德固赛有限责任公司 | Stabilised aluminium zirconium mixed oxide powder |
| CN102701736A (en) * | 2012-06-21 | 2012-10-03 | 上海海事大学 | Corrosion-resistant ceramic matrix composite in TiAlZr/ZrO2 deep sea hydrothermal fluid area and preparation method thereof |
| CN104388713A (en) * | 2014-10-31 | 2015-03-04 | 三祥新材股份有限公司 | Preparation method of aluminum-zirconium alloy |
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