CN101191163A - Refining agent for magnesium alloy and preparation method thereof - Google Patents
Refining agent for magnesium alloy and preparation method thereof Download PDFInfo
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- CN101191163A CN101191163A CNA2006101440042A CN200610144004A CN101191163A CN 101191163 A CN101191163 A CN 101191163A CN A2006101440042 A CNA2006101440042 A CN A2006101440042A CN 200610144004 A CN200610144004 A CN 200610144004A CN 101191163 A CN101191163 A CN 101191163A
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Abstract
The invention relates to a magnesium alloy refining agent and a preparation method for the magnesium alloy refining agent. The compositions and content of the magnesium alloy refining agent are that: 25 to 35 weight percent of potassium chloride, 5 to 10 weight percent of calcium fluoride, 5 to 9 weight percent of barium chloride, 1 to 10 weight percent of manganese chloride, 0.2 to 0.7 weight percent of titanium sponge and 0.1 to 1.0 weight percent of boron oxide, and the residual is magnesium chloride. By adoption of the magnesium alloy refining agent of the invention, iron content in alloys can be obviously reduced. In the embodiment, wrought magnesium alloys AZ31D are prepared; analytically, contents of main metallic impurities are that: iron: less than or equal to 0.002 percent; copper: less than or equal to 0.001 s; nickel: less than or equal to 0.001 percent.
Description
Technical field
The present invention relates to a kind of refining agent and preparation method, the particularly a kind of refining agent and preparation method that can reduce iron level in the magnesium alloy.
Background technology
Magnesium alloy is a kind of metal of density minimum in the practical up to now structural metallic materials, have high specific tenacity and specific rigidity, heat-conductivity conducting, electromagnetic wave shielding, advantages such as good damping shock absorption and Environmental compatibility are good, but do not obtain large-scale application as the aluminium alloy, a wherein most important reason is exactly its poor corrosion resistance, is difficult to satisfy the requirement of Application Areas to material corrosion resistance.Studies show that metallic impurity such as iron, nickel, cobalt, copper are very harmful to the erosion resistance of magnesium alloy, it allows content that strict restriction is arranged.In above metallic impurity, iron is a kind of impurity that is difficult to most to avoid entering in the magnesium alloy.Therefore, the content of the iron in the reduction magnesium alloy has important effect for the corrosion resistance nature that improves magnesium alloy.
Summary of the invention
One of purpose of the present invention provides a kind of refining agent that can reduce iron level in the magnesium alloy.
For achieving the above object, the present invention takes following technical scheme:
A kind of refining agent that is used for magnesium alloy, its component and content are: 25-35 weight % Repone K, 5-10 weight % Calcium Fluoride (Fluorspan), 5-9 weight % bariumchloride, the Manganous chloride tetrahydrate of 1-10 weight %, 0.2 weight %-0.8 weight % titanium sponge, 0.1 weight %-1.0 weight % boron oxide, surplus is a magnesium chloride.
Another object of the present invention provides a kind of preparation method of above-mentioned refining agent of Mg alloy.
Above-mentioned purpose of the present invention reaches by the following technical programs:
A kind of preparation method who is used for the refining agent of magnesium alloy comprises the steps:
(1), earlier magnesium chloride is put into the crucible bottom, again Repone K, Calcium Fluoride (Fluorspan), bariumchloride, Manganous chloride tetrahydrate are mixed the back and add, furnace temperature rises to 550～600 ℃, furnace charge all melts the back and stirs 20～30min, and is incubated 1～3h, makes furnace temperature rise to 750～850 ℃ again, stir 20～30min, insulation 1～2h is poured in the mould then, and it is block that cooled and solidified becomes;
(2), the block refining agent of step (1) gained is broken into fritter, place ball mill to be crushed to powder about 100 orders;
(3), with titanium sponge particle and boron oxide powder and the made refining agent powder uniform mixing of step (2), divide bag hermetic package at last, refining agent of Mg alloy.
Advantage of the present invention is:
Titanium sponge, Manganous chloride tetrahydrate and three kinds of activeconstituentss of boron oxide that the magnesium alloy that the present invention makes falls in the iron refining agent all can generate compound and slag making discharge with the ferro element generation chemical reaction in the melt, significantly reduce the content of ferro element in the magnesium alloy.The iron refining agent falls in this magnesium alloy has the intensive adsorption to other oxide inclusion in the magnesium alloy fused mass, can capture inclusion and sinking slag making rapidly effectively.This magnesium alloy falls the iron refining agent and the magnesium melt has bigger density difference, and separation property is good, and can prevent effectively that flux is mingled in becomes flux in the magnesium melt and be mingled with.Adopt this to fall that the magnesium alloy subscale that the iron refining agent makes is mingled with, flux is mingled with and metals content impurity is low, has significantly improved the mechanical property and the corrosion resistance nature of alloy.Simultaneously, for the iron contamination in the melt, can improve the mechanical property and the corrosion resistance nature of magnesium alloy.This refining agent chemical stability is good, and the obnoxious flavour output is few, and add convenient in the melt, operating procedure is simple, cheap.
Embodiment
% used in following examples is wt%.Adopt the process that the iron refining agent prepares a kind of wrought magnesium alloys AZ31D of falling of the present invention in following examples.But refining agent of Mg alloy of the present invention has more than the preparation that is limited to AZ31D magnesium alloy among the embodiment, according to the characteristics of refining agent of the present invention, can also be used for the preparation of other high-quality magnesium alloy.
Embodiment 1
A kind of refining agent that is used for magnesium alloy, its component and content are: 25 weight % Repone K, 5-10 weight % Calcium Fluoride (Fluorspan), 9 weight % bariumchlorides, the Manganous chloride tetrahydrate of 10 weight %, 0.8 weight % titanium sponge, 1.0 weight % boron oxides, surplus is a magnesium chloride.
A kind of preparation method who is used for the refining agent of magnesium alloy comprises the steps:
(1), get the raw materials ready, require purity of raw materials all 〉=90%, sheet ore reduction becomes the fritter of 10～15mm, and selecting particle diameter for use is titanium sponge about 5mm, the boron oxide powder of industrial level according to the component content of above-mentioned refining agent.
(2), adopt resistance furnace and steel crucible as melting equipment, earlier magnesium chloride is put into the crucible bottom, again Repone K, Calcium Fluoride (Fluorspan), bariumchloride, Manganous chloride tetrahydrate different materials are mixed the back and add, furnace temperature rises to 550～600 ℃, furnace charge all melts the back and stirs 20～30min, and be incubated 1～3h, and make furnace temperature rise to 750～850 ℃ again, stir 20～30min, insulation 1～2h, emerge until the tranquil no bubble of bath surface, be poured into then in the iron flat groove-shaped mold, it is block that cooled and solidified becomes.
(3), will pour into a mould good block refining agent and be broken into fritter, place ball mill to be crushed to powder about 100 orders.Titanium sponge particle and boron oxide powder with above-mentioned content evenly is incorporated in the refining agent powder of making then, divides bag hermetic package at last, gets refining agent of Mg alloy 1.
Embodiment 2
A kind of refining agent that is used for magnesium alloy, its component and content are: 35 weight % Repone K, 5 weight % Calcium Fluoride (Fluorspan), 5 weight % bariumchlorides, the Manganous chloride tetrahydrate of 1 weight %, 0.2 weight % titanium sponge, 0.1 weight % boron oxide, surplus is a magnesium chloride.
A kind of preparation method who is used for the refining agent of magnesium alloy comprises the steps:
(1), get the raw materials ready, require purity of raw materials all 〉=90%, sheet ore reduction becomes the fritter of 10～15mm, and selecting particle diameter for use is titanium sponge about 5mm, the boron oxide powder of industrial level according to the component content of above-mentioned refining agent.
(2), adopt resistance furnace and steel crucible as melting equipment, earlier magnesium chloride is put into the crucible bottom, again Repone K, Calcium Fluoride (Fluorspan), bariumchloride, Manganous chloride tetrahydrate different materials are mixed the back and add, furnace temperature rises to 550～600 ℃, furnace charge all melts the back and stirs 20～30min, and be incubated 1～3h, and make furnace temperature rise to 750～850 ℃ again, stir 20～30min, insulation 1～2h, emerge until the tranquil no bubble of bath surface, be poured into then in the iron flat groove-shaped mold, it is block that cooled and solidified becomes.
(3), will pour into a mould good block refining agent and be broken into fritter, place ball mill to be crushed to powder about 100 orders.Titanium sponge particle and boron oxide powder with above-mentioned content evenly is incorporated in the refining agent powder of making then, divides bag hermetic package at last, gets refining agent of Mg alloy 2.
Embodiment 3
A kind of refining agent that is used for magnesium alloy, its component and content are: 30 weight % Repone K, 7 weight % Calcium Fluoride (Fluorspan), 7 weight % bariumchlorides, the Manganous chloride tetrahydrate of 6 weight %, 0.5 weight % titanium sponge, 0.6 weight % boron oxide, surplus is a magnesium chloride.
A kind of preparation method who is used for the refining agent of magnesium alloy comprises the steps:
(1), get the raw materials ready, require purity of raw materials all 〉=90%, sheet ore reduction becomes the fritter of 10～15mm, and selecting particle diameter for use is titanium sponge about 5mm, the boron oxide powder of industrial level according to the component content of above-mentioned refining agent.
(2), adopt resistance furnace and steel crucible as melting equipment, earlier magnesium chloride is put into the crucible bottom, again Repone K, Calcium Fluoride (Fluorspan), bariumchloride, Manganous chloride tetrahydrate different materials are mixed the back and add, furnace temperature rises to 550～600 ℃, furnace charge all melts the back and stirs 20～30min, and be incubated 1～3h, and make furnace temperature rise to 750～850 ℃ again, stir 20～30min, insulation 1～2h, emerge until the tranquil no bubble of bath surface, be poured into then in the iron flat groove-shaped mold, it is block that cooled and solidified becomes.
(3), will pour into a mould good block refining agent and be broken into fritter, place ball mill to be crushed to powder about 100 orders.Titanium sponge particle and boron oxide powder with above-mentioned content evenly is incorporated in the refining agent powder of making then, divides bag hermetic package at last, gets refining agent of Mg alloy 3.
Application Example
Component content according to magnesium alloy AZ31D is got the raw materials ready, and mainly comprises: Al 2.5～3.5%, and Zn 0.6～1.4%, and Mn 0.2～1.0%, and surplus is Mg.Mn adopts the master alloy of Al-10%Mn to add, wherein impurity F e≤0.08%; Impurity F e≤0.01% among Al, the Zn; Impurity F e≤0.004% among the Mg.
1. magnesium alloy smelting
Adopt resistance furnace and plumbago crucible as melting equipment.At first Mg, Al, Al-Mn alloy are packed in the plumbago crucible, at CO
2+ 0.5% (volume) SF
6Protective atmosphere under the fusing that begins to heat up, smelting temperature is 660～700 ℃.Metal in the crucible adds Zn after all melting, and stirs 5min, insulation 10～20min.
2. magnesium alloy refining
Furnace temperature remains on 660～700 ℃, and the limit is stirred the melt limit and added the refining agent 3 that the embodiment of the invention 3 is made.Make magnesium alloy fused mass and refining agent thorough mixing in the whipping process as far as possible.The add-on of refining agent is about 1.5～2.2% of alloy gross weight.Refining is carried out at twice, and each churning time continues 5～8min, twice midfeather time 15～20min.After refining for the second time finished, melt insulation 30～40min can pour into a mould under protective atmosphere.
3. magnesium alloy pouring
The steel mold is preheating to 200～300 ℃, and at mold cavity surface spraying Mg alloy with metal mould gravitational casting tailor-(made) coating, coating composition is: talcum powder 30%, and water glass 5%, surplus is a water.Then, again mould fully is preheated to 200～300 ℃, guarantees the coating complete drying.The good magnesium alloy fused mass of above-mentioned refining is poured in the mould after surperficial skimming, in the casting process, keeps the liquid levelling surely to fill type as far as possible, avoids washing away mould inner wall.Melt is frozen into magnesium alloy ingot through naturally cooling.
4. foreign matter content analysis
On the AZ31D magnesium alloy ingot, take a sample, impurity content is analyzed.Analytical results is: Fe≤0.002%, Cu≤0.001%, Ni≤0.001%.
Finish the preparation of AZ31D magnesium alloy to this.
Claims (2)
1. refining agent that is used for magnesium alloy, its component and content are: 25-35 weight % Repone K, 5-10 weight % Calcium Fluoride (Fluorspan), 5-9 weight % bariumchloride, the Manganous chloride tetrahydrate of 1-10 weight %, 0.2 weight %-0.8 weight % titanium sponge, 0.1 weight %-1.0 weight % boron oxide, surplus is a magnesium chloride.
2. the preparation method of the refining agent of magnesium alloy according to claim 1 comprises the steps:
(1), earlier magnesium chloride is put into the crucible bottom, again Repone K, Calcium Fluoride (Fluorspan), bariumchloride, Manganous chloride tetrahydrate are mixed the back and add, furnace temperature rises to 550～600 ℃, furnace charge all melts the back and stirs 20～30min, and is incubated 1～3h, makes furnace temperature rise to 750～850 ℃ again, stir 20～30min, insulation 1～2h is poured in the mould then, and it is block that cooled and solidified becomes;
(2), the block refining agent of step (1) gained is broken into fritter, place ball mill to be crushed to powder about 100 orders;
(3), with titanium sponge particle and boron oxide powder and the made refining agent powder uniform mixing of step (2), divide bag hermetic package at last, refining agent of Mg alloy.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2006101440042A CN101191163B (en) | 2006-11-23 | 2006-11-23 | Refining agent for magnesium alloy and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2006101440042A CN101191163B (en) | 2006-11-23 | 2006-11-23 | Refining agent for magnesium alloy and preparation method thereof |
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| CN101191163A true CN101191163A (en) | 2008-06-04 |
| CN101191163B CN101191163B (en) | 2010-09-22 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103911522A (en) * | 2012-12-31 | 2014-07-09 | 北京有色金属研究总院 | Recovery treatment method for used magnesium smelting fluxing agent or magnesium alloy smelting fluxing agent |
| CN103952611A (en) * | 2014-04-10 | 2014-07-30 | 铜陵南江鑫钢实业有限公司 | Attapulgite-containing refining agent for melting of magnesium alloy |
| CN105385873A (en) * | 2015-11-19 | 2016-03-09 | 南京云海轻金属精密制造有限公司 | Refining agent capable of being used for purifying magnesium alloy liquid in pressure casting process and production process of refining agent |
| CN110387480A (en) * | 2019-08-21 | 2019-10-29 | 闻喜县凯利达贸易有限公司 | A kind of particle refining agent used for magnesium alloy and preparation method thereof |
| CN117344351A (en) * | 2023-12-06 | 2024-01-05 | 北京道思克能源设备有限公司 | Metal magnesium and preparation method thereof |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| IL122376A (en) * | 1997-12-01 | 2001-06-14 | Dead Sea Works Ltd | Bromide salts as weightening agents for molten salts |
| CN1142301C (en) * | 2002-07-25 | 2004-03-17 | 上海交通大学 | Flux for removing iron from Mg alloy and its preparing process |
| CN1195087C (en) * | 2003-07-03 | 2005-03-30 | 上海交通大学 | Magnesium alloy boride iron illiminating flux and its production method |
| RU2283887C1 (en) * | 2005-02-24 | 2006-09-20 | Федеральное государственное унитарное предприятие "Всероссийский научно-исследовательский институт авиационных материалов" (ФГУП "ВИАМ") | Flux for melting magnesium alloys |
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2006
- 2006-11-23 CN CN2006101440042A patent/CN101191163B/en not_active Expired - Fee Related
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103911522A (en) * | 2012-12-31 | 2014-07-09 | 北京有色金属研究总院 | Recovery treatment method for used magnesium smelting fluxing agent or magnesium alloy smelting fluxing agent |
| CN103911522B (en) * | 2012-12-31 | 2016-03-30 | 北京有色金属研究总院 | Magnesium smelting fusing agent after using or magnesium alloy smelting flux recovery and treatment method |
| CN103952611A (en) * | 2014-04-10 | 2014-07-30 | 铜陵南江鑫钢实业有限公司 | Attapulgite-containing refining agent for melting of magnesium alloy |
| CN103952611B (en) * | 2014-04-10 | 2016-05-04 | 铜陵南江鑫钢实业有限公司 | A kind of magnesium alloy smelting refining agent that contains attapulgite |
| CN105385873A (en) * | 2015-11-19 | 2016-03-09 | 南京云海轻金属精密制造有限公司 | Refining agent capable of being used for purifying magnesium alloy liquid in pressure casting process and production process of refining agent |
| CN110387480A (en) * | 2019-08-21 | 2019-10-29 | 闻喜县凯利达贸易有限公司 | A kind of particle refining agent used for magnesium alloy and preparation method thereof |
| CN110387480B (en) * | 2019-08-21 | 2020-05-22 | 闻喜县凯利达贸易有限公司 | Particle refining agent for magnesium alloy and preparation method thereof |
| CN117344351A (en) * | 2023-12-06 | 2024-01-05 | 北京道思克能源设备有限公司 | Metal magnesium and preparation method thereof |
| CN117344351B (en) * | 2023-12-06 | 2024-02-13 | 北京道思克能源设备有限公司 | Metal magnesium and preparation method thereof |
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| CN101191163B (en) | 2010-09-22 |
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Effective date of registration: 20190626 Address after: 101407 No. 11 Xingke East Street, Yanqi Economic Development Zone, Huairou District, Beijing Patentee after: Research Institute of engineering and Technology Co., Ltd. Address before: 100088, 2, Xinjie street, Beijing Patentee before: General Research Institute for Nonferrous Metals |
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