CN102080164A - Method for preparing Mg-Li alloy by vacuum synchronous thermal reduction - Google Patents
Method for preparing Mg-Li alloy by vacuum synchronous thermal reduction Download PDFInfo
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Abstract
The invention relates to a method for preparing an Mg-Li alloy by vacuum synchronous thermal reduction, belonging to the novel technical field of preparing magnesium alloy materials. The process course comprises the following steps of: preparing reactants according to stoichiometry of reduction reaction; pulverizing solid reactants and uniformly mixing; pressing the reactant powder into blocks and placing the blocks into a reduction tank, and carrying out thermal reduction reaction at the vacuum degree of 1-20Pa and the temperature of 950-1,500 DEG C; collecting alloy steam generated by reaction; and condensing the alloy steam to obtain an Mg-Li alloy in a condensed state. In the invention, the oxides of metals Mg and Li or a precursor of the oxides are utilized as raw materials, the synchronous reduction of the metals Mg and Li is realized through vacuum thermal reduction to prepare the Mg-Li alloy directly. The alloy preparation process has short route, wide sources of the raw materials, high material utilization rate, favorable economy and manufacturability, high efficiency and energy saving.
Description
Technical field
The present invention relates to the method that the synchronous thermal reduction of a kind of vacuum prepares the Mg-Li alloy, belong to magnesium alloy materials new preparation technology field.
Background technology
The density of magnesium is 1.74g/cm
3, the density of lithium is 0.53g/cm
3, exist marvellous structural transformation relation between MAGNESIUM METAL and the metallic lithium, when the content of elemental lithium was lower than 5.7%wt, the lithium solid solution was in magnesium, and alloy is made up of the αGu Rongti of hexagonal close packed lattice; When the content of elemental lithium is between 5.7%-11.5%wt, the softer β phase with body centered structure structure of character appears in the tissue, and the β sosoloid that group of alloys is woven with the αGu Rongti of hexagonal close packed lattice and body centered structure mixes to be formed; When lithium content was higher than 11.5%wt, alloy was made up of single β sosoloid with body centered structure.
The density of Mg-Li alloy is at 1.35-1.65g/cm
3Between, be the lightest present structural metallic materials, be also referred to as the ultralight magnesium alloy, it has low density, high specific strength, advantageous feature such as good deformation property have broad application prospects in fields such as aerospace and weapon industries.
" to the method for mixing " adopted in the preparation of traditional Mg-Li alloy more, to the method for mixing be with molten magnesium and molten lithium element to mixing, form the method for Mg-Li alloy after the condensation.When employing is equipped with the Mg-Li alloy to mixing legal system, magnesium and lithium must add with the form of pure metal, because the chemically reactive height of magnesium and lithium, in the alloy melting process easily with reactions such as airborne oxygen, nitrogen, hydrogen, therefore adopt to be equipped with the Mg-Li alloy to mixing legal system, Production Flow Chart is long, the material scaling loss is serious in the preparation process, and is oxidized easily at fusion process interalloy element, the foreign matter content height, the utilization ratio of material is not high, and is less economical.
Vacuum-thermal reduction method energy sources is extensive, material use efficiency is high, productivity is high, low cost of manufacture, be easy to realize to produce in enormous quantities.Vacuum-thermal reduction at present has been applied in the suitability for industrialized production of volatile metals such as MAGNESIUM METAL, metallic lithium, and the production that still vacuum-thermal reduction is applied to the Mg-Li alloy yet there are no report.
Summary of the invention
The objective of the invention is: overcome the deficiency of existing Mg-Li alloy preparation method, a kind of novel industrialized Mg-Li alloy vacuum-thermal reduction preparation method that can reduce production costs, be easy to realize is provided.
The synchronous thermal reduction of vacuum provided by the present invention prepares the method for magnesium lithium alloy, it is characterized in that, the component of prepared Mg-Li alloy and mass percent are for containing Li:1-50%wt; All the other are Mg and unavoidable impurities.
Technical scheme of the present invention is:
(1) get the raw materials ready: raw material is made up of oxide compound or its precursor, reductive agent and the auxiliary agent of MAGNESIUM METAL to be restored and metallic lithium, and the consumption of reductive agent is 1-5 times according to the theoretical requirement of thermal reduction chemical equation calculating; The consumption of Calcium Fluoride (Fluorspan) is the 2-5%wt of nonmetallic ingredient consumption in the raw material;
(2) with reaction mass powder process and mix, briquetting;
(3) according to calculating consumption with pack into reduction jar of reaction mass, at vacuum tightness 1-20Pa, temperature 950-1500 ℃ of reduction 1-10 hour down;
(4) collect the alloy steam and the condensation of reacting generation and obtain condensed state Mg-Li alloy.
Simultaneously, can make micro mist and make reduction reaction more thorough by reducing raw material; In the reduction process, also can be by measures such as stirring reaction material or rotation reduction jars, the forced disturbance reaction mass promotes reaction to carry out.
Wherein: can prepare the various Mg-Li alloys that contain lithium amount 1-50%wt by the mass ratio of magnesium elements and elemental lithium in the adjustment starting material; Magnesium oxide in the starting material and Lithium Oxide 98min can partly or entirely substitute with the magnesium ore deposit that at high temperature produces magnesium oxide and Lithium Oxide 98min, lithium ore deposit or its compound; Reductive agent can be alloys such as ferrosilicon, copper silicon, sial, also can be aluminium or carbon simple substance.
Compared with prior art, advantage of the present invention is: utilize directly preparation Mg-Li alloy from the oxide compound of MAGNESIUM METAL and metallic lithium or its precursor of vacuum-thermal reduction, realized the synchronous thermal reduction of metal M g and metal Li and prepared the Mg-Li alloy of different components.In the preparation process of alloy, starting material no longer are highly purified metal M g and metal Li, have avoided the scaling loss of Mg and Li element secondary cast, improved the utilization ratio of metal M g and metal Li, shortened preparation technology's flow process of alloy, material source is extensive, the material use efficiency height, Technological Economy is good; Can realize the high-level efficiency of the Mg-Li alloy of heterogeneity, production low-costly and in high volume.
Embodiment
Further specify the specific embodiment of the present invention below in conjunction with embodiment.
Embodiment 1
(1) ready reaction material, reaction mass is by MgO, Li
2Ferrosilicon and the CaF of O, CaO, Si content 75wt%
2Form, the batching mass ratio is: MgO: Li
2O: CaO: ferrosilicon: CaF
2=65: 5: 112: 50: 8;
(2) reaction mass is crushed to particle diameter less than 0.10mm, mixes and briquetting;
(3) reaction mass is packed into vacuum reducing jar, at vacuum tightness 1-20Pa, 1200 ± 50 ℃ of temperature, following reduction 3 hours;
(4) collect the alloy steam that reaction generates, and be condensed into condensed state Mg-Li alloy.Its chemical ingredients is for containing Li:5%wt, and the total amount of Mg and Li is greater than 99%wt.
Embodiment 2
(1) ready reaction material, reaction mass is by the calcined magnesium ore deposit of MgO content 90%, Li
2The ferrosilicon of the calcining lithium ore deposit of O content 80%, CaO, Si content 75wt% and fluorite are formed, and the batching mass ratio is: the calcined magnesium ore deposit: calcining lithium ore deposit: calcium oxide: ferrosilicon: fluorite=30: 5: 100: 48: 7;
(2) reaction mass is crushed to particle diameter less than 0.10mm, mixes and briquetting;
(3) reaction mass is packed into behind the vacuum reducing jar, at vacuum tightness 1-20Pa, the reduction 5 hours down of 1200 ± 50 ℃ of temperature;
(4) collect the alloy steam that reaction generates, and be condensed into condensed state Mg-Li alloy.Its chemical ingredients is for containing Li:10%wt, and the total amount of Mg and Li is greater than 99%wt.
Embodiment 3
(1) ready reaction material, reaction mass is by MgO, Li
2O and Al form, and the batching mass ratio is: MgO: Li
2O: Al=42: 10: 70;
(2) reaction mass is crushed to particle diameter less than 0.10mm, mixes and briquetting;
(3) reaction mass is packed into vacuum reducing jar, at vacuum tightness 1-20Pa, the reduction 5 hours down of 1100 ± 50 ℃ of temperature;
(4) collect the alloy steam that reaction generates, and be condensed into condensed state Mg-Li alloy.Its chemical ingredients is for containing Li:14%wt, and the total amount of Mg and Li is greater than 99.5%wt.
Embodiment 4
(1) ready reaction material, reaction mass is by MgO, Li
2O, carbon dust and CaF
2Form, the batching mass ratio is: MgO: Li
2O: C: CaF
2=21: 10: 32: 3.
(2) reaction mass is crushed to particle diameter less than 0.10mm, mixes and briquetting.
(3) reaction mass is packed into vacuum reducing jar, at vacuum tightness 1-20Pa, the reduction 7 hours down of 1400 ± 50 ℃ of temperature;
(4) collect the alloy steam that reaction generates, and be condensed into condensed state Mg-Li alloy.Its chemical ingredients is for containing Li:25%wt, and the total amount of Mg and Li is greater than 99.5%wt.
Claims (5)
1. the synchronous thermal reduction of vacuum prepares the method for Mg-Li alloy, it is characterized in that raw material has MgO, Li
2O, reductive agent and auxiliary agent are formed.Processing step is: according to the stoichiometry configuration reactant of reduction reaction; With solid reactant powder process and mix; With the reactant powders briquetting and put into the reduction jar; Raw material carries out thermal reduction reaction under vacuum tightness 1-20Pa, temperature 950-1500 ℃ condition, collect the alloy steam that reaction generates, obtain condensed state Mg-Li alloy after the condensation, it is characterized in that, realize the synchronous reduction of MAGNESIUM METAL and metallic lithium, directly prepare magnesium lithium alloy.
2. the synchronous thermal reduction of vacuum according to claim 1 prepares the method for Mg-Li alloy, it is characterized in that, described MgO can replace with the compound of magnesium ore deposit that at high temperature produces MgO or magnesium.
3. the synchronous thermal reduction of vacuum according to claim 1 prepares the method for Mg-Li alloy, it is characterized in that described Li
2O can be with at high temperature producing Li
2The lithium ore deposit of O or the compound of lithium replace.
4. the synchronous thermal reduction of vacuum according to claim 1 prepares the method for Mg-Li alloy, it is characterized in that, the reduction auxiliary agent can be alloys such as ferrosilicon, copper silicon, sial, also can be pure aluminum or carbon.
5. prepare the method for Mg-Li alloy according to the synchronous thermal reduction of vacuum under the claim 1, it is characterized in that contain Li:1-50%wt in the prepared Mg-Li alloy, the total amount of Mg and Li is greater than 99%wt.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103484676A (en) * | 2013-08-23 | 2014-01-01 | 大连融德特种材料有限公司 | Method for processing intermediate alloy after aluminothermic reduction reaction |
| CN105525108A (en) * | 2015-12-16 | 2016-04-27 | 东北大学 | Method for preparing magnesium-calcium alloy through aluminothermic reduction |
| CN105908036A (en) * | 2016-06-21 | 2016-08-31 | 清华大学 | Preparation method for magnesium-lithium alloy with regular structure |
| CN107195895A (en) * | 2017-01-06 | 2017-09-22 | 中国计量大学 | A kind of silica-base material preparation method using alloy as reducing agent |
| CN110042240A (en) * | 2019-04-29 | 2019-07-23 | 安徽工业大学 | A kind of technique that vacuum thermit reduction produces lithium metal and magnesium metal simultaneously |
| CN110195174A (en) * | 2019-05-28 | 2019-09-03 | 昆明理工大学 | A kind of preparation method of aluminium lithium intermediate alloy |
| CN110289391A (en) * | 2019-06-25 | 2019-09-27 | 中南大学 | A kind of lithium metal alloy and the preparation method and application thereof |
| CN111097920A (en) * | 2020-01-03 | 2020-05-05 | 四川万邦胜辉新能源科技有限公司 | Method for producing magnesium-lithium alloy by gaseous co-condensation method |
| CN111286653A (en) * | 2020-03-31 | 2020-06-16 | 东北大学 | Method for producing magnesium-lithium alloy by vacuum aluminothermic reduction |
| CN113042728A (en) * | 2021-03-11 | 2021-06-29 | 北京大学 | Mg-Li alloy nano powder and preparation method and application thereof |
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| CN1834270A (en) * | 2006-04-17 | 2006-09-20 | 重庆大学 | Method of preparing Mg, Sr alloy by vacuum heat reduction |
| CN1924055A (en) * | 2006-09-15 | 2007-03-07 | 苏州有色金属加工研究院 | Magnesium-lithium alloy and manufacture method thereof |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1834270A (en) * | 2006-04-17 | 2006-09-20 | 重庆大学 | Method of preparing Mg, Sr alloy by vacuum heat reduction |
| CN1924055A (en) * | 2006-09-15 | 2007-03-07 | 苏州有色金属加工研究院 | Magnesium-lithium alloy and manufacture method thereof |
Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103484676A (en) * | 2013-08-23 | 2014-01-01 | 大连融德特种材料有限公司 | Method for processing intermediate alloy after aluminothermic reduction reaction |
| CN105525108A (en) * | 2015-12-16 | 2016-04-27 | 东北大学 | Method for preparing magnesium-calcium alloy through aluminothermic reduction |
| CN105525108B (en) * | 2015-12-16 | 2017-10-17 | 东北大学 | A kind of method that magnesium calcium alloy is produced in aluminothermic reduction |
| CN105908036A (en) * | 2016-06-21 | 2016-08-31 | 清华大学 | Preparation method for magnesium-lithium alloy with regular structure |
| CN105908036B (en) * | 2016-06-21 | 2017-08-11 | 清华大学 | Magnesium lithium alloy preparation method with regular weaves |
| CN107195895A (en) * | 2017-01-06 | 2017-09-22 | 中国计量大学 | A kind of silica-base material preparation method using alloy as reducing agent |
| CN110042240A (en) * | 2019-04-29 | 2019-07-23 | 安徽工业大学 | A kind of technique that vacuum thermit reduction produces lithium metal and magnesium metal simultaneously |
| CN110195174B (en) * | 2019-05-28 | 2021-10-15 | 昆明理工大学 | Preparation method of aluminum-lithium intermediate alloy |
| CN110195174A (en) * | 2019-05-28 | 2019-09-03 | 昆明理工大学 | A kind of preparation method of aluminium lithium intermediate alloy |
| CN110289391A (en) * | 2019-06-25 | 2019-09-27 | 中南大学 | A kind of lithium metal alloy and the preparation method and application thereof |
| WO2021135399A1 (en) * | 2020-01-03 | 2021-07-08 | 四川万邦胜辉新能源科技有限公司 | Method for producing magnesium-lithium alloy by means of gaseous co-condensation |
| CN111097920A (en) * | 2020-01-03 | 2020-05-05 | 四川万邦胜辉新能源科技有限公司 | Method for producing magnesium-lithium alloy by gaseous co-condensation method |
| EP3960337A4 (en) * | 2020-01-03 | 2022-09-28 | Sichuan Union Shine New Energy Sci-Tech Co., Ltd | Method for producing magnesium-lithium alloy by means of gaseous co-condensation |
| JP2022547287A (en) * | 2020-01-03 | 2022-11-11 | スーチュァン ユニオン シャイン ニュー エネルギー サイ－テック カンパニー リミテッド | Magnesium Lithium Alloy Production Method by Gas State Coaggregation Method |
| JP7381140B2 (en) | 2020-01-03 | 2023-11-15 | スーチュァン ユニオン シャイン ニュー エネルギー サイ－テック カンパニー リミテッド | Magnesium lithium alloy production method using gas state co-aggregation method |
| CN111286653A (en) * | 2020-03-31 | 2020-06-16 | 东北大学 | Method for producing magnesium-lithium alloy by vacuum aluminothermic reduction |
| CN111286653B (en) * | 2020-03-31 | 2021-06-22 | 东北大学 | Method for producing magnesium-lithium alloy by vacuum aluminothermic reduction |
| CN113042728A (en) * | 2021-03-11 | 2021-06-29 | 北京大学 | Mg-Li alloy nano powder and preparation method and application thereof |
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Application publication date: 20110601 |