CN101928845A - Preparation method of lithium-contained alloy material - Google Patents

Preparation method of lithium-contained alloy material Download PDF

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Publication number
CN101928845A
CN101928845A CN2009101463086A CN200910146308A CN101928845A CN 101928845 A CN101928845 A CN 101928845A CN 2009101463086 A CN2009101463086 A CN 2009101463086A CN 200910146308 A CN200910146308 A CN 200910146308A CN 101928845 A CN101928845 A CN 101928845A
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alloy
lithium
soup
production method
alloy material
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叶明堂
戴云城
傅荣顺
陈诗薇
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Anli Material Science & Technology Co Ltd
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Abstract

The invention discloses a preparation method of a lithium-contained alloy material and provides a design application of the light alloy material which is used to prepare the light structural element. The technology comprises the following steps: firstly fusing alloy materials according to a demand ratio to obtain homogeneous alloy soup, secondly pouring the alloy soup in a ladle with prestored lithium material under the protection of inert gas, utilizing the heat flow of the alloy soup and the diffusion of the lithium material in the alloy soup to perform violent eroding and mixing, and pouring the evenly mixed alloy soup with the lithium material in a mould to form lithium alloy. By adopting the preparation method of the invention, the fundamental problems that the traditional smelting method causes pollutions owning to long reaction time and superheated temperature and components are difficult to handle are solved; and the preparation method is novel, safe, economical and efficient.

Description

The alloy material production method that contains lithium
Technical field
The present invention relates to a kind of alloy material, relate in particular to a kind of manufacture method that contains the alloy material of lithium.
Background technology
The lithium material is that (density of lithium is 0.534 gram/cubic centimeter (g/cm to the minimum metal of density 3)), make the relative reduction of density of its alloy, thereby be the splendid candidate material of lightweight structure element when making design.Yet lithium is very active element, fusing point low again (fusing point of lithium be centigradetemperature 180.54 degree (℃)); very easily oxidation and volatilization when being heated; only the fusing point of the alloying element that is added in the lithium alloy is much higher with respect to lithium, so cause the unusual difficulty of the melting of lithium alloy.
Traditional smelting process of lithium alloy is that (Vacuum Induction Melting, VIM) technology generally are divided into forward reinforced method and two kinds of technology of reverse reinforced method to the employing vacuum induction melting.Wherein, forward the step of reinforced method smelting technique is: (1-1) with induction furnace pumping high vacuum (10 -1To 10 -5Pa (handkerchief)), so as to the cavity in the cleaning induction furnace; (1-2) the lithium piece is inserted in the crucible, and this crucible is positioned in the induction furnace cavity,, and continue to vacuumize with the intravital gas in abundant eliminating chamber with the small power induction heating; (1-3) inject argon gas in cavity, and begin to improve heating power, make the lithium piece in down fusing of high temperature, this high temperature reaches can be with other alloy material interfused temperature, for example, and the melting temperature of metals such as titanium, aluminium, manganese and magnesium; (1-4) then add the alloy material successively and in the lithium material of melted state, carry out alloying reaction, to form lithium alloy soup.Because the proportion of alloy material is greater than the lithium material, therefore, make the alloy material directly sink to crucible bottom, at this moment, be attached to impurity such as the lip-deep aqueous vapor of alloy material, oil stain, to enter together in the lithium material of melted state, make in the lithium material of melted state to have pollutents such as oxygen, hydrogen or carbon, and then cause compounds such as lithium oxide compound, lithium carbide in lithium alloy soup, to form.
Here wanting ben is, the proportion of these lithium oxide compounds or lithium carbide is suitable with the proportion of lithium alloy soup, and be mixed in the lithium alloy soup, therefore, can't lithium oxide compound and lithium carbide be separated from lithium alloy soup with gravity method, and its activity will be more stable when hydrogen is solid-solubilized in the alloy soup that contains lithium, when so in a single day lithium alloy soup be subjected to polluting, will be extremely difficult that these contaminant exclusion are clean; (1-5) desire to make the alloy material that sinks to crucible bottom and the lithium of melted state to fuse fully, have only and lean on hoisting power to draw high temperature and time expand again, still, this kind method not only makes the lithium volatilization more, and make the lithium material of melted state draw more pollutent again, and cause composition failure out of control; (1-6) treat that lithium alloy soup fuses back (in fact the blow piece does not sink to very difficult perceiving at the bottom of the crucible) fully, leave standstill slightly to pour into again to become ingot in the mold, and finish the making of lithium alloy.
Smelting technique step as for reverse reinforced method is as follows: (2-1) the still first pumping high vacuum of induction furnace is with peace and quiet as far as possible cavity; (2-2) continue to vacuumize, put into the high-meltiing alloy material in the crucible, first small power and high-power heating make it fusion, and maintain suitable high temperature, up to the complete soupization of alloy material; (2-3) injecting argon gas inserts the lithium material in the crucible again, the lithium material is subjected to high hot melt to separate and float in the superiors, it is place for being vulnerable to pollute most, yet, because of alloy material and lithium material proportion differ very great disparity (density is than about 3~20 times), must consume longer time fusion, fundamentally also can't avoid facing failure because of the pollution and the composition volatilization problem of melting time due to long, overheated; (2-4) treat that lithium alloy soup fuses fully after, leave standstill slightly to pour into again and become ingot in the mold.
In sum, in existing lithium alloy smelting technique, process for vacuum induction smelting be owing to essential first be heated to the melting temperature (Tm) of alloy material with the lithium material, and maintains this temperature for a long time and fuse fully with the alloy material of guaranteeing to be added in waiting a moment.Because the fusing point difference between lithium material and the alloy material is very big, therefore, the lithium material is volatilized under this hot environment, cause lithium material content in the lithium alloy can't effectively control waste with the lithium material.And, this prior art is that the alloy material directly is incorporated in the lithium material of melted state, makes the lithium material of melted state be subjected to the impurity that alloy material adhering on surface easily and pollutes, therefore, exist in the lithium alloy soup to have pollutent, and then cause the composition problem that makes lithium alloy make failure out of control.
In addition, in reverse reinforced method smelting technique, because the difference of specific gravity between lithium material and the alloy material is very big, therefore, when the lithium material is incorporated in alloy soup, the lithium material after the fusing will fly at the superiors of alloy soup, and the coating that can't be subjected to alloy soup owing to the lithium material is exposed to alloy soup surface, therefore, the degree of risk that the lithium material is polluted increases.And,, make between lithium material and the alloy soup and can't in the short period of time, mix completely, and must elongate the lithium alloy that the fusion time between the two just can obtain mixing because the lithium material can't be settled down in the alloy soup.
Therefore, existing lithium alloy smelting technique all can't be avoided making whole technology be full of variable because of long-time overheated institute deutero-pollutes and factor such as composition is out of control, causes the quality of lithium alloy effectively to promote.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of alloy material production method that contains lithium, pollutes and composition defective out of control because of long-time overheated institute deutero-so as to overcoming in the existing lithium alloy smelting technique.
For achieving the above object, the present invention discloses a kind of alloy material production method that contains lithium, and its step comprises: (1) is put at least one alloying element in the smelting pot of one vacuum induction furnace; (2) induction heating in vacuum induction furnace, making the alloying element fusion is a uniform alloy soup; (3) this alloy soup is poured into contained protection of inert gas and preset in the Sheng bucket of lithium material; (4) shake the Sheng bucket, so that alloy soup washes away intensely the lithium material and mixes; And (5) pour the molten soup of lithium alloy in one mold into and become ingot, to form lithium alloy.
The disclosed alloy material production method that contains lithium of the present invention, wherein, step (2) is with pumping high vacuum in the vacuum induction furnace, makes alloying element carry out induction heating under vacuum environment.
The disclosed alloy material production method that contains lithium of the present invention, wherein, step (2) is to the alloying element induction heating under atmospheric environment.
The disclosed alloy material production method that contains lithium of the present invention wherein, also comprises the step that bucket is contained in a preheating before in step (3).
The disclosed alloy material production method that contains lithium of the present invention, wherein, step (4) comprises and is aided with an agitator and adds strong mixing alloy soup and lithium material.
The disclosed alloy material production method that contains lithium of the present invention, wherein, agitator is an electromagnetic shaker.
The disclosed alloy material production method that contains lithium of the present invention, wherein, agitator is a ruhmkorff coil.
The disclosed alloy material production method that contains lithium of the present invention, wherein, alloying element be selected from the group that forms by aluminium, magnesium, manganese, zirconium, zinc, titanium, scandium, yttrium, copper, silver and silicon one of them and composition thereof.
The disclosed alloy material production method that contains lithium of the present invention, wherein, alloying element is a magnesium, to found a lithium magnesium alloy.
The disclosed alloy material production method that contains lithium of the present invention, wherein, alloying element is an aluminium, to found a lithium-aluminium alloy.
The disclosed alloy material production method that contains lithium of the present invention, heat fusion in the vacuum induction furnace to form alloy soup for earlier alloying element being placed in, by this step the pollutent that is attached to the alloying element surface is removed completely, be subjected to the pollution of pollutent to avoid the lithium material.Then; again alloy soup is poured in containing protection of inert gas and presetting in the Sheng bucket of lithium material; by alloy soup the lithium material is washed away; mix; and make the lithium material be subjected to the alloy steamed dumping to cover; when making the fusing of lithium material; in alloy soup, produce diffusion; therefore; the lithium material is except the protection that is subjected to alloy soup and avoid being polluted; and the purpose that makes lithium material and alloy soup mix and significantly reduce mixing time simultaneously; and obtain high-quality Zinc-lithium alloy material; volatilize under hot environment thereby solved existing lithium material, and cause the waste of lithium material and the lithium alloy that completes in the problem that can't control of the component content of lithium material, and when lithium material and the fusion of alloy material; be subjected to the pollution of impurity easily; contain pollutent in the lithium alloy and cause lithium alloy to make the problem of failure, and solved simultaneously between lithium material and the alloy material, because the relation of difference of specific gravity; and exist the lithium material can't effectively to mix, and need long fusion just can obtain the problem of even interfused lithium alloy with the alloy material.
Above about content of the present invention explanation and the explanation of following embodiment in order to demonstration with explain principle of the present invention, and provide claim of the present invention further to explain.
Embodiment
For realizing the technique means of the aforementioned purpose of the present invention, illustrate with the following example now:
<embodiment one〉melting of lithium-magnesium alloy
Magnesium is epochmaking light metal (1.74g/cm 3), if can add in a large number in the lithium alloy, more can keep the low density characteristic of lithium alloy, therefore, the present invention attempt with magnesium as with lithium blended main alloy element.By the disclosed alloy material production method that contains lithium of the present invention, at first look demand percentage magnesium (Mg), aluminium (Al), zinc (Zn), zirconium (Zr), scandium (Sc), yttrium (Y) etc. are had dystectic alloying element counterweight or select to adopt magnesium as single alloying element and lithium formation magnesium lithium alloy to scale.Be the manufacturing of carrying out lithium alloy with a plurality of alloying elements in present embodiment, and counterweight is allocated the alloying element mixture of finishing to scale, proportion that it had and fusing point are greater than elemental lithium.
The mixed alloying element of counterweight is to scale put into the crucible of vacuum induction melting furnace, with induction furnace pumping high vacuum (10 -1To 10 -5Handkerchief (Pa)), alloy material is in the vacuum environment.Wherein the counterweight ratio of each alloy material as shown in Table 1, the unit of counterweight ratio represents with weight percent (wt%).
, break away from small power preheating alloy material by induction heating, in subsequent step, the lithium material is polluted to avoid these pollutents with the pollutent that helps alloy material degasification scrubbing, make to be attached to the alloy material surface.Then inject argon gas in induction furnace, and walk unhurriedly and carry the heating superpower, form alloy soup with induction heating alloying material.Holding warm appropriate time (kind and amount on alloying element are decided) between 700 ℃ to 850 ℃, is alloy soup until the complete penetration of alloying element.
Then, the alloy soup of complete penetration is poured in the Sheng bucket of specific dimensions into (the bucket footpath that makes the degree of depth of alloy soup be equivalent to contain bucket), and contained the lithium piece that presets requirement in the bucket.Pouring into when containing in the bucket when alloy soup, is with alloy soup hot-fluid the lithium piece to be carried out fierce washing away, mixes, and makes the lithium piece be subjected to the coating of alloy soup and fuse in alloy soup and the generation diffusion.At this moment,, therefore, make the lithium material in alloy soup, have the characteristic of high diffusion because the proportion of lithium material is lower than alloy material, and then, reach lithium material and the mixed uniformly purpose of alloy soup.For improving the success ratio of founding of lithium alloy, must consider the relation between amount, temperature and the lithium material amount of alloy soup in this step.And, can before containing bucket, will contain bucket earlier and carry out the operation of preheating by pouring into, and will contain and barrel be arranged on an electromagnetic shaker or add strong mixing, with the mixing efficiency between increase lithium material and the alloy material with agitators such as electromagnetic induction coils at alloy soup.
In alloy soup pour into contain last about 2 minutes in the bucket after, the lithium alloy soup that lithium material and alloy soup are uniformly mixed to form is poured in the mold again, and is to be cooled to the temperature below 100 ℃, can take out the lithium magnesium alloy ingot from mold.
By the disclosed alloy material production method that contains lithium of the present invention, avoided in the existing smelting technique, the lithium material is because of the long-time overheated produced pollution and composition problem out of control, success a series of high quality ultralight lithium magnesium alloy of refining such as following table one are listed, ingot casting is of a size of 205 millimeters of external diameters (mm), be about 500mm, heavily about 25 kilograms (Kg).
Table one
Remove the section of dead head from the outward appearance of ingot casting and saw, all discoveries of pore-free bubble, these lithium magnesium alloy are squeezed type processing 180 ℃ to 250 ℃ intercropping, directly extrude the thick sheet material of 3mm, then detect its cold rolling, because the forming property of these alloys is very excellent stable, can roll the amount of prolonging and surpass 50%, roll smoothly and prolong into thin plate (0.15 to 1.0mm), technology annealing (Inter-annealing) temperature wherein adopts 220 ℃, sum up their mechanical and physical performance and lightweight aluminium, titanium material and make comparisons, result relatively is as shown in table two.
Table two
Figure B2009101463086D0000052
Because above-mentioned each lithium magnesium alloy all has rerum naturas such as low density, high specific stiffness, high in-fighting absorbing and high formability, this three high one low characteristic extremely is fit to the application of horn vibration film.Select the thick C latten of 0.15mm for use, it is struck out horn vibration film, and be assembled into the loudspeaker monomer, in anechoic chamber, measure acoustic pressure (the sound Pressure Level of different frequency according to loudspeaker standard criticism test method, SPL) curvilinear motion, make comparisons with homotype aluminium matter loudspeaker, find that the following acoustic pressure difference of 500Hz (hertz) is also little, but between 500 to 7000Hz frequency range, the acoustic pressure performance of lithium magnesium loudspeaker is then more steady, (Harmonic Distortion) is less in the variation of tonequality, demonstrates application potential in this regard.
<embodiment two〉melting of lithium-aluminium alloy
Aluminium also is a kind of light metal (2.71g/cm 3), also for containing the preferred alloy additive of lithium alloy, so the present invention also selects lithium-aluminium alloy to do the melting comparison, its melting step is as follows: earlier with aluminium (Al), magnesium (Mg), manganese (Mn), copper (Cu), titanium (Ti), zirconium (Zr), silver (Ag), zinc (Zn), silicon alloy materials such as (Si) the ratio weighing according to following table three, and according to the step of embodiment one, found into alloy soup at 800 ℃, then pour into to contain in the bucket and puddle evenly with lithium, reinjecting becomes ingot in the mold, has also avoided the long-time overheated produced pollution and composition problem out of control.Ingot casting external diameter 205mm, the about 500mm of length, heavily about 40kg.Inspect the section that these ingot casting outward appearances and saw remove dead head, the also discovery of pore-free bubble, and directly extrude into tubing and sheet material at 400 ℃, the material unit elongation that squeezes under the attitude surpasses 15%, the cold rolling character of tool, warm-rolling is then better, and the design that is fit to the light structure material is used, for example sports equipment such as bicycle.
Table three
Figure B2009101463086D0000062
Figure B2009101463086D0000071
<embodiment three〉medium-sized gas lithium alloy smelting process
In order to reduce the cost of manufacture of lithium alloy again; simplify smelter flowsheet among this embodiment; the magnesium alloy soup of embodiment one is imposed the melting of flux (Flux) cladding process atmosphere instead; the aluminium alloy soup of embodiment two then changes melting in the atmosphere into; after both all carry out degasification (hydrogen) step; immigration has in the separate space of protection of inert gas; pour in the Sheng bucket that presets the lithium material; become ingot in the impouring mold again after waiting to puddle evenly; the long-time overheated produced pollution and composition problem out of control have been avoided equally; ingot quality and previous result are the same as a result, and medium-sized gas lithium alloy smelting process is succeedd again.
The disclosed alloy material production method that contains lithium of the present invention owing to earlier alloying element is placed in heating fusion in the vacuum induction furnace, is removed the pollutent that is attached to the alloying element surface fully, and is avoided lithium alloy to be polluted in manufacturing processed.And the lithium material is washed away, mixes by alloy soup; and the diffusion that in alloy soup, produced of lithium material; the lithium material fuses by the temperature of alloy soup; can prevent the lithium material from producing volatilization and cause the loss of lithium material; and can further protect the lithium material to avoid being polluted, also can reach the purpose that makes lithium material and alloy soup mix, significantly reduce mixing time and obtain the high quality Zinc-lithium alloy material simultaneously.
Certainly; the present invention also can have other various embodiments; under the situation that does not deviate from spirit of the present invention and essence thereof; those of ordinary skill in the art work as can make various corresponding changes and distortion according to the present invention, but these corresponding changes and distortion all should belong to the protection domain of the appended claim of the present invention.

Claims (10)

1. an alloy material production method that contains lithium is characterized in that, comprises step:
Step 1: at least one alloying element is put in the smelting pot of a vacuum induction furnace;
Step 2: carry out induction heating in this vacuum induction furnace, making this alloying element fusion is an alloy soup;
Step 3: this alloy soup poured into contain protection of inert gas and preset one of a lithium material and contain in the bucket;
Step 4: shake this Sheng bucket, so that this alloy soup washes away intensely this lithium material and mixes; And
Step 5: the molten soup of this lithium alloy poured in the mold become ingot, to form a lithium alloy.
2. the alloy material production method that contains lithium according to claim 1 is characterized in that, this step 2 is with pumping high vacuum in this vacuum induction furnace, makes this alloying element carry out induction heating under vacuum environment.
3. the alloy material production method that contains lithium according to claim 1 is characterized in that, this step 2 is to this alloying element induction heating under atmospheric environment.
4. the alloy material production method that contains lithium according to claim 1 is characterized in that, also comprises the step of this Sheng bucket of a preheating before this step 3.
5. the alloy material production method that contains lithium according to claim 1 is characterized in that, this step 4 comprises and is aided with an agitator and adds this alloy soup of strong mixing and this lithium material.
6. the alloy material production method that contains lithium according to claim 5 is characterized in that, this agitator is an electromagnetic shaker.
7. the alloy material production method that contains lithium according to claim 5 is characterized in that, this agitator is an electromagnetic induction coil.
8. the alloy material production method that contains lithium according to claim 1 is characterized in that, this alloying element is selected from the group that is made up of aluminium, magnesium, manganese, zirconium, zinc, titanium, scandium, yttrium, copper, silver and silicon one of them or its mixture.
9. the alloy material production method that contains lithium according to claim 1 is characterized in that the composition of this alloying element is mainly magnesium, to found a lithium magnesium alloy.
10. the alloy material production method that contains lithium according to claim 1 is characterized in that the composition of this alloying element is mainly aluminium, to found a lithium-aluminium alloy.
CN2009101463086A 2009-06-19 2009-06-19 Preparation method of lithium-contained alloy material Pending CN101928845A (en)

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108337622A (en) * 2018-03-05 2018-07-27 苏州市艾倍力精密电子有限公司 A kind of acoustic diaphragm, diaphragm materials and vibrating diaphragm preparation process
CN109093077A (en) * 2018-10-14 2018-12-28 昆山建金工业设计有限公司 A kind of device of ferro element and aluminium element composite material
CN109280785A (en) * 2018-11-22 2019-01-29 奉新赣锋锂业有限公司 A kind of process units and method of lithium magnesium alloy
US10280496B2 (en) 2016-01-07 2019-05-07 Amli Materials Technology Co., Ltd. Light magnesium alloy and method for forming the same
CN109913719A (en) * 2017-12-12 2019-06-21 富士通株式会社 Magnesium alloy and its manufacturing method and electronic equipment
CN110666114A (en) * 2019-11-14 2020-01-10 江西江锐新材料科技有限公司 Nickel-lithium alloy preparation equipment and preparation method thereof
CN112373738A (en) * 2020-11-23 2021-02-19 北京空间机电研究所 Thin-wall structure vibration test device and test method considering pressure difference condition
CN113042728A (en) * 2021-03-11 2021-06-29 北京大学 Mg-Li alloy nano powder and preparation method and application thereof
CN115786751A (en) * 2022-11-15 2023-03-14 重庆天齐锂业有限责任公司 Lithium magnesium silicon alloy smelting method

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US10280496B2 (en) 2016-01-07 2019-05-07 Amli Materials Technology Co., Ltd. Light magnesium alloy and method for forming the same
CN109913719A (en) * 2017-12-12 2019-06-21 富士通株式会社 Magnesium alloy and its manufacturing method and electronic equipment
CN109913719B (en) * 2017-12-12 2021-12-07 富士通株式会社 Magnesium alloy, method for producing same, and electronic device
CN108337622A (en) * 2018-03-05 2018-07-27 苏州市艾倍力精密电子有限公司 A kind of acoustic diaphragm, diaphragm materials and vibrating diaphragm preparation process
CN109093077A (en) * 2018-10-14 2018-12-28 昆山建金工业设计有限公司 A kind of device of ferro element and aluminium element composite material
CN109280785A (en) * 2018-11-22 2019-01-29 奉新赣锋锂业有限公司 A kind of process units and method of lithium magnesium alloy
CN110666114A (en) * 2019-11-14 2020-01-10 江西江锐新材料科技有限公司 Nickel-lithium alloy preparation equipment and preparation method thereof
CN112373738A (en) * 2020-11-23 2021-02-19 北京空间机电研究所 Thin-wall structure vibration test device and test method considering pressure difference condition
CN113042728A (en) * 2021-03-11 2021-06-29 北京大学 Mg-Li alloy nano powder and preparation method and application thereof
CN115786751A (en) * 2022-11-15 2023-03-14 重庆天齐锂业有限责任公司 Lithium magnesium silicon alloy smelting method
CN115786751B (en) * 2022-11-15 2024-01-19 重庆天齐锂业有限责任公司 Smelting method of lithium-magnesium-silicon alloy

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Application publication date: 20101229