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CN1266297C - In-situ synthesized TiC-AI composite ultra-fine grain refining agent and process for preparing same - Google Patents

In-situ synthesized TiC-AI composite ultra-fine grain refining agent and process for preparing same Download PDF

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Publication number
CN1266297C
CN1266297C CN 200310108740 CN200310108740A CN1266297C CN 1266297 C CN1266297 C CN 1266297C CN 200310108740 CN200310108740 CN 200310108740 CN 200310108740 A CN200310108740 A CN 200310108740A CN 1266297 C CN1266297 C CN 1266297C
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grain refiner
prefabricated block
melt
tic
flux
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CN1544678A (en
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王浩伟
马乃恒
张亦杰
李险峰
于敞
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Shanghai Jiao Tong University
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Shanghai Jiao Tong University
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Abstract

The present invention relates to an ultrafine grain refiner of an in-situ self-generating TiC/Al composite material and a preparing method thereof, which belongs to the field of metal materials. The grain refiner of the present invention comprises the following components: 0.1 to 36 wt% of Ti, 0.02 to 8 wt% of C and Al as the rest, wherein the ratio of Ti to C is 4.5:1. A fluxing agent is covered on an Al melting body to melt, and then the fluxing agent is used to flux the prefabricated block of the grain refiner. The preparing method comprises the following steps: (1) using a high-temperature vacuum reaction sintering method to synthesize the prefabricated block of the ultrafine grain refiner; (2) carrying out temperature preservation and baking to the prefabricated block; (3) adding Al ingots to completely melt, then adding chlorine salts and fluorine salts as the fluxing agent to cover the melting body; (4) adding the dried prefabricated block of the ultrafine grain refiner of the composite material after the fluxing agent is melted; (5) stirring the mixture after the prefabricated block is completely melted; (6) statically placing the melting body, then pouring the melting body in an ingot mould to obtain the ultrafine grain refiner of the in-situ self-generating TiC/Al composite material. The ultrafine grain refiner synthesized by the technology has the advantages of obvious refining efficiency, long refining decay time and easy industrial production.

Description

In-situ authigenic TiC/Al matrix material superfine crystal particle fining agent preparation technology
Technical field
The present invention relates to a kind of superfine crystal particle fining agent preparation technology, particularly a kind of in-situ authigenic TiC/Al matrix material superfine crystal particle fining agent preparation technology.Belong to metal material field.
Background technology
Over nearly 20 years, along with the improvement of Al-Ti-B production technique, the purity and the thinning effect of metal are greatly improved, but owing to TiB in the Al-Ti-B master alloy 2Aggregation of particles, to reason such as elements such as Zr, Cr, V, Mn " poisoning " and anti-decay property be relatively poor, the aluminium industry member wishes to develop a kind of novel aluminum grain refiner.As the grain refining effect that the master alloy of grain-refining agent will obtain, will satisfy following two conditions at least: 1. there is a large amount of potential forming core cores in melt; 2. most potential forming core core is active, does not have " poisoning ".The Al-Ti-C grain-refining agent has overcome the defective of Al-Ti-B, and its heterogeneous forming core core TiC compares TiB 2Gathering tendency littler, with Al good coherence effect is arranged, and to element " poisoning " immunity such as Zr, Cr, V, Mn, when identical addition, the Al-Ti-C strengthening effect is better than Al-Ti-B, and the antidamping ability is strong, is to produce aluminium and aluminium alloy ideal grain-refining agent.
Find by literature search, the Chinese patent name is called: Al-Ti-C grain-refining agent and manufacturing process thereof, number of patent application is: 01133647.1, this patent has been introduced and has been utilized from spreading the synthetic Al-Ti-C grain-refining agent of method high temperature, Al-Ti-C grain-refining agent composition weight percent is Ti 30～60%, C 7～15%, all the other are Al, from spreading the synthetic grain-refining agent of method high temperature its unique advantage is arranged, but still have the following disadvantages: 1. reaction is difficult to control, can not effectively control size, form and the content etc. that generate TiC in the grain-refining agent; 2. it is not high enough to react gained grain-refining agent density, and porosity is big, and it is air-breathing that melting aluminium and aluminium alloy add the fashionable melt that easily makes; 3. required time is longer during industrial production time fusing grain-refining agent, prolongs with the melt high temperature hold-time, and melt is air-breathing serious more, thereby produces deleterious oxide inclusion and waste energy, and reduces production efficiency.
Summary of the invention
The objective of the invention is at above-mentioned deficiency of the prior art and defective, a kind of in-situ authigenic TiC/Al matrix material superfine crystal particle fining agent preparation technology is provided, its stirring casting and original position are synthesized to be combined, existing Al-Ti-C grain-refining agent is further improved, prepares that a kind of performance is more excellent, save energy, environmental protection, be easy to the grain-refining agent of suitability for industrialized production.
The present invention is achieved by the following technical solutions, grain-refining agent of the present invention, and its composition and weight percent thereof are: Ti 0.1～36%, and C 0.02～8%, and all the other are Al, wherein Ti: the C ratio is 4.5: 1.This grain-refining agent is used for the grain refining of aluminium and aluminium alloy.
In-situ authigenic TiC/Al matrix material superfine crystal particle fining agent preparation technology of the present invention carries out melting with fusing assistant aluminium coating melt, with the fusing assistant grain-refining agent prefabricated section of fluxing, may further comprise the steps:
(1) utilizes high-temperature vacuum reaction sintering synthesizing superfine grain-refining agent prefabricated section;
(2) to above-mentioned prefabricated section insulation oven dry;
(3) add aluminium ingot and all promptly add villaumite, villiaumite fusing assistant covering melt after the fusing;
(4) fusing assistant fusing back adds the matrix material superfine crystal particle fining agent prefabricated section of drying;
(5) prefabricated section all stirs after the fusing;
(6) pour into ingot mould after melt leaves standstill, promptly obtain in-situ authigenic TiC/Al matrix material superfine crystal particle fining agent.
In the inventive method, described fusing assistant comprises that all contain Cl -, F -Villaumite, villiaumite, as KCl, NaCl, BaCl 2, MgCl 2, CaCl 2, MgCl 2KCl, Na 2SiF 6, Na 3AlF 6, K 2TiF 6, KBF 4, NaF, KF.
In the step (2), prefabricated section is incubated oven dry 2～5 hours in 150 ℃～250 ℃ scope.
In the step (4), prefabricated section adds temperature between 750 ℃～850 ℃.
In the step (5), stirring velocity is 200～400rpm, and churning time is 10～30min, 750 ℃～800 ℃ of whipping temps.
In the step (6), the melt dwell temperature is 700 ℃～750 ℃, and time of repose is 10～20min.
The present invention utilizes the mixing salt superfine crystal particle fining agent prefabricated section of fluxing can shorten fusion time of prefabricated section greatly, reduce the time of molten aluminium at high-temperature residence, reduce and generate harmful oxide inclusion and the air-breathing probability of melt, and the TiC particle that can effectively disperse in-situ authigenic, and stirring casting and in-situ authigenic combined, be suitable for the suitability for industrialized production of grain-refining agent more.
Compare with other technology, gained in-situ authigenic TiC/Al matrix material superfine crystal particle fining agent of the present invention has the following advantages: (1) in-situ authigenic TiC is a thermodynamically stable phase and close with the aluminium lattice parameter, and good coherency is arranged; (2) cleaning of in-situ authigenic TiC particle surface is pollution-free, combines well with the aluminum substrate interface; (3) thinning effect is obvious, and grain size is about 50um～100um; (4) the anti-ageing ability of moving back is good, no refinement decay in three hours; (5) fusing time was fast after the grain-refining agent prefabricated section added aluminium and aluminium alloy melt, save energy; (6) be adapted to the production forging type of various aluminum alloy castinges; (7) simple to operate, be easy to suitability for industrialized production.In view of above advantage, the aluminium of new generation that realizability of the present invention can be excellent and the preparation of industrialization of aluminum grain refiner.
Embodiment
Provide following examples in conjunction with content of the present invention, the present invention done further understanding:
Embodiment 1
The superfine crystal particle fining agent weight percentages of components of preparation is: Ti 0.1%, and C 0.02%, and Al 98.9%, and preparation process is as follows:
Fine aluminium fusing back adds KCl, NaCl, Na 3AlF 6, the KF fusing assistant covers, thermometric after the whole fusions of fusing assistant, temperature reaches 750 ℃, adds through 5 hours prefabricated section of 150 ℃ of insulation oven dry, prefabricated section all melts the back and stirs speed stirring 10min with whipping appts with the commentaries on classics of 200rpm, whipping temp is 750 ℃.Pour ingot mould through 700 ℃ into after leaving standstill 10min and promptly get TiC/Al matrix material superfine crystal particle fining agent.Gained matrix material superfine crystal particle fining agent is added in the ZL101 alloy, and add-on is 0.15% (weight percent), and the sample after solidifying has tiny equiax crystal, and grain-size is 60um～90um, and the refinement decline does not appear in its grain refining effect in 3 hours.
Embodiment 2
The superfine crystal particle fining agent weight percentages of components of preparation is: Ti 18%, and C 4%, and Al 68%, and preparation process is as follows:
Fine aluminium fusing back adds MgCl 2, Na 2SiF 6, K 2TiF 6, BaCl 2Fusing assistant covers, thermometric after the whole fusions of fusing assistant, and temperature reaches 800 ℃, adds through 3.5 hours prefabricated section of 200 ℃ of insulation oven dry, and prefabricated section all melts the back and stirs 15min with whipping appts with the commentaries on classics of the 300rpm speed of stirring, and whipping temp is 780 ℃.Pour ingot mould through 730 ℃ into after leaving standstill 15min and promptly get TiC/Al matrix material superfine crystal particle fining agent.Gained matrix material superfine crystal particle fining agent is added in the ZL 109 alloy, and add-on is 0.06% (weight percent), and the sample after solidifying has tiny equiax crystal, and grain-size is 50um～90um, and the refinement decline does not appear in its grain refining effect in 3 hours
Embodiment 3
The superfine crystal particle fining agent weight percentages of components of preparation is: Ti 36%, and C 8%, and Al 56%, and preparation process is as follows:
With the fine aluminium MgCl after the fusing 2KCl, CaCl 2, NaF 6, KBF 4Fusing assistant covers, thermometric after the whole fusions of fusing assistant, temperature reach 850 ℃, add through 2 hours grain-refining agent prefabricated section of 250 ℃ of insulation oven dry, prefabricated section all melts the back and stirs 30min with whipping appts with the commentaries on classics of the 400rpm speed of stirring, and whipping temp is 800 ℃.Pour ingot mould through 750 ℃ into after leaving standstill 20min and promptly get TiC/Al matrix material superfine crystal particle fining agent.Gained matrix material superfine crystal particle fining agent is added in the ZL204 alloy, and add-on is 0.01% (weight percent), and the sample after solidifying has tiny equiax crystal, and grain-size is 50um～80um, and the refinement decline does not appear in its grain refining effect in 3 hours.

Claims (2)

1、一种原位自生TiC/Al复合材料超细晶粒细化剂制备工艺，其特征在于，晶粒细化剂的成份及其重量百分比为：Ti 0.1～36％，C 0.02～8％，其余为Al，其中Ti∶C比为4.5∶1，用助熔剂覆盖铝熔体进行熔炼，用助熔剂助熔晶粒细化剂预制块，包括以下步骤：1. A process for preparing an in-situ self-generated TiC/Al composite material ultra-fine grain refiner, characterized in that the composition and weight percentage of the grain refiner are: Ti 0.1-36%, C 0.02-8% , the rest being Al, wherein the Ti:C ratio is 4.5:1, covering the aluminum melt with a flux for smelting, and prefabricating a block with a flux flux grain refiner, comprising the following steps: (1)利用高温真空反应烧结法合成超细晶粒细化剂预制块；(1) Utilize the high-temperature vacuum reaction sintering method to synthesize the ultra-fine grain refiner prefabricated block; (2)对上述预制块保温烘干；(2) drying the above-mentioned prefabricated blocks insulated; (3)加入铝锭全部熔化后即加入氯盐、氟盐助熔剂覆盖熔体；(3) Add chlorine salt and fluorine salt flux to cover the melt after all the aluminum ingots are melted; (4)助熔剂熔化后加入经烘干的复合材料超细晶粒细化剂预制块；(4) After the melting agent is melted, add the dried composite material ultrafine grain refiner prefabricated block; (5)预制块全部熔化后进行搅拌；(5) Stir after the prefabricated blocks are all melted; (6)熔体静置后浇入锭模，即获得原位自生TiC/Al复合材料超细晶粒细化剂；(6) After the melt is allowed to stand still, it is poured into an ingot mold to obtain an in-situ authigenic TiC/Al composite ultrafine grain refiner; 步骤(2)中，预制块在150℃～250℃的范围内保温烘干2～5小时；In step (2), the prefabricated block is heat-preserved and dried within the range of 150°C to 250°C for 2 to 5 hours; 步骤(4)中，预制块加入温度在750℃～850℃之间；In step (4), the prefabricated block is added at a temperature between 750°C and 850°C; 步骤(5)中，搅拌速度为200～400rpm，搅拌时间为10～30min，搅拌温度750℃～800℃；In step (5), the stirring speed is 200-400rpm, the stirring time is 10-30min, and the stirring temperature is 750°C-800°C; 步骤(6)中，熔体静置温度为700℃～750℃，静置时间为10～20min。In step (6), the resting temperature of the melt is 700° C. to 750° C., and the resting time is 10 to 20 minutes. 2、根据权利要求1所述的原位自生TiC/Al复合材料超细晶粒细化剂制备工艺，其特征是，所述的助熔剂为：KCl、NaCl、BaCl2、MgCl2、CaCl2、MgCl2·KCl、Na2SiF6、Na3AlF6、K2TiF6、KBF4、NaF、KF含Cl-、F-的氯盐、氟盐。2. The process for preparing an in-situ self-generated TiC/Al composite ultra-fine grain refiner according to claim 1, characterized in that the flux is: KCl, NaCl, BaCl 2 , MgCl 2 , CaCl 2 , MgCl 2 ·KCl, Na 2 SiF 6 , Na 3 AlF 6 , K 2 TiF 6 , KBF 4 , NaF, KF Cl - , F - chloride salt, fluorine salt.
CN 200310108740 2003-11-20 2003-11-20 In-situ synthesized TiC-AI composite ultra-fine grain refining agent and process for preparing same Expired - Fee Related CN1266297C (en)

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CN101812649B (en) * 2010-02-05 2012-01-04 新星化工冶金材料(深圳)有限公司 Method for controlling variable quantity of grain refining capability of aluminum-titanium-carbon alloy during pressure processing of aluminum-titanium-carbon alloy
CN101775564B (en) * 2010-02-05 2012-07-04 深圳市新星轻合金材料股份有限公司 Method for controlling variation of grain refinement ability of aluminum-titanium-boron alloy during pressure processing
CN101768708B (en) * 2010-02-05 2012-05-23 深圳市新星轻合金材料股份有限公司 Method for controlling variable quantity of grain refining capacity of aluminum-titanium-boron alloy by controlling compression ratio
CN102489692A (en) * 2011-12-05 2012-06-13 大连理工大学 Method for preparing Al-Ti-C-Gd grain refiner of magnesium alloys by utilizing ultrasonic waves
CN103820683B (en) * 2014-02-28 2016-10-05 华南理工大学 The multiple elements design fine degenerate processing method of Fe phase in a kind of high Fe alusil alloy
CN106544531A (en) * 2015-09-22 2017-03-29 中国矿业大学 A kind of process of In-situ Synthesis TiC Particle refining aluminum alloy solidified structure
CN106086500B (en) * 2016-08-02 2018-01-19 西安交通大学 A kind of method for preparing the continuous reinforced Al matrix composite of in-situ three-dimensional
CN106244866A (en) * 2016-09-20 2016-12-21 桂林理工大学 A kind of preparation method of nano TiN reinforced aluminum matrix composites
CN107236873B (en) * 2017-08-02 2018-10-23 合肥市田源精铸有限公司 A kind of method of aluminium alloy fine degenerate processing
GB201713005D0 (en) * 2017-08-14 2017-09-27 Univ Brunel The alloy and manufacturing method of Al-Si-Mg castings for improved mechanical performance
CN112899512B (en) * 2021-01-19 2022-08-12 合肥波林新材料股份有限公司 Aluminum-titanium-carbon alloy grain refiner and preparation method thereof

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