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 PDFInfo
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- 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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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
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, a kind of in-situ authigenic TiC/Al matrix material superfine crystal particle fining agent preparation technology, it is characterized in that, the composition of grain-refining agent and weight percent thereof are: Ti 0.1～36%, C 0.02～8%, all the other are Al, wherein Ti: the C ratio is 4.5: 1, 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 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.
2, in-situ authigenic TiC/Al matrix material superfine crystal particle fining agent preparation technology according to claim 1 is characterized in that described fusing assistant is: KCl, NaCl, BaCl
2, MgCl
2, CaCl
2, MgCl
2KCl, Na
2SiF
6, Na
3AlF
6, K
2TiF
6, KBF
4, NaF, KF contain Cl
-, F
-Villaumite, villiaumite.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200310108740 CN1266297C (en) | 2003-11-20 | 2003-11-20 | In-situ synthesized TiC-AI composite ultra-fine grain refining agent and process for preparing same |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200310108740 CN1266297C (en) | 2003-11-20 | 2003-11-20 | In-situ synthesized TiC-AI composite ultra-fine grain refining agent and process for preparing same |
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|---|---|
| CN1544678A CN1544678A (en) | 2004-11-10 |
| CN1266297C true CN1266297C (en) | 2006-07-26 |
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Families Citing this family (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
| 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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