CN106498201B - The preparation method of aluminium and its alloy Al-Nb-Cr-B grain refiner - Google Patents

The preparation method of aluminium and its alloy Al-Nb-Cr-B grain refiner Download PDF

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CN106498201B
CN106498201B CN201611046981.9A CN201611046981A CN106498201B CN 106498201 B CN106498201 B CN 106498201B CN 201611046981 A CN201611046981 A CN 201611046981A CN 106498201 B CN106498201 B CN 106498201B
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grain refiner
pure
preparation
aluminium
potassium fluoborate
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CN106498201A (en
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韩延峰
陆树生
徐钧
张佼
顾孙望
尤伟任
孙宝德
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SHANGHAI ZHONGTIAN ALUMINIUM WIRE CO Ltd
Shanghai Jiaotong University
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SHANGHAI ZHONGTIAN ALUMINIUM WIRE CO Ltd
Shanghai Jiaotong University
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/02Making non-ferrous alloys by melting
    • C22C1/026Alloys based on aluminium
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/06Making non-ferrous alloys with the use of special agents for refining or deoxidising
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C21/00Alloys based on aluminium

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

The present invention discloses a kind of aluminium and its alloy Al-Nb-Cr-B grain refiner and preparation method thereof, and the fining agent includes the component of following each weight content: 1.00-6.00%Nb, 1.00-3.00%Cr, 0.50-1.00%B, surplus Al;Step are as follows: (1) weigh pure niobium, pure chromium, potassium fluoborate and commercial-purity aluminium respectively, and pure niobium, pure chromium and potassium fluoborate powder are uniformly mixed;(2) the weighed commercial-purity aluminium of heating fusing institute, obtains aluminum melt;(3) prepared pure niobium, pure chromium and potassium fluoborate mixed powder are pressed into aluminum melt using graphite bell jar;(4) processing of continual ultrasonic wave is introduced on the aluminum melt top that pure niobium, pure chromium and potassium fluoborate mixed powder is added;(5) make melt natural cooling, obtain Al-Nb-Cr-B grain refiner.The present invention breaks through existing Al-Ti-B system grain refiner to the refinement limit of aluminium alloy.

Description

The preparation method of aluminium and its alloy Al-Nb-Cr-B grain refiner
Technical field
The present invention relates to grain refiner of a kind of metal material field and preparation method thereof, specifically a kind of aluminium and its conjunction Gold Al-Nb-Cr-B grain refiner and preparation method thereof.
Background technique
In method of modifying of the tradition to solidified structure, thinning solidification structure crystal grain, i.e. refined crystalline strengthening can be promoted simultaneously The intensity and plasticity and toughness of material effectively inhibit loose, reduce hot cracking tendency, are to promote the most effective side of alloy comprehensive mechanical property One of method.For aluminium alloy, early in the thirties in last century, find that the Ti element being added in aluminum melt can be with refining aluminum alloy The crystallite dimension of solidified structure, many decades, the aluminium alloy fining agent containing Ti are gradually developed, improve and be applied to industry life later It produces.
Currently, technique is the most simple and convenient in aluminium alloy manufacture field, the most excellent crystal fining method of effect is Al-Ti-B system grain refiner is added into melt, to introduce the heterogeneous nucleation mass point of boride, promotes heterogeneous forming core and thin Change solidified structure.Due to the nucleation mass point TiB in Al-Ti-B grain refiner2Lattice between solidification Nucleation α-Al is wrong It is 6%, TiB with degree2The effective percentage of nucleation mass point only has 1% or so, and to the refinement of aluminium alloy as-cast grain size, there are skills Art bottleneck;By taking Al-5Ti-1B grain refiner as an example, 0.2% Al-5Ti-1B is added usually into commercial-purity aluminium melt Commercial-purity aluminium as-cast grain size can be reduced to 200 μm or so by grain refiner, but as grain refiner additive amount continues Increase, crystallite dimension cannot continue to reduce, and crystallite dimension the limit occurs when reaching 120 μm or so.
In order to break through existing fining agent to the refinement limit of aluminium alloy as-cast grain size, need to research and develop highly efficient aluminium And its alloy grain refiner.
Summary of the invention
The purpose of the present invention is being directed to the above problem of existing Al-Ti-B grain refiner, a kind of aluminium and its conjunction are provided Gold Al-Nb-Cr-B grain refiner and preparation method thereof, breaks through existing Al-Ti-B grain refiner to aluminium alloy Refine the limit.
The present invention is achieved by the following technical solutions:
According to a first aspect of the present invention, a kind of aluminium is provided and its alloy Al-Nb-Cr-B grain refiner, crystal grain are thin Agent includes the component of following each weight content: 1.00-6.00%Nb, 1.00-3.00%Cr, 0.50-1.00%B, surplus For Al.
Preferably, in the Al-Nb-Cr-B grain refiner, Nb weight percentage can be 4.00- 6.00%, the detailed performance of grain refiner of the present invention can be preferably improved under this condition.
Preferably, in the Al-Nb-Cr-B grain refiner, Cr weight percentage can with 2.00-3.00%, The detailed performance of grain refiner of the present invention can be preferably improved under this condition.
According to a second aspect of the present invention, a kind of above-mentioned aluminium and its alloy Al-Nb-Cr-B grain refiner are provided Preparation method, steps are as follows:
(1) according to generation weight percent are as follows: 1.00-6.00%Nb, 1.00-3.00%Cr, 0.50-1.00%B, The amount of remaining Al weighs pure niobium, pure chromium, potassium fluoborate and commercial-purity aluminium respectively, and pure niobium, pure chromium and potassium fluoborate powder is equal Even mixing;
Preferably, the pure niobium grain diameter is 0.5-1.0 centimetres.
Preferably, the pure niobium grain diameter is 0.5-1.0 centimetres.
(2) the weighed commercial-purity aluminium of heating fusing institute;
Preferably, the weighed commercial-purity aluminium of the heating fusing institute, refer to: being warming up to 900-1200 DEG C will first be weighed Commercial-purity aluminium melted in resistance furnace.
(3) pure niobium prepared in (1), pure chromium and potassium fluoborate mixed powder are pressed into aluminum melt using graphite bell jar In;
(4) processing of continual ultrasonic wave is introduced on the aluminum melt top that pure niobium, pure chromium and potassium fluoborate mixed powder is added;
Preferably, the ultrasonic frequency is 20 ± 1kHz, power 500-5000W.
Preferably, the continual ultrasonic wave processing time is 1-20 minutes.
(5) make melt natural cooling, obtain Al-Nb-Cr-B grain refiner;
Preferably, described to make melt natural cooling, when being cooled to 700-720 DEG C, cast ingot shape Al-Nb-Cr- B grain refiner.
Compared with prior art, the invention has the following advantages:
Innovation of the invention is to be led to based on the cross reaction between each constituent element in Al-Nb-Cr-B quaternary system Cross Cr substitution NbB2In part Nb atom, thus in adjusting seed size fining agent boride and solidification Nucleation α-Al between lattice Mismatch;Apply high-energy ultrasonic vibration in fining agent preparation process simultaneously, increases the pure niobium of high-melting-point, pure chromium in aluminum melt It melts, shortens fining agent preparation time, improves boride particle distribution state, to obtain a kind of aluminium and its alloy with efficient Al-Nb-Cr-B grain refiner breaks through existing Al-Ti-B system grain refiner to the refinement limit of aluminium alloy.
Detailed description of the invention
By reading referring to the following drawings, other features, objects and advantages of the present invention will be become more apparent upon:
Commercial-purity aluminium metallographic macrograin tissue of the Fig. 1 without refinement;
Fig. 2 adds the commercial-purity aluminium metallographic macrograin tissue after 0.20% weight percent Al-5Ti-1B refinement;
Fig. 3 adds the commercial-purity aluminium metallographic after the refinement of 0.20% weight percent Al-Nb-Cr-B prepared by embodiment 4 Macrograin tissue.
Specific embodiment
The present invention is described in detail combined with specific embodiments below.Following embodiment will be helpful to the technology of this field Personnel further understand the present invention, but the invention is not limited in any way.It should be pointed out that the ordinary skill of this field For personnel, without departing from the inventive concept of the premise, various modifications and improvements can be made.These belong to the present invention Protection scope.
Embodiment
Following example 1-7 is implemented in accordance with the following steps:
(1) according to generation weight percent are as follows: 1.00-6.00%Nb, 1.00-3.00%Cr, 0.50-1.00%B, The amount of remaining Al weighs pure niobium, pure chromium, potassium fluoborate and commercial-purity aluminium respectively, and pure niobium, pure chromium and potassium fluoborate powder is equal Even mixing;
(2) 900-1200 DEG C is warming up to melt the weighed commercial-purity aluminium of institute in resistance furnace;
(3) prepared pure niobium, pure chromium and potassium fluoborate mixed powder are pressed into aluminum melt using graphite bell jar;
(4) it is in 20 ± 1kHz of aluminum melt top introducing, the power that pure niobium, pure chromium and potassium fluoborate mixed powder is added The ultrasonic wave of 500-5000W is persistently handled 1-20 minutes;
(5) make melt natural cooling, when being cooled to 700-720 DEG C, ingot shape Al-Nb-Cr-B crystal grain refinement of casting Agent.
Refinement: 500 grams of commercial-purity aluminiums, heating are melted to 720 DEG C, prepared according to the amount addition of 0.2 gram/100 grams aluminium Al-Nb-Cr-B quaternary grain refiner keeps the temperature 5 minutes, pours into Reynolds standard golf T-shaped mould, measures away from sample bottom surface Crystallite dimension at 51mm.
The parameter and implementation result of specific embodiment 1-7 see the table below:
The present invention is based on the cross reactions between each constituent element in Al-Nb-Cr-B quaternary system, substitute NbB by Cr2 In part Nb atom, thus in adjusting seed size fining agent boride and solidification Nucleation α-Al between lattice equations, break through Existing Al-Ti-B system grain refiner is to the refinement limit of aluminium alloy, for example that postindustrial fine aluminium is refined in above-described embodiment 4 is brilliant Particle size can achieve 100 μm.
As shown in Figure 1, being the commercial-purity aluminium metallographic macrograin tissue without refinement;
As shown in Fig. 2, brilliant for the commercial-purity aluminium metallographic macroscopic view after addition 0.20% weight percent Al-5Ti-1B refinement Grain tissue, wherein column crystal is obviously refined, and about 150 μm of the crystallite dimension after refinement.
Fig. 3 adds the commercial-purity aluminium metallographic after the refinement of 0.20% weight percent Al-Nb-Cr-B prepared by embodiment 4 Macrograin tissue, wherein compared to Fig. 2, grain refining effect is more excellent, and the crystallite dimension after refinement is 100 μm or so, breaks through The refinement limit of the Al-Ti-B system grain refiner to aluminium alloy.
It is discussed in detail although the contents of the present invention have passed through above preferred embodiment, but it should be appreciated that above-mentioned Description is not considered as limitation of the present invention.After those skilled in the art have read above content, for of the invention A variety of modifications and substitutions all will be apparent.Therefore, protection scope of the present invention should be limited to the appended claims.

Claims (7)

1. the preparation method of a kind of aluminium and its alloy Al-Nb-Cr-B grain refiner, it is characterised in that: steps are as follows:
(1) pure niobium, pure chromium, potassium fluoborate and commercial-purity aluminium are weighed respectively, and pure niobium, pure chromium and potassium fluoborate powder are uniformly mixed It closes;
(2) the weighed commercial-purity aluminium of heating fusing institute, obtains aluminum melt;
(3) pure niobium prepared in step (1), pure chromium and potassium fluoborate mixed powder are pressed into step (2) using graphite bell jar In obtained aluminum melt;
(4) it is introduced at continual ultrasonic wave in the aluminum melt top that pure niobium, pure chromium and potassium fluoborate mixed powder is added in step (3) Reason;
(5) make melt natural cooling, obtain Al-Nb-Cr-B grain refiner;
The component of each weight content of the Al-Nb-Cr-B grain refiner are as follows: 4.00-6.00%Nb, 2.00-3.00% Cr, 0.50-1.00%B, surplus Al.
2. the preparation method of Al-Nb-Cr-B grain refiner according to claim 1, characterized in that step (2) In, the weighed commercial-purity aluminium of the heating fusing institute refers to: being warming up to 900-1200 DEG C for the weighed commercial-purity aluminium of institute in electricity It is melted in resistance furnace.
3. the preparation method of Al-Nb-Cr-B grain refiner according to claim 1, characterized in that step (4) In, the ultrasonic frequency is 20 ± 1kHz, power 500-5000W.
4. the preparation method of Al-Nb-Cr-B grain refiner according to claim 1, characterized in that step (4) In, the continual ultrasonic wave processing time is 1-20 minutes.
5. the preparation method of Al-Nb-Cr-B grain refiner according to claim 1, characterized in that step (5) In, it is described to make melt natural cooling, when being cooled to 700-720 DEG C, ingot shape Al-Nb-Cr-B grain refiner of casting.
6. the preparation method of Al-Nb-Cr-B grain refiner according to claim 1-5, characterized in that The pure niobium grain diameter is 0.5-1.0 centimetres.
7. the preparation method of Al-Nb-Cr-B grain refiner according to claim 1-5, characterized in that The pure chromium grain diameter is 0.5-1.0 centimetres.
CN201611046981.9A 2016-11-23 2016-11-23 The preparation method of aluminium and its alloy Al-Nb-Cr-B grain refiner Active CN106498201B (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108251675B (en) * 2017-12-26 2020-04-03 上海大学 Al-Ti-Nb-B refiner for casting aluminum-silicon alloy and preparation method and application thereof
CN113862534B (en) * 2021-10-08 2022-07-29 上海交通大学 Method for regulating and controlling tissue inheritance of aluminum alloy material and method for preparing 7085 aluminum alloy thick plate

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1605642A (en) * 2004-11-18 2005-04-13 上海交通大学 Method for preparing Al-Ti-B grain refiner
CN101294247A (en) * 2007-04-26 2008-10-29 中南大学 Aluminum alloy refiner and aluminum alloy produced with the refiner
CN102703738A (en) * 2012-05-17 2012-10-03 上海交通大学 Preparation method of Al-Ti-B-C quaternary grain refiner
CN103146965A (en) * 2011-12-06 2013-06-12 贵州华科铝材料工程技术研究有限公司 Cr(CO)6 modified low-zinc hot-dip aluminum alloy coating material
CN103667759A (en) * 2013-12-27 2014-03-26 江苏中联铝业有限公司 Al-Mg-Si alloy alpha-Al grain refiner and preparation method thereof
CN105648250A (en) * 2015-12-31 2016-06-08 北京航空航天大学 Low-cooling-rate-sensitivity high-nucleation-capability AlNbBRE refiner for cast aluminum alloy and preparation method of refiner

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1605642A (en) * 2004-11-18 2005-04-13 上海交通大学 Method for preparing Al-Ti-B grain refiner
CN101294247A (en) * 2007-04-26 2008-10-29 中南大学 Aluminum alloy refiner and aluminum alloy produced with the refiner
CN103146965A (en) * 2011-12-06 2013-06-12 贵州华科铝材料工程技术研究有限公司 Cr(CO)6 modified low-zinc hot-dip aluminum alloy coating material
CN102703738A (en) * 2012-05-17 2012-10-03 上海交通大学 Preparation method of Al-Ti-B-C quaternary grain refiner
CN103667759A (en) * 2013-12-27 2014-03-26 江苏中联铝业有限公司 Al-Mg-Si alloy alpha-Al grain refiner and preparation method thereof
CN105648250A (en) * 2015-12-31 2016-06-08 北京航空航天大学 Low-cooling-rate-sensitivity high-nucleation-capability AlNbBRE refiner for cast aluminum alloy and preparation method of refiner

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