CN109971981A - A kind of high evenness Al-TiB2 intermediate alloy preparation method - Google Patents

A kind of high evenness Al-TiB2 intermediate alloy preparation method Download PDF

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Publication number
CN109971981A
CN109971981A CN201910318931.9A CN201910318931A CN109971981A CN 109971981 A CN109971981 A CN 109971981A CN 201910318931 A CN201910318931 A CN 201910318931A CN 109971981 A CN109971981 A CN 109971981A
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intermediate alloy
tib
tio
high evenness
preparation
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陈子勇
王洪达
王汉光
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Dalian Ke Tianxin Material Co Ltd
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Dalian Ke Tianxin Material Co Ltd
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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
    • C22C1/03Making non-ferrous alloys by melting using master alloys
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/10Alloys containing non-metals
    • C22C1/1036Alloys containing non-metals starting from a melt
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/10Alloys containing non-metals
    • C22C1/1036Alloys containing non-metals starting from a melt
    • C22C1/1047Alloys containing non-metals starting from a melt by mixing and casting liquid metal matrix composites
    • C22C1/1052Alloys containing non-metals starting from a melt by mixing and casting liquid metal matrix composites by mixing and casting metal matrix composites with reaction
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C21/00Alloys based on aluminium
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C32/00Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
    • C22C32/0047Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents
    • C22C32/0073Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents only borides

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Composite Materials (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Powder Metallurgy (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)

Abstract

A kind of high evenness Al-TiB2Intermediate alloy preparation method belongs to intermediate alloy technical field.Mass percent component, Ti:8.0-12.0%, B:3.0-5.0%, surplus Al;Ti/B=1/2, object phase composition include α-Al, TiB2.H is weighed as required3BO3、TiO2, aluminium powder, titanium valve, aluminium ingot, the molar ratio of intermediate alloy ingredient is Ti/B=1/4, Ti/TiO2=2/3, aluminium ingot purity 99.9%;First by TiO2、H3BO3It is uniformly mixed, 300 DEG C of two hours of heating;Powder after heating is placed in mold with aluminium powder mixing, is pressed into block;Aluminium ingot is heated and is melted, ice crystal is covered;Melt is heated up, block is pressed into, to after the reaction was completed, stirring is classified at 700 DEG C to 900 DEG C, is pressed into C2Cl6Refining, skims, and is poured.The present invention utilizes low cost feedstock, the high evenness TiB of preparation2Grain diameter degree is 1 μm.

Description

A kind of high evenness Al-TiB2 intermediate alloy preparation method
Technical field
The invention belongs to technical field of composite materials, in particular to a kind of high evenness Al-TiB2Intermediate alloy preparation side Method.
Background technique
The widely applied Al-TiB of aluminum i ndustry at present2Intermediate alloy still faces some technical problems, is mainly reflected in particle Content is low, and degree of purity is poor, and the second phase size, pattern and distribution are sub-standard etc..Industrially pass through villiaumite reaction method at present A large amount of preparation Al-TiB2Intermediate alloy, typical production process are: K is added into aluminum melt at 750-850 DEG C2TiF6With KBF4, it is reacted sufficiently by mechanical stirring, prepares Al-TiB2Intermediate alloy.The Al-TiB prepared using villiaumite reaction method2 TiAl is not contained in intermediate alloy tissue3Phase, the TiB in tissue2Particle be in aggregation bulk exist, agglomerated masses internal particle with Particle is sticked together, imaging material application, while generating serious pollution problem.In order to prepare excellent Al-TiB2In Between alloy, attempted various means both at home and abroad for example, conventional ceramic technique, self-propagating high-temperature synthetic method etc., are primarily present particle aggregation Seriously, the disadvantages of preparation cost is high.
Summary of the invention
The present invention uses melt self-spread synthesizing method, utilizes raw material sources low-cost TiO extensively2、H3BO3, develop one Kind granule content is high, size is small, the Al-TiB of high uniformity distribution2Intermediate alloy.
To solve the above problems, this patent main technical schemes are as follows: utilize melt self-spread synthesizing method preparation process, preparation A kind of high evenness Al-TiB2Intermediate alloy.
A kind of high evenness Al-TiB2Intermediate alloy, comprising following mass percent component, Ti:8.0-12.0%, B: 3.0-5.0%, surplus Al;Ti/B=1/2, object phase composition include α-Al, TiB2。TiB2Grain diameter degree is at 1 μm hereinafter, height It is uniformly distributed.
The preparation method of above-mentioned intermediate alloy, which is characterized in that Ti and B is with the addition of oxide powder shape, certainly using melt Synthetic method preparation is spread, specifically includes the following steps:
(1) raw material preparation weighs H as required3BO3、TiO2, aluminium powder, aluminium ingot, it is desirable that Al-TiB2The molar ratio of intermediate alloy ingredient Are as follows: Ti/B=1:4, Ti/TiO2=2:3, aluminium ingot purity 99.9%;
(2) by H3BO3、TiO2It is uniformly mixed, in 300 DEG C of two hours of heating, dispels moisture;
(3) by the TiO after heating2、H3BO3It is uniformly mixed, uniformly mixed powder is placed in mold, briquet with aluminium powder Body;
(4) aluminium ingot is heated to 780-800 DEG C using well formula resistance furnace, is completely melt to aluminium ingot, cover one layer of ice crystal covering Agent;Melt is warming up to 900-1000 DEG C, graphite bell jar is pressed into the block of step (3), using mixing plant 700-900 DEG C into Row classification stirring 10min;After the reaction was completed, 5 min are stood, C is pressed into2Cl6Refining, skims, aluminum melt is poured into warmed-up In 250 DEG C of punching block, Al-TiB is obtained2Intermediate alloy.
Above-mentioned preferred ice crystal and C2Cl6In 100 DEG C of heating 1h, moisture removal is removed;By mold and the tools such as spoon brushing one of skimming Coating prevents Fe impurity element from polluting intermediate alloy.Intermediate frequency furnace is selected to carry out melting, graphite rod stirring prevents Si's Pollution.
H3BO3And TiO2300 DEG C of mixture two hours of heating, by the TiO after heating2、H3BO3It is uniformly mixed with aluminium powder, The powder agglomates volume of compacting is by 120 × Φ 80mm3Change to 70 × Φ 80mm3, cannot excessively consolidation.
Aluminum melt reaches certain temperature, is pressed into powder agglomates, carries out classification stirring at 700-900 DEG C using mixing plant, make it Combustion reaction occurs.
The utility model has the advantages that the present invention solves, conventional method particle aggregation is serious, the high problem of preparation cost, in intermediate alloy TiB2Particle size is small, high uniformity distribution.
Detailed description of the invention
Fig. 1 is Al-TiB2Intermediate alloy microscopic structure.
Specific embodiment
Embodiment 1
Melt self-spread synthesizing method prepares Al-TiB2Intermediate alloy process is as follows:
1. raw material preparation, Al-TiB2Intermediate alloy is by H3BO3、TiO2, aluminium powder, aluminium ingot, C2Cl6It is prepared with ice crystal coverture, Middle aluminium ingot purity 99.9%.
2. preparing the Al-TiB of 1Kg2Intermediate alloy weighs H as required3BO3、TiO2, aluminium powder, aluminium ingot, aluminium burn out rate is 3%.It is required that Al-TiB2The molar ratio of intermediate alloy ingredient are as follows: Ti/B=1:4, Ti/TiO2=2:3。
3 by H3BO3、TiO2Powder dispels moisture in 300 DEG C of two hours of heating.
4. titanium valve, aluminium powder, boron powder are uniformly mixed, uniformly mixed powder is placed in mold, 70 × Φ is pressed into 80mm3Cylindricality powder agglomates.
5. preventing Fe impurity element from polluting intermediate alloy on mold and one coating of the tools such as spoon brushing of skimming.In selection Frequency induction furnace carries out melting, and graphite rod stirring prevents the pollution of Si.
6. clean aluminium ingot is heated to 780 DEG C using intermediate frequency furnace, it is completely melt to aluminium ingot, covers one layer of ice crystal Stone prevents the oxidation and air-breathing of aluminium;Furnace temperature is risen to 900 DEG C again, the cylindricality powder agglomates suppressed in advance is pressed into aluminium by graphite bell jar Melt carries out classification stirring 10min using mixing plant at 700-900 DEG C;The C of 3%wt is added2Cl6Refining degasification is carried out, is stood 5min;The slag and oxide skin on surface are removed with spoon of skimming;720 DEG C are reduced to temperature, is poured into warmed-up 250 DEG C of punching blocks; The Al-TiB of this method preparation2Intermediate alloy, particle size is small, and distribution height is uniform.
Embodiment 2:
Difference from Example 1 is, after block is added, in 700-900 DEG C of progress 5min-30min stirring, when preferably stirring Between be 10min, be poured into after isothermal holding in the metal type dies of 250 DEG C of preheating.It can reach with this condition and 1 phase of embodiment Same preparation effect.
Embodiment 3:
Difference from Example 1 is that block after the reaction was completed, is kept the temperature at 700-750 DEG C, and preferably holding temperature is It 720 DEG C, is poured into after isothermal holding in the metal type dies of 250 DEG C of preheating.It can reach with this condition same as Example 1 Prepare effect.

Claims (7)

1. a kind of high evenness Al-TiB2Intermediate alloy, which is characterized in that include following mass percent component, Ti:8.0- 12.0%, B:3.0-5.0%, surplus Al;Molar ratio is Ti:B=1:2, and the object phase composition of intermediate alloy includes α-Al, TiB2Phase.
2. a kind of high evenness Al-TiB described in accordance with the claim 12Intermediate alloy, which is characterized in that TiB2Particle size exists 1 μm hereinafter, high uniformity is distributed.
3. a kind of high evenness Al-TiB described in accordance with the claim 12Intermediate alloy, which is characterized in that the intermediate alloy is adopted It is prepared with melt self-spread synthesizing method.
4. a kind of high evenness Al-TiB2The preparation method of intermediate alloy, which is characterized in that Ti and B add in the form of the oxide Enter, is prepared using melt self-spread synthesizing method, specifically includes the following steps:
(1) raw material preparation weighs H as required3BO3、TiO2, aluminium powder, titanium valve, aluminium ingot, it is desirable that Al-TiB2Intermediate alloy ingredient is rubbed That ratio are as follows: Ti/B=1:4, Ti/TiO2=2:3, aluminium ingot purity 99.9%;
(2) first by proportioned H3BO3And TiO2In 300 DEG C of two hours of heating, moisture is dispelled;
(3) by TiO2、H3BO3, aluminium powder be uniformly mixed, uniformly mixed powder is placed in mold, block is pressed into;
(4) aluminium ingot is heated to 780-800 DEG C using well formula resistance furnace, is completely melt to aluminium ingot, cover one layer of ice crystal covering Agent;Melt is warming up to 900-1000 DEG C, graphite bell jar is pressed into the block of step (3), using mixing plant 700-900 DEG C into Row classification stirring 10min;After the reaction was completed, 5 min are stood, C is pressed into2Cl6Refining, skims, aluminum melt is poured into warmed-up In 250 DEG C of punching block, Al-TiB is obtained2Intermediate alloy.
5. a kind of high evenness Al-TiB according to claim 42The preparation method of intermediate alloy, which is characterized in that step (2) in, H3BO3And TiO2300 DEG C of mixture two hours of heating.
6. a kind of high evenness Al-TiB according to claim 42The preparation method of intermediate alloy, which is characterized in that by mould Have and one coatings of tools brushing such as spoon of skimming, prevent Fe impurity element from polluting intermediate alloy, intermediate frequency furnace is selected to be melted Refining, graphite rod stirring, prevents the pollution of Si.
7. a kind of high evenness Al-TiB according to claim 42The preparation method of intermediate alloy, which is characterized in that step (3) in, the powder agglomates volume of compacting is by 120 × Φ 80mm3Change to 70 × Φ 80mm3
CN201910318931.9A 2019-04-19 2019-04-19 A kind of high evenness Al-TiB2 intermediate alloy preparation method Withdrawn CN109971981A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5484493A (en) * 1993-06-02 1996-01-16 Kb Alloys, Inc. Aluminum base alloy
JP2009515041A (en) * 2005-11-02 2009-04-09 トゥビタク Method for producing grain refined mother alloy
CN103276253A (en) * 2013-04-18 2013-09-04 北京工业大学 Low-cost Al-Ti-B refiner and preparation method thereof
CN105671350A (en) * 2015-03-19 2016-06-15 中信戴卡股份有限公司 Aluminum alloy refiner, preparation method therefor and use thereof
CN107190161A (en) * 2017-05-12 2017-09-22 北京工业大学 A kind of Al TiB of large volume fraction2Pure phase intermediate alloy and preparation method

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5484493A (en) * 1993-06-02 1996-01-16 Kb Alloys, Inc. Aluminum base alloy
JP2009515041A (en) * 2005-11-02 2009-04-09 トゥビタク Method for producing grain refined mother alloy
CN103276253A (en) * 2013-04-18 2013-09-04 北京工业大学 Low-cost Al-Ti-B refiner and preparation method thereof
CN105671350A (en) * 2015-03-19 2016-06-15 中信戴卡股份有限公司 Aluminum alloy refiner, preparation method therefor and use thereof
CN107190161A (en) * 2017-05-12 2017-09-22 北京工业大学 A kind of Al TiB of large volume fraction2Pure phase intermediate alloy and preparation method

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