CN109825736A - A kind of Al-Ti-B refiner and preparation method thereof - Google Patents

Abstract

A kind of Al-Ti-B refiner and preparation method thereof, belongs to fining agent technical field.Mass percent component, Ti:8.0-12.0%, B:3.0-5.0%, surplus Al；Molar ratio=1/2 Ti/B, object phase composition include α-Al, TiB₂.H is weighed as required₃BO₃、TiO₂, aluminium powder, aluminium ingot, the molar ratio of fining agent 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；By after heating powder and aluminium powder mix be placed in mold, be pressed into block；Aluminium ingot is heated and is melted, ice crystal is covered；Melt is heated up, block is pressed into, is stirred to react, is pressed into C₂Cl₆Refining, skims, and casts.The present invention utilizes low cost feedstock, the TiB of preparation₂Size is less than 1 μm.

Description

A kind of Al-Ti-B refiner and preparation method thereof

Technical field

The invention belongs to fining agent technical field, in particular to a kind of inexpensive fining agent preparation method.

Background technique

The widely applied fining agent of aluminum i ndustry is Al-Ti-B intermediate alloy wire rod at present, due to working condition and technology water Flat backwardness causes product and imported product there are also a certain distance, is mainly reflected in that B content is low, and degree of purity is poor, the second phase ruler Very little, pattern and distribution are sub-standard etc..Meanwhile containing TiAl in most of Al-Ti-B refiner₃Object phase, may be to part Certain elements in alloy pollute.Al-Ti-B intermediate alloy, allusion quotation are largely industrially prepared by villiaumite reaction method at present Type production technology is: K is added into aluminum melt at 750-850 DEG C₂TiF₆And KBF₄, it is reacted sufficiently by mechanical stirring, Prepare Al-Ti-B refiner.Contain TiAl in Al-Ti-B intermediate alloy tissue using the preparation of villiaumite reaction method₃Phase, in tissue TiB₂Particle is in that aggregation bulk exists more, and agglomerated masses internal particle is sticked together with particle, and refining efficiency is low, generates simultaneously Serious pollution problem.In order to prepare efficient Al-Ti-B refiner, various means have been attempted both at home and abroad for example, oxide Method, self-propagating high-temperature synthesis etc. are primarily present the disadvantages of preparation efficiency is not high, and preparation cost is high.This experiment utilizes melt certainly Sprawling building-up reactions method has successfully prepared cost-efficiently Al-Ti-B refiner.

Summary of the invention

The present invention uses melt self-propagating synthesis reaction method, utilizes low-cost TiO from a wealth of sources₂、H₃BO₃For former material Material develops a kind of stabilization, long-acting, efficient, clean Al-Ti-B refiner.

To solve the above problems, this patent main technical schemes are as follows: melt self-propagating synthesis reaction method preparation process is utilized, Prepare a kind of Low-cost Al-Ti-B refiner.

Al-Ti-B refiner includes following mass percent, Ti:8.0-12.0%, B:3.0-5.0%, surplus Al； Molar ratio=1/2 Ti/B, object phase composition include α-Al, TiB₂.Fining agent TiB₂Particle size is at 1 μm hereinafter, being evenly distributed.It is thin Change ability is apparently higher than traditional Al-Ti-B refiner, and preparation process is simple, low in cost.

The preparation method of above-mentioned fining agent, which is characterized in that Ti and B is with the addition of oxide powder shape, using melt from climing Prolong building-up reactions method preparation, 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 fining agent ingredient Are as follows: Ti/B=1:4, Ti/TiO₂=2:3, wherein 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), and graphite rod uniform stirring reacts 10min； After the reaction was completed, 5 min are stood, C is pressed into₂Cl₆Refining, skims, aluminum melt is poured into warmed-up 250 DEG C of punching block, obtains Al-Ti-B refiner.

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 fining agent.Graphite crucible is selected to carry out melting, graphite rod stirring prevents the pollution of Si.

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, and uniform stirring brings it about combustion reaction.

The present invention solves the problem of conventional method preparation is difficult, and preparation cost is done, TiAl in fining agent₃、TiB₂Particle ruler It is very little small, it is evenly distributed, improves refining efficiency.

Detailed description of the invention

Fig. 1 is Low-cost Al-Ti-B refiner microscopic structure.

Specific embodiment

Below with reference to embodiment, the invention will be further described, but the present invention is not limited to following embodiments.

Embodiment 1

It is as follows that melt self-propagating synthesis reaction method prepares Al-5Ti-1B fining agent process:

1. raw material preparation, fining agent is by H₃BO₃、TiO₂, aluminium powder, aluminium ingot, C₂Cl₆It is prepared with ice crystal coverture, wherein aluminium ingot Purity 99.9%.

2. preparing the fining agent of 1Kg, H is weighed as required₃BO₃、TiO₂, aluminium powder, aluminium ingot, aluminium burn out rate be 3%.It is required that Al- TiB₂The molar ratio of fining agent ingredient are as follows: Ti/B=1:2, 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 fining agent on mold and one coating of the tools such as spoon brushing of skimming.Select graphite Crucible carries out melting, and graphite rod stirring prevents the pollution of Si.

6. clean aluminium ingot is heated to 780 DEG C using well formula resistance 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, graphite rod uniform stirring bring it about combustion reaction, react 10min；3% C 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 cast in warmed-up 250 DEG C of punching blocks； The fining agent of this method preparation, particle size is small, and is evenly distributed.

Comparative example 1

1. raw material preparation, fining agent is by H₃BO₃、TiO₂, aluminium powder, aluminium ingot, C₂Cl₆It is prepared with ice crystal coverture, wherein aluminium ingot Purity 99.9%.

2. preparing the fining agent of 500g, H is weighed as required₃BO₃、TiO₂, aluminium powder, aluminium ingot, aluminium burn out rate be 3%.It is required that Al-TiB₂The molar ratio of fining agent 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, 90 × Φ is pressed into 80mm³Cylindricality powder agglomates.

5. clean aluminium ingot is heated to 780 DEG C using well formula resistance 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 950 DEG C, graphite bell jar melts the cylindricality powder agglomates suppressed in advance indentation aluminium Body, graphite rod uniform stirring bring it about combustion reaction, react 10min；3% C 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 cast in warmed-up 250 DEG C of punching blocks, Obtain fining agent ingot casting.

Claims (6)

1. a kind of Al-Ti-B refiner, which is characterized in that comprising following mass percent component, Ti:8.0-12.0%, B: 3.0-5.0%, surplus Al；Molar ratio=1/2 Ti/B, the object phase composition of fining agent include α-Al, TiB₂Phase.

2. a kind of Al-Ti-B refiner according to claim 1, which is characterized in that TiB₂Particle size is at 1 μm hereinafter, dividing Cloth is uniform.

3. a kind of Al-Ti-B refiner according to claim 1, it is characterised in that fining agent uses melt self-propagating synthesis Reaction method preparation.

4. a kind of preparation method of Al-Ti-B refiner, which is characterized in that Ti and B are added in the form of the oxide, using melt The preparation of self-propagating synthesis reaction method, 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 fining agent ingredient are as follows: Ti/B=1:4, Ti/TiO₂=2:3, wherein 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), and graphite rod uniform stirring reacts 10min； After the reaction was completed, 5 min are stood, C is pressed into₂Cl₆Refining, skims, aluminum melt is cast in warmed-up 250 DEG C of punching block, obtains Al-Ti-B refiner.

5. a kind of preparation method of Al-Ti-B refiner according to claim 4, which is characterized in that by mold and skim Spoon brushes a coating, prevents Fe impurity element from polluting fining agent, and graphite crucible is selected to carry out melting, and graphite rod stirring prevents The pollution of Si.

6. a kind of preparation method of Al-Ti-B refiner according to claim 4, which is characterized in that the powder agglomates body of compacting Product is by 120 × Φ 80mm³Change to 70 × Φ 80mm³。