CN109797318A - It is a kind of to prepare Al3The method of Ti enhancing alumina-base material - Google Patents
It is a kind of to prepare Al3The method of Ti enhancing alumina-base material Download PDFInfo
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Abstract
Al is prepared the present invention relates to a kind of3The method of Ti enhancing alumina-base material adds the fluoride of titanyl compound or titanium into molten aluminum at 920-1000 DEG C, using metallic aluminium as reducing agent, thermite reaction 0.5-2h occurs, the titanium restored during aluminothermic reduction further generates Al with reactive aluminum3Ti, Al3Ti enters molten aluminum, and is uniformly distributed, and forms Al3Ti enhances alumina-base material.This method shortens process flow, reduces preparation cost, and impurity content is also greatly reduced, improves the comprehensive performance of alumina-base material.Al3Ti enhances that clean interfaces of the particle with matrix in conjunction with, pollution-free, compatibility is good, and interface bond strength height, mechanical property and polishing machine have a greater degree of improvement, and Al3Ti enhancing particle is ordered into phase, shows high-intensitive and elasticity modulus.Furthermore also there is good anti-oxidant and corrosion resistance in fluoride atmosphere of the intermetallic phase more than aluminium fusing point.
Description
Technical field
The present invention relates to metal smelts to extract field, in particular to is prepared in industrial aluminium electrolysis process using aluminothermic reduction
Al3The method of Ti particle-reinforced aluminum based alloy.
Background technique
The characteristics such as aluminium is small with specific gravity, intensity is high, electrical and thermal conductivity performance is excellent, corrosion resistance is high and in communications and transportation, electricity
The various aspects such as power, machine-building, building materials and packaging are widely applied, and have become a kind of not replaceable metal material.
China's aluminium yield over the years is at the forefront in the world, and product is mainly distributed on cold-rolled products, aluminum profile, is related to high added value alloy material portion
Divide few.
Metal-base composites is with a wide range of applications in other structures engineering material.It generally includes Metal Substrate
Body and with reinforcement existing for particle, whisker or fibers form.These materials have the comprehensive performance of its constituent, because
This, can be customized, to provide better performance according to different engine requests.Metal Substrate particle reinforced composite materials respectively to
The same sex, microscopic structure is uniform, and enhancing particle is at low cost, and preparation process is relatively easy, is easy to be mass produced, it has also become most send out
One of the material of exhibition prospect.
Metal Substrate particle reinforced composite materials are using metal and its alloy as matrix, and ceramic particle or intermetallic compound are
The synthetic material of reinforcement.Basis material bears and transmits various load, fixed bonding reinforcement；Enhancing particle compensates for
Metal matrix material intensity, wear-resisting property, in terms of deficiency.In metal-base composites, with aluminium and its
Alloy is that the composite material research of matrix is more early, and specific strength is high, and plasticity is good, is easy to secondary operation, is widely used.And
Titanium-Al series metal compounds have many features such as: density is small, specific strength is high, high rigidity, high-melting-point, wherein Al3Ti is due to close
Spend minimum, specific strength highest and high intensity, elasticity modulus, good high-temperature oxidation resistance and generally pushed away by researcher
It is high, it is ideal lightweight high-temperature structural material.
The interface state of metallic matrix and enhancing particle determines the performance of composite material.Not according to the source of enhancing particle
Together, additional enhancing particle aluminum matrix composite and in-situ authigenic enhancing particle aluminum matrix composite can be divided into.The table of additional particle
Face is easy to pollute, and poor with the wetability of matrix, interface binding power is poor, seriously reduces the performance of composite material.And original position is certainly
Raw particle is generated by chemically reacting in matrix, clean surface, good with the wetability of matrix, and size is small, is had excellent high temperatures
Energy, wear-resisting property and mechanical performance.
Aluminum matrix composite industrially is prepared frequently with powder metallurgy process, powder processed, mixing, granulation, molding, burning need to be undergone
Knot and etc., process is tedious, high production cost.Additionally due to be formed by interface easy for the low wetability of enhancing particle and liquid aluminium
It is oxidized or destroys, seriously affect the comprehensive performance of composite material.And original position synthesis particle enhancing metal-base composites is logical
Reacting between the element in system or between element and compound is crossed, one or more of high rigidity, high resiliency mould are generated in system
The ceramics or intermetallic compound of amount as reinforced phase, to achieve the purpose that strengthen parent metal, its main feature is that enhancing body surface
Face is pollution-free, Dispersed precipitate, good with matrix compatibility.
Summary of the invention
In view of the above-mentioned problems existing in the prior art, the object of the present invention is to provide a kind of industrial aluminum electrolytic preparation Al3Ti
Enhance the method for alumina-base material.
To achieve the above object, the present invention adopts the following technical scheme: a kind of prepare Al3The side of Ti enhancing alumina-base material
Method, it is characterised in that: at 920-1000 DEG C, the fluoride of titanyl compound or titanium is added into molten aluminum, is reduction with metallic aluminium
Agent, occurs thermite reaction 0.5-2h, and the titanium restored during aluminothermic reduction further generates Al with reactive aluminum3Ti, Al3Ti
It into molten aluminum, and is uniformly distributed, forms Al3Ti enhances alumina-base material.
As an improvement, the Al3Ti, which enhances in alumina-base material, contains 2%≤Al by percent by volume3Ti≤25%。
As an improvement, the quality of the titanyl compound and molten aluminum mass ratio are 1% ~ 30%；The fluoride of the titanium with
Molten aluminum mass ratio is 2% ~ 70%.
As an improvement, the oxide is TiO2, the fluoride of the titanium is Na2TiF6 Or K2TiF6。
As an improvement, the TiO2Quality and molten aluminum mass ratio be 1.5% ~ 25%；The Na2TiF6 Quality and aluminium
Liquid mass ratio is 4% ~ 55%；The K2TiF6 Quality and molten aluminum mass ratio be 4.5% ~ 65%.
It is a kind of to prepare Al3The method that Ti enhances alumina-base material, using ice crystal ground mass fused salt as solvent, aluminium oxide is solute progress
It is electrolysed aluminium processed, the fluoride of titanyl compound or titanium is added in Xiang Bingjing ground mass fused salt, is also with metallic aluminium at 920-1000 DEG C
Former agent, occurs thermite reaction 0.5-2h, and the titanium restored during aluminothermic reduction further generates Al with reactive aluminum3Ti,
Al3Ti enters molten aluminum, and is uniformly distributed, and alloy and ice crystal ground mass fused salt are automatically separated, and obtains Al3Ti reinforced aluminum matrix composites.
As an improvement, the Al3Ti, which enhances in alumina-base material, contains 2%≤Al by percent by volume3Ti≤25%。
As an improvement, the ratio between the quality of the titanyl compound and quality of alumina are 0.5% ~ 20%；The fluorination of the titanium
The ratio between object and quality of alumina are 2% ~ 40%.
As an improvement, the oxide is TiO2, the fluoride of the titanium is Na2TiF6 Or K2TiF6。
As an improvement, the TiO2Quality and the ratio between quality of alumina be 0.7% ~ 15%；The Na2TiF6 Quality with
The ratio between quality of alumina is 2% ~ 30%；The K2TiF6 Quality and the ratio between quality of alumina be 2% ~ 35%.
Compared with the existing technology, the present invention at least has the advantages that
1, the present invention prepares aluminium base Al using aluminothermic reduction3Ti enhances composite material, passes through the in-situ preparation Al in molten aluminum3Ti increases
Qiang Xiang, reinforced phase is evenly distributed, size is tiny, some is up to nanoscale.
2、Al3Ti enhances that clean interfaces of the particle with matrix in conjunction with, pollution-free, compatibility is good, interface bond strength height,
Mechanical property and polishing machine have a greater degree of improvement, and avoid tradition preparation composite process and are easily formed in interface
Brittle layer reduces the strength of materials, influences aluminum matrix composite comprehensive performance.
3、Al3Ti enhancing particle is ordered into phase, shows high-intensitive and elasticity modulus (~220 GPa).Furthermore intermetallic phase
Also there is good anti-oxidant and corrosion resistance in fluoride atmosphere more than aluminium fusing point.
4, the method for the present invention shortens process flow, reduces preparation cost, while impurity content is greatly reduced, and improves aluminium base
The comprehensive performance of material.
Detailed description of the invention
Fig. 1 is that embodiment 2 prepares Al3Ti enhances the flow chart of the method for alumina-base material.
Fig. 2 is a kind of Al of form3Ti reinforced aluminum matrix composites crystal phase photo.
Fig. 3 is the Al of another form3Ti reinforced aluminum matrix composites crystal phase photo.
Specific embodiment
Invention is further described in detail below.
Embodiment 1: referring to figs. 2 and 3, a kind of to prepare Al3The method that Ti enhances alumina-base material, at 920-1000 DEG C, to
Using metallic aluminium as reducing agent thermite reaction 0.5-2h, aluminothermy occur for the fluoride that titanyl compound or titanium are added in molten aluminum
The titanium restored in reduction process further generates Al with reactive aluminum3Ti, Al3Ti enters molten aluminum, and is uniformly distributed, and forms Al3Ti increases
Strong alumina-base material.When it is implemented, reduction reaction temperature can choose 920 DEG C, and 930 DEG C, 940 DEG C, 950 DEG C, 960 DEG C, 970
DEG C, 980 DEG C, 990 DEG C or 1000 DEG C, the recovery time can choose 0.5h, 0.8h, 1.0h, 1.2h, 1.4h, 1.5h, 1.6h,
1.8h or 2h.
The Al3Ti, which enhances in alumina-base material, contains 2%≤Al by percent by volume3Ti≤25%.Specifically, Al3Ti enhances aluminium
Al in sill3The percent by volume of Ti can choose the above-mentioned model of 2%, 5%, 8%, 10%, 13%, 15%, 18%, 20%, 22% or 25%
Enclose interior Al3Ti enhancing alumina-base material all has excellent comprehensive performance.
The quality and molten aluminum mass ratio of the titanyl compound are 1% ~ 30%；The fluoride of the titanium and molten aluminum quality it
Than being 2% ~ 70%, wherein the quality of titanyl compound and molten aluminum mass ratio specifically can choose 1%, 3%, 5%, 8%, 10%, 12%,
15%, 18%, 20%, 25% or 30%, the fluoride of titanium and molten aluminum mass ratio specifically can choose 2%, 5%, 10%, 18%, 25%,
30%, 35%, 40%, 45%, 50%, 55%, 60%, 65% or 70%, when it is implemented, can be according to Al3Ti enhances in alumina-base material
Al3The percent by volume of Ti adjusts the dosage of the fluoride of titanyl compound or titanium and adds number.
The oxide is TiO2, the fluoride of the titanium is Na2TiF6 Or K2TiF6。TiO2Quality and molten aluminum quality
The ratio between be 1.5% ~ 25%；The Na2TiF6 Quality and molten aluminum mass ratio be 4% ~ 55%；The K2TiF6 Quality and molten aluminum
Mass ratio is 4.5% ~ 65%.TiO2Quality and molten aluminum mass ratio specifically can choose 1.5%, 5%, 10.5%, 15%,
15.5%, 18.5%, 20% or 25%；Na2TiF6 Quality and molten aluminum mass ratio specifically can choose 4%, 8%, 12%, 18%,
20%, 25%, 30%, 35%, 40%, 45%, 50% or 55%；K2TiF6 Quality and molten aluminum mass ratio specifically can choose 4.5%,
8.5%, 15%, 20.5%, 24%, 29.5%, 35%, 40.5%, 45.5%, 55%, 60% or 65%.
The method of the present invention restores TiO by thermit reduction2、Na2TiF6 、K2TiF6Equal titanyl compounds or fluoride,
Because of molten aluminum excess, resulting Ti can further be reacted with Al generates Al3Ti。
As an improvement, the molten aluminum is the production of Hall Heroult process (Hall-H é roult process) metal smelting aluminium
Metal aluminium liquid.The temperature of aluminum liquid that this method electrolysis production obtains can not have to heating i.e. at 920-1000 DEG C, save production
While cost, environmental protection is also helped, it is often more important that also simplify production technology.
The method that the present embodiment proposes carries out aluminothermic reduction by the fluoride to titanyl compound or titanium at high temperature,
Titanyl compound or fluoride are restored to obtain titanium, further by titanium and aluminium, the reaction was continued obtains Al3It is multiple that Ti enhances aluminium base
Condensation material, the method for the present invention process is simple, reduces energy consumption.
Embodiment 2: a kind of to prepare Al referring to Fig. 1 to Fig. 33Ti enhance alumina-base material method, be with ice crystal ground mass fused salt
Solvent, aluminium oxide (aluminium oxide, that is, Al in the present embodiment2O3) it is that solute carries out electrolysis aluminium processed, it is added in Xiang Bingjing ground mass fused salt
, using metallic aluminium as reducing agent, thermite reaction 0.5-2h occurs for the fluoride of titanyl compound or titanium at 920-1000 DEG C,
The titanium restored during aluminothermic reduction further generates Al with reactive aluminum3Ti, Al3Ti enters molten aluminum, and is uniformly distributed, by alloy
It is separated with ice crystal ground mass fused salt, obtains Al3Ti reinforced aluminum matrix composites.When it is implemented, reduction reaction temperature can choose
920 DEG C, 930 DEG C, 940 DEG C, 950 DEG C, 960 DEG C, 970 DEG C, 980 DEG C, 990 DEG C or 1000 DEG C, the recovery time can choose 0.5h,
0.8h, 1.0h, 1.2h, 1.4h, 1.5h, 1.6h, 1.8h or 2h.
The Al3Ti, which enhances in alumina-base material, contains 2%≤Al by percent by volume3Ti≤25%.Specifically, Al3Ti enhances aluminium
Al in sill3The percent by volume of Ti can choose the above-mentioned model of 2%, 5%, 8%, 10%, 13%, 15%, 18%, 20%, 22% or 25%
Enclose interior Al3Ti enhancing alumina-base material all has excellent comprehensive performance.When it is implemented, can be according to Al3Ti enhances aluminium base
Al in material3The percent by volume of Ti adjusts the dosage of the fluoride of titanyl compound or titanium and adds number, due to the present embodiment
In, the fluoride of titanyl compound or titanium can be added directly in electrolysis stage, in order to not influence electrolysis stage, titanyl compound
Or the fluoride of titanium is preferably added several times, such as can in three times, four times or five times addition.The quality of the titanyl compound
It is 0.5% ~ 20% with the ratio between quality of alumina；The ratio between fluoride and quality of alumina of the titanium are 2% ~ 40%.The matter of oxide
Amount and the ratio between quality of alumina specifically can choose 0.5%, 4.5%, 8%, 12.5%, 15%, 18.5% or 20%, fluoride and oxidation
Aluminium mass ratio specifically can choose 2%, 6%, 8%, 12%, 16%, 20%, 25%, 28%, 33%, 36% or 40%.
The oxide is TiO2, the fluoride of the titanium is Na2TiF6 Or K2TiF6.The TiO2Quality and oxidation
Aluminium mass ratio is 0.7% ~ 15%；The Na2TiF6 Quality and the ratio between quality of alumina be 2% ~ 30%；The K2TiF6 Matter
The ratio between amount and quality of alumina are 2% ~ 35%.
Specifically, TiO2Quality and the ratio between quality of alumina can choose 0.7%, 1.5%, 5%, 8.5%, 10%, 12%,
15%, Na2TiF6 Quality and the ratio between quality of alumina can choose 2%, 6%, 9%, 12%, 15%, 18%, 20%, 25%, 28% or
30%, K2TiF6 Quality and the ratio between quality of alumina can choose 2%, 6%, 9%, 12%, 15%, 18%, 20%, 25%, 28%, 30%
Or 35%.
The ingredient of the ice crystal ground mass fused-salt medium contains 70 ~ 85% Na according to weight percent3AlF6, 8 ~ 15%AlF3, 1 ~
3%Al2O3, 0 ~ 5%CaF2, 0 ~ 5%LiF, 0 ~ 5%MgF2, fused salt parameter CR is 2.0 ~ 2.8:1.The ice crystal ground mass fused-salt medium
Aluminium oxide/fluoaluminate that titanyl salt/titanium villiaumite and thermite reaction generate can be dissolved simultaneously.
It is electrolysed aluminium processed to refer to using ice crystal ground mass fused salt as solvent, aluminium oxide or fluorine aluminium salt are solute, are electrolysis yin with graphite
Anode, 920-1000 DEG C is electrolysed, the cathode of electrolytic process and anodic current density with current industrial aluminum electrolytic current density,
After the mixing of ice crystal ground mass fused salt, aluminium oxide and/or aluminum fluoride adds DC voltage, positively charged aluminium ion can be gathered in cathode
Near, aluminium ion acquisition is electronically generated pure aluminum, and oxonium ion then loses electronics near the anode made of graphite or coke, raw
At oxygen atom.At high temperature, oxygen atom and carbon generate carbon monoxide and carbon dioxide gas escapes electrolytic cell.
Since ice crystal ground mass molten salt system and metal aluminium liquid are there are biggish density contrast, can be good at separating metal
Molten aluminum and fused salt.Thermite reaction reacts in molten aluminum and ice crystal ground mass fused salt interface, and the Ti of generation enters in molten aluminum into one
Step forms Al3Ti, Al3Ti density is 3.366g/cm3, it is slightly larger than molten aluminum, Al3Ti enters in aluminium base, and distribution is more uniform,
And the Al generated2O3With Na3AlF6It is then gradually dissolved into ice crystal ground mass fused salt, alloy and the separation of ice crystal ground mass fused salt is (made
Standby rich Al3Ti enhances aluminium based metal melt and is discharged by aluminium flowing-out mouth, so that subsequent handling is handled), obtain Al3Ti enhancing
Aluminum matrix composite and Al2O3Or Na3AlF6, Al2O3Or Na3AlF6It may continue as industrial aluminium electroloysis raw material to be electrolysed, prepare
The higher metallic aluminium of purity out.
The Al of generation2O3With Na3AlF6It is then gradually dissolved into ice crystal ground mass fused salt, this is conducive to the subsequent aluminium in molten aluminum-interface
The progress of thermal reduction reaction, and in particular to reaction equation it is as follows:
1.5TiO2 + 2Al = 1.5Ti + Al2O3
1.5TiO2 + 6.5Al = 1.5Al3Ti + Al2O3
Na2TiF6 + Al = Al3Ti + Na3AlF6+NaF
At 1000 DEG C, TiO2Solubility in ice crystal is 4.87%, and Na2TiF6It can mutually be melted with cryolite-based system well
So that Ti ion is spread to molten aluminum-fused salt interface and then generates Al by aluminium reducing3Ti reinforced aluminum matrix composites.
The present invention is that titanium oxide/titanium fluorination is added into fused salt using existing industrial aluminum electrolysis production technique and equipment
Object carries out thermite reaction on interface, due to Al generated3Ti solubility in fused salt is low, in addition density and fused salt
Architectural difference is big, is able to achieve preferable separating effect.
Reduction process is that the titanium ion in liquid metal and fused salt reacts in ice crystal ground mass molten salt system, reduction reaction
Rate is fast, metal and fused salt good separating effect after reaction, and controlling titanium salt amount be added can be obtained different Al3The aluminium base of Ti content is multiple
Different Al can be obtained by control reaction and soaking time in condensation material3The aluminum matrix composite of Ti shape characteristic.
The aluminium oxide that fused salt after separation contains saturation can obtain the higher metallic aluminium of purity with Direct Electrolysis, and be generated
Cryolite can also serve as one of raw material of aluminium electroloysis, directly participation cell reaction.Powder is used compared with prior art
The method of metallurgy prepares Al3Ti reinforced aluminum matrix composites.Required process is greatly shortened, required temperature reduces, reduces
Energy consumption does not lose metallic aluminium and other raw material, and it is more excellent to restore resulting aluminum matrix composite purity high combination property
It is different.
Preparation Al in embodiment 23The method of Ti enhancing alumina-base material makes full use of existing aluminium electroloysis device to directly adopt
It is electrolysed molten aluminum reduction titanium salt generated, process is simple, reduces energy consumption, does not lose metallic aluminium, and it is higher to obtain purity
Al3Ti enhances alumina-base material.
Finally, it is stated that the above examples are only used to illustrate the technical scheme of the present invention and are not limiting, although referring to compared with
Good embodiment describes the invention in detail, those skilled in the art should understand that, it can be to skill of the invention
Art scheme is modified or replaced equivalently, and without departing from the objective and range of technical solution of the present invention, should all be covered at this
In the scope of the claims of invention.
Claims (10)
1. a kind of prepare Al3The method of Ti enhancing alumina-base material, it is characterised in that: at 920-1000 DEG C, titanium is added into molten aluminum
The fluoride of oxide or titanium occurs thermite reaction 0.5-2h, restores during aluminothermic reduction using metallic aluminium as reducing agent
Titanium further with reactive aluminum generate Al3Ti, Al3Ti enters molten aluminum, and is uniformly distributed, and forms Al3Ti enhances alumina-base material.
2. preparation Al as described in claim 13The method of Ti enhancing alumina-base material, it is characterised in that: the Al3Ti enhances aluminium
Contain 2%≤Al by percent by volume in sill3Ti≤25%。
3. preparation Al as claimed in claim 23The method of Ti enhancing alumina-base material, it is characterised in that: the titanyl compound
Quality and molten aluminum mass ratio be 1% ~ 30%；The fluoride and molten aluminum mass ratio of the titanium are 2% ~ 70%.
4. preparation Al as described in any one of claims 1-33The method of Ti enhancing alumina-base material, it is characterised in that: the oxidation
Object is TiO2, the fluoride of the titanium is Na2TiF6 Or K2TiF6。
5. preparation Al as claimed in claim 43The method of Ti enhancing alumina-base material, it is characterised in that: the TiO2Quality with
Molten aluminum mass ratio is 1.5% ~ 25%；The Na2TiF6 Quality and molten aluminum mass ratio be 4% ~ 55%；The K2TiF6 Matter
Amount is 4.5% ~ 65% with molten aluminum mass ratio.
6. a kind of prepare Al3The method of Ti enhancing alumina-base material, it is characterised in that: using ice crystal ground mass fused salt as solvent, aluminium oxide is
Solute carries out electrolysis aluminium processed, the fluoride of titanyl compound or titanium is added in Xiang Bingjing ground mass fused salt, at 920-1000 DEG C, with gold
Category aluminium is reducing agent, and thermite reaction 0.5-2h occurs, and the titanium restored during aluminothermic reduction is further generated with reactive aluminum
Al3Ti, Al3Ti enters molten aluminum, and is uniformly distributed, and alloy and ice crystal ground mass fused salt are automatically separated, and obtains Al3It is multiple that Ti enhances aluminium base
Condensation material.
7. preparation Al as claimed in claim 63The method of Ti enhancing alumina-base material, it is characterised in that: the Al3Ti enhances aluminium
Contain 2%≤Al by percent by volume in sill3Ti≤25%。
8. preparation Al as claimed in claim 73The method of Ti enhancing alumina-base material, it is characterised in that: the titanyl compound
The ratio between quality and quality of alumina are 0.5% ~ 20%；The ratio between fluoride and quality of alumina of the titanium are 2% ~ 40%.
9. such as the described in any item preparation Al of claim 6-83The method of Ti enhancing alumina-base material, it is characterised in that: the oxidation
Object is TiO2, the fluoride of the titanium is Na2TiF6 Or K2TiF6。
10. preparation Al as claimed in claim 93The method of Ti enhancing alumina-base material, it is characterised in that: the TiO2Quality
It is 0.7% ~ 15% with the ratio between quality of alumina；The Na2TiF6 Quality and the ratio between quality of alumina be 2% ~ 30%；It is described
K2TiF6 Quality and the ratio between quality of alumina be 2% ~ 35%.
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Cited By (2)
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| CN110229979A (en) * | 2019-07-05 | 2019-09-13 | 西安交通大学 | A kind of transgranular crystal boundary distribution micro-nano multiphase granules reinforced aluminum matrix composites and preparation method thereof |
| CN112981102A (en) * | 2021-02-04 | 2021-06-18 | 昆明理工大学 | Preparation of TiAl3Method for alloying and purifying Fe-containing waste aluminum alloy |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110229979A (en) * | 2019-07-05 | 2019-09-13 | 西安交通大学 | A kind of transgranular crystal boundary distribution micro-nano multiphase granules reinforced aluminum matrix composites and preparation method thereof |
| CN112981102A (en) * | 2021-02-04 | 2021-06-18 | 昆明理工大学 | Preparation of TiAl3Method for alloying and purifying Fe-containing waste aluminum alloy |
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| CN109797318B (en) | 2021-08-20 |
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