CN102560199B - Use TiSiN and EuH2aluminium alloy of powder-processed and preparation method thereof - Google Patents
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Abstract
The present invention relates to a kind of employing TiSiN and EuH2Aluminium alloy of powder-processed and preparation method thereof; 1.0～the Ti of 1.7% are added with powder in wrought aluminium alloy; 1.0～the Si of 1.7%; 1.0～the Eu element of the N of 1.7%, 1.0～1.7%; during adding aluminium alloy melt with fluidization form with protective gas; there is the specific surface area more much bigger than general cake mass, it is possible to realize quickly dispersion and be fully contacted with melt, significantly shorten dispersion and uniform time.Use the high-strength aluminum alloy of the present invention simultaneously in casting process, heterogeneous forming core core can be effectively increased in alloy graining process, thus reach the effect of crystal grain refinement, strengthen alloy strength；And the element added can promote to form interstitial atom and gap phase, during high temperature, in α (Al) solid solution, dissolubility is big, and the least when room temperature, so that alloy has higher heat-treatability matter, after heat treatment, its intensity and hardness all have significant improvement.
Description
Technical field
The present invention relates to a kind of high-strength aluminum alloy, further relate to its preparation method.
Background technology
The aluminium alloy of deep processing generally requires and is first cast as large-scale ingot blank, such as slab ingot, pole etc., again by rolling, extrude, the means such as forging, it is processed into various finished product, these processes substantially will combine with heat treatment phase, if to the final products that can directly use, the most also will be through operations such as over-segmentation, Surface Machining, Passivation Treatment.These manufacturing process, need aluminum alloy materials itself to possess good deep shaping property, including casting character, pressure processing deformation performance, heat treatment reinforcement performance, corrosion resistance, resisting fatigue destructive characteristics, Surface Machining and paintability etc..Wherein, founding performance is the basis of aluminium alloy deep shaping property.Large-scale ingot blank, the pole of slab ingot, slab and more than the diameter 500mm of especially more than thickness 500mm, it is the representative base material of Large Efficient deep processing, and large-scale ingot blank can be prefabricated into, be also that test aluminum alloy materials itself is if appropriate for the first technology critical point carrying out deep processing.
When improper due to composition and pouring technology in Al-Si-Cu line aluminium alloy, easily form high hardness compound.Particularly with silicon content less than 12% (mass fraction), when the content of Mn+Fe is higher than 0.8% (mass fraction), it is very easy to generateAl 12Si(FeMn)3Compound.Hardness after shaping due to this aluminium alloy is higher, and during machining, tool wear is serious, and the white light tone Hard Inclusion heaved seen from the surface naked eyes after processing, microexamination Hard Inclusion is skeleton shape or irregular particle shape.Being grouped into Al-Si-Mn-Fe through the one-tenth of this Hard Inclusion of power spectrum composition measurement, its form is easily obscured mutually with primary silicon in alloy.Part after the aluminium alloy with this Hard Inclusion compound shapes, not only poor in processability, and have a strong impact on the roughness of finished surface and the quality of anodic film.
Owing to alloying component or the big one-tenth branch of compound Midst density are deposited in foundry goods bottom, the composition that density is little floats on top.Such as add this refractory metal of Ti for crystal grain thinning and form dystectic flaky compound Al with Al3Ti can crystallize out earlier from aluminium alloy, it is easy for when growing up to bigger sinking to producing the gravity segregation of local code, can see the compound of the white bright ash of surfacing when segregation is more serious on foundry goods fracture, primary silicon thick in hypereutectic Al-Si aluminium alloy is easily formed segregation owing to density is less.
Additionally causing eutectic segregation owing to stirring is uneven when this aluminium alloy before cast, at Eutectic Silicon in Al-Si Cast Alloys concentration, hardness high fragility is big, and process tool abrasion is big；The position that Eutectic Silicon in Al-Si Cast Alloys is few forms α (Al) solid solution soft spots, and intensity is low, adds and not only glues cutter man-hour, deteriorates processing characteristics, and the deformation of α (Al) solid solution can be made under the effect of cutting force to cause machined surface white macula occur.When in ZL108 (ZAlSi12Cu2Mg1) aluminium alloy, magnesium content is less than 0.6% (mass fraction), the most easily there is white macula in finished surface.When in Al-Si-Cu aluminium alloy, the segregation of Cu element causes regional area thick Al occur2Cu phase edge are brilliant in net distribution, and heat treatment can not be dissolved completely in α (Al) solid solution and remain in intergranular, also makes alloy fragility increase.
Meanwhile, when using this aluminium alloy to cast, in foundry goods cast, often appearance is various is mingled with, and mainly has oxide to be mingled with, Modeling Material and flux mixture etc..Wherein, be mingled with aluminum oxide the most universal.Especially in the aluminium alloy containing Mg, majority is mingled with the mixture for aluminium oxide and magnesium oxide, so during aluminium alloy smelting, the content that oxide is mingled with is one of important mark matter of reflection aluminum liquid metallurgical quality.
As can be seen here: in addition to current aluminum alloy materials forming property when founding large-scale ingot blank is poor, large-scale ingot blank is the highest in the quenching degree of heat treatment process, tempering resistance is poor and can not meet higher mechanical property requirements or some property (as heat-resisting, anti-corrosion) etc., is also significant deficiency.These defects make it substitute in field of engineering technology in the process of the strong materials of weight such as steel part and structure and define the technology breakpoint being difficult to cross over.
Summary of the invention
In order to overcome the deficiencies in the prior art, the present invention provides a kind of and uses TiSiN and EuH2Aluminium alloy of powder-processed and preparation method thereof, it is possible to overcome the deficiency of existing aluminium alloy capability, improves its obdurability, formability and quenching degree, provides high-end base material for efficient deep processing.
A kind of employing TiSiN and EuH2The aluminium alloy of powder-processed, it is characterized in that by percentage to the quality, including the Fe less than or equal to 0.5%, 0.15～the Cu of 0.4%, 0.4～the Mn of 1.0%, Cr less than or equal to 0.1%, 0.5～the Mg of 1.2%, the Zn less than or equal to 0.25%, 1.0～the Ti of 1.7%, 1.0～the Si of 1.7%, 0.29～the Eu of the N of 0.49% and 3.17～5.38%, surplus is Al and inevitable impurity；The content of described single contaminant is less than the 0.05% of gross mass percentage ratio, and content of impurities is less than the 0.15% of gross mass percentage ratio.
A kind of employing TiSiN and EuH2The preparation method of the aluminium alloy of powder-processed, it is characterised in that step is as follows:
Step 1: aluminium ingot is added heating in smelting furnace and is allowed to be completely melt, it is subsequently adding the Fe accounting for output aggregate mass percent less than or equal to 0.5%, 0.15～the Cu of 0.4%, 0.4～the Mn of 1.0%, Cr less than or equal to 0.1%, 0.5～the Mg of 1.2% and less than or equal to 0.25% Zn, be completely dissolved and melt；Described fusion process completes in enclosed environment；
Step 2: be incubated at 700～1000 DEG C, obtain alloy melt；
Step 3: use mixed gas that aluminium alloy melt carries out degassing and purifying operation, and output aggregate the mass percent 1.87～EuH of the TiSiN of 3.18% and 3.21～5.45% will be accounted for2Powder joins in aluminium alloy melt with above-mentioned gas with fluidized regime and mixes, and makes TiSiN and EuH2Aluminium alloy melt is evenly distributed, and Continuous aeration is until reacting complete；Described mixed gas is: nitrogen or noble gas or nitrogen are mixed to get according to arbitrary proportion with noble gas；
Step 4: reaction terminates rear homoiothermic to 680～730 DEG C, obtains the aluminium alloy melt that melting completes.
Aluminium ingot in step 1 is replaced with molten aluminum liquid.
A kind of by described employing TiSiN and EuH2The method that the aluminium alloy of powder-processed carries out casting, it is characterized in that: the aluminium alloy melt of claim 2 melting is toppled over along chute and comes out of the stove, to vertical water cooling casting machine system, large-scale slab ingot more than casting processing ingot blank, particularly cast thickness 500mm and the pole of more than diameter 500mm.
A kind of by described employing TiSiN and EuH2The method that the aluminium alloy of powder-processed carries out casting, it is characterized in that: the aluminium alloy melt tuberculosis of claim 2 melting is entered in the mold of foundry goods, use metal mold, sand mold or mixed type casting mode, use gravitational casting, compression casting or counter-pressure casting technique, the aluminium alloy castings of Casting Aluminum Alloy Based, particularly casting large-scale, thin-walled or labyrinth.
Employing TiSiN and EuH that the present invention provides2Aluminium alloy of powder-processed and preparation method thereof, adds 1.87～the EuH of the TiSiN of 3.18% and 3.21～5.45% with powder in wrought aluminium alloy2, during adding aluminium alloy melt with fluidization form with protective gas, there is the specific surface area more much bigger than general cake mass, it is possible to realize quickly dispersion and be fully contacted with melt, significantly shorten dispersion and uniform time.Use the high-strength aluminum alloy of the present invention simultaneously in casting process, heterogeneous forming core core can be effectively increased in alloy graining process, thus reach the effect of crystal grain refinement, strengthen alloy strength；And the element added can promote to form interstitial atom and gap phase, during high temperature, in α (Al) solid solution, dissolubility is big, and the least when room temperature, so that alloy has higher heat-treatability matter, after heat treatment, its intensity and hardness all have significant improvement.
Make a concrete analysis of as follows:
Before this alloy is without adding above-mentioned element, in melt in addition to forming the common solution of various elements, the compound phase possibly together with being formed between more following metals:
Mg2Si phase, N phase (Al7Cu2Fe), α phase (Al12Fe3Si), S-phase (Al2CuMg)；
These metallic compounds are when melt cooling, due to system minimum free energy principle, can not stable existence in the crystal grain formed, to move to crystal boundary under the driving that distortion of lattice can differ from and concentrate, simultaneously, significantly reduce owing to alloying element saturation solubility in aluminum substrate declines along with temperature, so along with the cooling of melt, oversaturated melt constantly separates out the intermetallic compound rich in alloying element, these compounds are enriched with at intergranular, it is difficult to each other merge, thick intergranular compound group is become in microstructure, alloy is produced crisp hardening effect, deteriorate alloy cast form performance, reduce its uniformity, toughness, corrosion resistance and through hardening performance.So, when alloy graining becomes the basic structure of supersaturated solid solution matrix+intergranular metallic compound, commonly referred to pure as-cast structure, just can have mechanical property and other technical specification of satisfied needs after having the heat treatment that the alloy of this tissue has to pass through " solid solution+timeliness ".
Although, the heat treatment through formulation optimization process and raising alloy property can be improved, but alloy itself still exists a lot of defect: insufficient strength is high, it is impossible to cast big specification type ingot etc..
The present invention is by comparing selection, the nitride developing transition element processes the mode of melt, by adding 1.0～the Ti of 1.7%, 1.0～the Si of 1.7%, 1.0～the N of 1.7%, 1.0～the Eu element of 1.7%, the atomic state M metal that nitride after decomposition produces, without the potential barrier that between the powerful metal bond energy and similar atom produced, the lattice energy of tightly packed generation is formed of combining closely with d/f/s electronics between metallic atom under elemental stage, merge with surrounding substantial amounts of matrix atom with " naked state ", form solution and metallic compound altogether, and leading phase when becoming crystallization and grain refining phase, also it is High-Temperature Strengthening phase simultaneously.Therefore, carbide, to produce the decomposition under high temperature and the disperse state of formation in fluidization addition melt, solves refractory metal and dissolves problem difficult, that be uniformly distributed difficulty in aluminum liquid, it is achieved that the microcosmic homogenization of distortion of lattice energy is distributed and the refinement of crystal grain.
The nitrogen being additionally filled with in fusion process, beneficially aluminum synthesize AlN in the blanket of nitrogen of 800～1000 DEG C.It is atomic crystal owing to N with Al reacts the AlN generated, belongs to diamond like carbon nitride, the highest be stabilized to 2200 DEG C；Room temperature strength is high, and intensity declines slower with the rising of temperature, it is possible to be effectively improved elevated temperature strength and the resistance to corrosion of alloy；Heat conductivity is good, and thermal coefficient of expansion is little, can improve matrix material thermal shock resistance.Therefore, N is worked as2When being filled with high temperature aluminium alloys melt, inherently it is provided with the activity reacted with various metals gold.So temperature when suitably regulating cleaning molten operation and the concentration of protectiveness nitrogen, the content of AlN in scalable melt, this provides method for the content of transition metal in regulation melt further.
The degree that the nitride being added additionally in melt decomposes, changes along with the stability of nitride itself and the difference of melt temperature, i.e. reaction has certain reversibility, is a kind of dynamic balance.Most of transition elements saturation solubility in aluminum melt is less, and, except the maximum solid solution degree of chromium, titanium, vanadium, zirconium occurs in addition to Peritectic Temperature, and the maximum solid solution degree of other elements all occurs in eutectic temperature；Dissolubility at room temperature, respectively less than 0.1%wt.
Visible: due to the means using fluidization nitride to process in the present invention, the multi-effect of strengthening matrix and crystal grain thinning is integrated, replace intermediate alloy, enable aluminum alloy to manufacturing enterprise and be no longer limited by intermediate alloy manufacturer, be conducive to creating the Green line of " nearly molding, short route, intensive ", energy-saving and cost-reducing, reduce integrated cost；Simultaneously, in heat treatment process, owing to defining the material microstructure of excellence, the residual stress of ingot blank is less, therefore can significantly improve heat treatment usefulness, improve the quenching degree of ingot blank, when comparing with similar alloy, thicker blank (sheet material of more than thickness 500mm and the bar of more than diameter 500mm) can be produced with " casting+heat treatment mode ", the cut deal manufacturing technology of series specification (thickness 15～200mm) realizes " rolling with casting generation ".
Sum it up, the invention has the beneficial effects as follows:
In aluminum melt, cause multiple grain refining element, particle, the coarsening preventing matrix and hardening constituent is had good result.Aluminum substrate after the cooling period causes the high interstitial atom of stability and gap phase, becomes new efficient hardening constituent, make the intensity of material and hardness be improved.
Below in conjunction with embodiment, the present invention is further described.
Detailed description of the invention
Embodiment 1:
A kind of employing TiSiN and EuH2The aluminium alloy of powder-processed, by percentage to the quality, including the Fe of 0.5%, the Cu of 0.15%, the Mn of 0.4%, the Cr of 0.1%, the Mg of 0.5%, the Zn of 0.25%, the Ti of 1.0%, the Si of 1.0%, the N of 1.0%, the Eu of 1.0%, surplus is Al and inevitable impurity, and the content of every kind of impurity is less than the 0.05% of gross mass percentage ratio, and the content of all impurity is less than the 0.15% of gross mass percentage ratio.
The present invention also provides for described employing TiSiN and EuH2The preparation method of the aluminium alloy of powder-processed, adds TiSiN and EuH in Combined Processing mode2, comprise the following steps:
Step one: according to described employing TiSiN and EuH2The component of the aluminium alloy of powder-processed is got the raw materials ready, including the Fe, the Cu of 0.15%, the Mn of 0.4%, the Cr of 0.1%, the Mg of 0.5%, the Zn of 0.25% that account for output aggregate mass percent 0.5%；
Step 2: first adding aluminium ingot or molten aluminum liquid in smelting furnace, heating is allowed to be completely melt, is initially charged getting the raw materials ready of step one by formula proportion, is allowed to be completely dissolved and melt, and is incubated, obtains alloy melt after refine at 700～1000 DEG C；Fusion process completes in enclosed environment；
Step 3: use nitrogen or noble gas or nitrogen, with the mixed gas of noble gas arbitrary proportion, alloy melt carries out degassing and purifying operation, and Continuous aeration is until reacting complete；The TiSiN of output aggregate mass percent 1.0%, the EuH of 1.0% will be accounted for simultaneously2Powder joins in alloy melt with above-mentioned gas with fluidized regime；It is stirred, makes TiSiN and EuH2Alloy melt is evenly distributed, and fully reacts with alloy melt；Standing, homoiothermic to 680～730 DEG C, obtain the aluminium alloy melt that melting completes.
Embodiment 2:
A kind of employing TiSiN and EuH2The aluminium alloy of powder-processed, by percentage to the quality, including the Fe of 0.4%, the Cu of 0.25%, the Mn of 0.8%, the Cr of 0.08%, the Mg of 0.9%, the Zn of 0.2%, the Ti of 1.3%, the Si of 1.3%, the N of 1.3%, the Eu of 1.3%, surplus is Al and inevitable impurity, and the content of every kind of impurity is less than the 0.05% of gross mass percentage ratio, and the content of all impurity is less than the 0.15% of gross mass percentage ratio.
The present invention also provides for described employing TiSiN and EuH2The preparation method of the aluminium alloy of powder-processed, adds TiSiN and EuH in Combined Processing mode2, comprise the following steps:
Step one: according to described employing TiSiN and EuH2The component of the aluminium alloy of powder-processed is got the raw materials ready, including the Fe, the Cu of 0.25%, the Mn of 0.8%, the Cr of 0.08%, the Mg of 0.9%, the Zn of 0.2% that account for output aggregate mass percent 0.4%；
Step 2: first adding aluminium ingot or molten aluminum liquid in smelting furnace, heating is allowed to be completely melt, is initially charged getting the raw materials ready of step one by formula proportion, is allowed to be completely dissolved and melt, and is incubated, obtains alloy melt after refine at 700～1000 DEG C；Fusion process completes in enclosed environment；
Step 3: use nitrogen or noble gas or nitrogen, with the mixed gas of noble gas arbitrary proportion, alloy melt carries out degassing and purifying operation, and Continuous aeration is until reacting complete；The TiSiN of output aggregate mass percent 1.3%, the EuH of 1.3% will be accounted for simultaneously2Powder joins in alloy melt with above-mentioned gas with fluidized regime；It is stirred, makes TiSiN and EuH2Alloy melt is evenly distributed, and fully reacts with alloy melt；Standing, homoiothermic to 680～730 DEG C, obtain the aluminium alloy melt that melting completes.
Embodiment 3:
A kind of employing TiSiN and EuH2The aluminium alloy of powder-processed, by percentage to the quality, including the Fe of 0.3%, the Cu of 0.4%, the Mn of 1.0%, the Cr of 0.05%, the Mg of 1.2%, the Zn of 0.1%, the Ti of 1.7%, the Si of 1.7%, the N of 1.7%, the Eu of 1.7%, surplus is Al and inevitable impurity, and the content of every kind of impurity is less than the 0.05% of gross mass percentage ratio, and the content of all impurity is less than the 0.15% of gross mass percentage ratio.
The present invention also provides for described employing TiSiN and EuH2The preparation method of the aluminium alloy of powder-processed, adds TiSiN and EuH in Combined Processing mode2, comprise the following steps:
Step one: according to described employing TiSiN and EuH2The component of the aluminium alloy of powder-processed is got the raw materials ready, the Fe, the Cu of 0.4%, the Mn of 1.0%, the Cr of 0.05%, the Mg of 1.2%, the Zn of 0.1% including accounting for output aggregate mass percent 0.3%:
Step 2: first adding aluminium ingot or molten aluminum liquid in smelting furnace, heating is allowed to be completely melt, is initially charged getting the raw materials ready of step one by formula proportion, is allowed to be completely dissolved and melt, and is incubated, obtains alloy melt after refine at 700～1000 DEG C；Fusion process completes in enclosed environment；
Step 3: use nitrogen or noble gas or nitrogen, with the mixed gas of noble gas arbitrary proportion, alloy melt carries out degassing and purifying operation, and Continuous aeration is until reacting complete；The TiSiN of output aggregate mass percent 1.7%, the EuH of 1.7% will be accounted for simultaneously2Powder joins in alloy melt with above-mentioned gas with fluidized regime；It is stirred, makes TiSiN and EuH2Alloy melt is evenly distributed, and fully reacts with alloy melt；Standing, homoiothermic to 680～730 DEG C, obtain the aluminium alloy melt that melting completes.
Use employing TiSiN and EuH of the inventive method melting2After the aluminum alloy melt of powder-processed is come out of the stove, carry out the Foundry Production of different goods respectively along following two flow process.
Flow process one: topple over along chute and come out of the stove, to vertical water cooling casting machine system, large-scale slab ingot more than casting processing ingot blank, particularly cast thickness 500mm and the pole of more than diameter 500mm.
Flow process two: tuberculosis enters in the mold of foundry goods, uses metal mold, sand mold or mixed type casting mode, uses gravitational casting, compression casting or counter-pressure casting technique, Casting Aluminum Alloy Based, the particularly aluminium alloy castings of casting large-scale, thin-walled or labyrinth.
Claims (5)
1. one kind uses TiSiN and EuH2The aluminium alloy of powder-processed, it is characterised in that by percentage to the quality, including little
In the Fe equal to 0.5%, 0.15～the Cu of 0.4%, 0.4～the Mn of 1.0%, the Cr less than or equal to 0.1%, 0.5～1.2%
Mg, the Zn less than or equal to 0.25%, 1.0～the Ti of 1.7%, 1.0～the Si of 1.7%, 0.29～the N of 0.49%
With 3.17～the Eu of 5.38%, surplus is Al and inevitable impurity；The content of single contaminant is less than total matter
The 0.05% of amount percentage ratio, content of impurities is less than the 0.15% of gross mass percentage ratio.
2. employing TiSiN and EuH described in a claim 12The preparation method of the aluminium alloy of powder-processed, its feature
It is that step is as follows:
Step 1: aluminium ingot is added heating in smelting furnace and is allowed to be completely melt, be subsequently adding and account for output aggregate mass percent
Fe less than or equal to 0.5%, 0.15～the Cu of 0.4%, 0.4～the Mn of 1.0%, the Cr less than or equal to 0.1%, 0.5～1.2%
Mg and less than or equal to 0.25% Zn, be completely dissolved and melt；Described fusion process completes in enclosed environment；
Step 2: be incubated at 700～1000 DEG C, obtain alloy melt；
Step 3: use mixed gas that aluminium alloy melt carries out degassing and purifying operation, and output aggregate percent mass will be accounted for
The ratio 1.87～EuH of the TiSiN of 3.18% and 3.21～5.45%2Powder joins aluminum with fluidized regime with above-mentioned gas
Alloy melt mixes, makes TiSiN and EuH2Aluminium alloy melt is evenly distributed, and Continuous aeration is until anti-
Should be complete；Described mixed gas is: nitrogen is mixed to get according to arbitrary proportion with noble gas；
Step 4: reaction terminates rear homoiothermic to 680～730 DEG C, obtains the aluminium alloy melt that melting completes.
Preparation method the most according to claim 2, it is characterised in that: the aluminium ingot in step 1 is replaced with molten aluminum liquid.
4. the method that aluminium alloy melt preparation method described in claim 2 obtained carries out casting, it is characterised in that:
The aluminium alloy melt of institute's melting is toppled over along chute and comes out of the stove, to vertical water cooling casting machine system, cast processing ingot
Base.
5. the method that aluminium alloy melt preparation method described in claim 2 obtained carries out casting, it is characterised in that:
The aluminium alloy melt tuberculosis of institute's melting is entered in the mold of foundry goods, uses metal mold, sand mold or mixed type casting mode,
Use gravitational casting, compression casting or counter-pressure casting technique, Casting Aluminum Alloy Based.
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| CN1936050A (en) * | 2006-10-18 | 2007-03-28 | 东华大学 | Fine grained aluminium alloy and its preparing method |
| CN101597709A (en) * | 2008-10-23 | 2009-12-09 | 无锡麟龙铝业有限公司 | A kind of environmentally friendly cast aluminium alloy and manufacture method thereof |
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| CN1936050A (en) * | 2006-10-18 | 2007-03-28 | 东华大学 | Fine grained aluminium alloy and its preparing method |
| CN101597709A (en) * | 2008-10-23 | 2009-12-09 | 无锡麟龙铝业有限公司 | A kind of environmentally friendly cast aluminium alloy and manufacture method thereof |
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