CN109811169A - A kind of spontaneous Al of situ high pressure2O3The preparation method of particle reinforced Al matrix composite - Google Patents
A kind of spontaneous Al of situ high pressure2O3The preparation method of particle reinforced Al matrix composite Download PDFInfo
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Abstract
The invention discloses a kind of spontaneous Al of situ high pressure2O3The preparation method of particle reinforced Al matrix composite, the method are by Al powder, Si powder, Fe2O3Powder matches in proportion and is uniformly mixed it by ball mill, is sintered under GPa grades of condition of high voltage later, obtains in-situ authigenic Al2O3Particle reinforced Al matrix composite.The present invention utilizes oxide Fe under GPa grades of condition of high voltage2O3With Al reaction in-situ, eliminates the nuisance that reaction in-situ is also easy to produce and increase matrix elements solid solubility in Al based composites.Solid solubility increase can improve material mechanical performance.This method process is simple, high-efficient, is suitble to large area production.
Description
Technical field
The invention belongs to metal-base composites technical fields, and in particular to a kind of spontaneous Al of situ high pressure2O3Particle enhancing
The preparation method of Al based composites.
Background technique
With the continuous promotion of automobile engine power and revolving speed, the thermic load and mechanical load that piston is born are increasingly
Height, common aluminum alloy service performance have been increased to Limiting Level, it is therefore desirable to the more preferably material of mechanical property and heat resistance,
The service life of piston is improved, guarantees its reliability during military service.Fabricated in situ prepares Al2O3Particle REINFORCED Al base
Composite material has many advantages, such as low-density, high intensity, good heat resistance, good fatigue strength, these excellent performances make
Al based composites are obtained not only to be widely applied on the auto parts and components such as cylinder body, drag friction part, piston but also navigate in aviation
It, shipbuilding, industrially there is one seat in army.
Currently, Al2O3The method of particle reinforced Al matrix composite is divided into outer addition and original position in such a way that particle is added
From thinking of a way, outer addition is compared, the reinforced phase of in-situ authigenic method is generated and is evenly distributed in chemical reaction, overcomes reinforced phase pair
Surface contamination between reinforced phase and matrix the problems such as interfacial reaction, is obviously improved the performance of material；The process letter of in-situ authigenic method
Single, cost is relatively low, thus in-situ authigenic method becomes the composite material and preparation method thereof quickly grown in recent years.But in-situ authigenic reacts
Harmful substance can be generated in the process influences the performance of aluminum matrix composite, and the intensity of composite material is such as greatly reduced or reduces material
Fatigability etc., need to be improved composite material and preparation method thereof thus.
Constantly develop recently as high pressure technique, high pressure is widely used in material science.Pressure is
One of the important parameter for influencing solidified structure, Al based composites are prepared under condition of high voltage has good Research Prospects, and normal
Pressure is compared, and the Al based composites tissue of high pressure preparation is refined, and mechanical property is more preferable, and alloying element solubility improves, and is had
Conducive to subsequent heat treatment technique.
Summary of the invention
It is an object of the invention to overcome prior art defect, and provide a kind of spontaneous Al of situ high pressure2O3Particle REINFORCED Al
The preparation method of based composites.The present invention regulates and controls the preparation method of in-situ authigenic by a kind of efficient high pressure to eliminate original
The problem of being also easy to produce hazardous compound during the in-situ reaction of position, to obtain the Al based composites of strong mechanical performance.
Specific technical solution of the present invention is as follows:
A kind of spontaneous Al of situ high pressure2O3The preparation method of particle reinforced Al matrix composite the following steps are included:
1) Al powder, Si powder and Fe are weighed2O3Powder is simultaneously mixed to get mixed-powder；
2) the resulting mixed-powder of step 1), mill ball and ethylene glycol are put into ball mill and mix powder；Make after the completion of mixed powder
Mill ball is sifted out with sieve, and obtains mixed liquor；
3) the resulting mixed liquor of step 2) is put into revolving in Rotary Evaporators, and obtains blocky powder；
4) the resulting blocky powder of step 3) is ground into uniform powder using Agate grinding alms bowl；
5) the resulting uniform powder of step 4) is put into cold stamping die, and obtains biscuit using hydraulic press green compact；
6) the obtained biscuit of step 5) is wrapped in boron nitride ceramics, is then placed in pyrophillite mold；It reuses
Cubic hydraulic press is forced into 3-5GPa to pyrophillite grinding tool, is then sintered at a temperature of 1000-1200 DEG C；It keeps the temperature later, so
Furnace cooling afterwards finally obtains Al2O3Particle reinforced Al matrix composite.
Preferably, the Al powder, Si powder, Fe2O3The partial size of powder is 100-300 μm.
Preferably, the revolving speed of ball mill is 400r/min, mixing time 6h in the mixed powder operation of the step 2).
Preferably, the ball material mass ratio of the mill ball and mixed-powder is 5:1；The mill ball is Al2O3Ceramics are ground
Abrading-ball；The additional amount of the ethylene glycol is every 50g mixed-powder 200mL.
Preferably, the water bath temperature of Rotary Evaporators is 75 DEG C, rotation speed in the revolving operation of the step 3)
For 15r/min.
Preferably, the soaking time in the step 6) is 1h.
Preferably, the Al2O3The mass ratio of simple substance Al and elemental silicon is (65- in particle reinforced Al matrix composite
90): (10-35).
Preferably, the Al2O3Al in particle reinforced Al matrix composite2O3The volume fraction of particle is 5-15%.
The track weight that GPa grade high pressure of the present invention can effectively shorten atomic distance, increase adjacent electronics
It is folded, and then change the crystal habit of substance, improve the solid solubility of alloying element in metastable state tissue.
The present invention in terms of existing technologies, has the advantages that
(1) for the present invention using situ high pressure from thinking of a way, process is simple and high-efficient, is suitble to large area production；
(2) secondly, the Al that the present invention is prepared2O3Al in particle reinforced Al matrix composite2O3Particulates reinforcements distribution
Uniformly, and technology controlling and process ingredient can be passed through；
(3) Al that the present invention is prepared2O3Particle reinforced Al matrix composite intensity height, endurance, high temperature resistant, power
Performance is learned to significantly improve；
(4) it is easy to eliminate reaction in-situ using oxide Fe2O3 and Al reaction in-situ under GPa grades of condition of high voltage by the present invention
The nuisance of generation simultaneously increases matrix elements solid solubility in Al based composites, and solid solubility increase can improve the mechanics of materials
Performance.
(5) Al being prepared using the present invention2O3Particle reinforced Al matrix composite aerospace, automobile manufacture and
There is huge application potential on the fields such as army's industry.
Detailed description of the invention
Fig. 1 is Al2O3The scanning electron microscope (SEM) photograph of the microstructure of particle reinforced Al matrix composite.
Specific embodiment
The present invention is further elaborated and is illustrated with reference to the accompanying drawings and detailed description.Each implementation in the present invention
The technical characteristic of mode can carry out the corresponding combination under the premise of not conflicting with each other.
Embodiment one:
1) Al powder 39.9g, Si powder 5.4g and Fe are weighed2O3Powder 4.7g, is then mixed to get mixed-powder；
2) mixed-powder that step 1) configures is put into the jar of ball mill, Al is added2O3Mill ball, ball material mass ratio
For 5:1,200mL ethylene glycol is then added；Later, it puts jar well and starts mixed powder, revolving speed 200r/min, Ball-milling Time 6h,
Use sieve by Al after the completion of mixed powder2O3Mill ball sifts out, and obtains mixed liquor.
3) mixed liquor obtained in step 2) is put into Rotary Evaporators, and it is 75 DEG C that water bath temperature, which is arranged, rotation
Speed is 15r/min；The blocky powder of flask inner wall is taken out after the completion of revolving.
4) blocky powder obtained by step 3) is ground into alms bowl with Agate and is ground into uniform powder.
5) uniform powder obtained by step 4) is put into cold stamping die, biscuit is obtained to uniform powder green compact using hydraulic press.
6) the obtained biscuit of step 5) is wrapped in boron nitride ceramics, is then placed in pyrophillite mold, uses six
Face top hydraulic press is pressurized to 3GPa high pressure to it and is sintered；Sintering temperature is 1000 DEG C, soaking time 1h；After furnace cooling,
Obtain Al2O3Particle reinforced Al matrix composite.
Finally obtained Al2O3In particle reinforced Al matrix composite, Al2O3Volume ratio shared by particle and Al-Si base
The ratio of simple substance Al and simple substance Si pass through Al powder, Si powder and Fe in body2O3The ingredient proportion of powder controls.It can be according to final required material
The adjustment that ratio in material carries out, there are two types of methods of adjustment:
One is empirical method, adjusts Al powder, Si powder and Fe according to practical experiences such as embodiments2O3The ratio of powder, to obtain
Need the Al of ratio2O3Particle reinforced Al matrix composite；The second is according to the matter of simple substance Al, simple substance Si, simple substance Fe in final material
Amount ratio retrodicts required Al powder, Si powder and Fe2O3The quality of powder；Al wherein can be calculated according to the amount of simple substance Fe2O3Reinforced phase
Volume, and according to aluminium alloy density calculation formula D=1/ (NAl/DAl+NSi/DSi+NFe/DFe) (wherein D indicates density, and N is indicated
Element shared mass fraction in the alloy), Al in final material can be estimated2O3The volume fraction of reinforced phase；Therefore, root
It is estimated that value and can determine Al powder, Si powder and Fe in conjunction with basis material ratio2O3The ingredient proportion of powder.
It is shown through detection, Al obtained by embodiment one2O3The matrix of particle reinforced Al matrix composite is Al-12Si,
Al2O3The volume fraction of particulates reinforcements is 5%.The scanning electron microscope (SEM) photograph of its microstructure is as shown in Figure 1.
Fig. 1 shows that the present invention uses to be sintered under 3-5GPa condition of high voltage, obtained Al2O3Particulates reinforcements partial size is smaller,
Draw ratio is small and is distributed in matrix boundary mostly.Conventional Al2O3Particle has good intensity hardness and low thermal coefficient of expansion
But brittleness is too big, therefore partial size and draw ratio is small can reduce it to matrix damage in the present invention, improves the comprehensive of composite material
Close mechanical property.And the low hardening constituent of thermal expansion coefficient is distributed in the expansion that matrix boundary is able to suppress matrix, and enhancing is multiple
The thermal stability of condensation material.
Embodiment two:
1) Al powder 36.1g, Si powder 4.9g and Fe are weighed2O3Powder 9g, is then mixed to get mixed-powder；
2) mixed-powder that step 1) configures is put into the jar of ball mill, Al is added2O3Mill ball, ball material mass ratio
For 5:1,200mL ethylene glycol is then added；Later, it puts jar well and starts mixed powder, revolving speed 200r/min, Ball-milling Time 6h,
Use sieve by Al after the completion of mixed powder2O3Mill ball sifts out, and obtains mixed liquor.
3) mixed liquor obtained in step 2) is put into Rotary Evaporators, and it is 75 DEG C that water bath temperature, which is arranged, rotation
Speed is 15r/min；The blocky powder of flask inner wall is taken out after the completion of revolving.
4) blocky powder obtained by step 3) is ground into alms bowl with Agate and is ground into uniform powder.
5) uniform powder obtained by step 4) is put into cold stamping die, biscuit is obtained to uniform powder green compact using hydraulic press.
6) the obtained biscuit of step 5) is wrapped in boron nitride ceramics, is then placed in pyrophillite mold, uses six
Face top hydraulic press is pressurized to 4GPa high pressure to it and is sintered；Sintering temperature is 1000 DEG C, soaking time 1h；After furnace cooling,
Obtain Al2O3Particle reinforced Al matrix composite.
It is shown through detection, Al obtained by embodiment two2O3The matrix of particle reinforced Al matrix composite is Al-12Si,
Al2O3The volume fraction of particulates reinforcements is 10%.The scanning electron microscope (SEM) photograph of its microstructure is similar to the result of embodiment one.
Embodiment three:
1) Al powder 32.6g, Si powder 4.5g and Fe are weighed2O3Powder 12.9g, is then mixed to get mixed-powder；
2) mixed-powder that step 1) configures is put into the jar of ball mill, Al is added2O3Mill ball, ball material mass ratio
For 5:1,200mL ethylene glycol is then added；Later, it puts jar well and starts mixed powder, revolving speed 200r/min, Ball-milling Time 6h,
Use sieve by Al after the completion of mixed powder2O3Mill ball sifts out, and obtains mixed liquor.
3) mixed liquor obtained in step 2) is put into Rotary Evaporators, and it is 75 DEG C that water bath temperature, which is arranged, rotation
Speed is 15r/min；The blocky powder of flask inner wall is taken out after the completion of revolving.
4) blocky powder obtained by step 3) is ground into alms bowl with Agate and is ground into uniform powder.
5) uniform powder obtained by step 4) is put into cold stamping die, biscuit is obtained to uniform powder green compact using hydraulic press.
6) the obtained biscuit of step 5) is wrapped in boron nitride ceramics, is then placed in pyrophillite mold, uses six
Face top hydraulic press is pressurized to 4GPa high pressure to it and is sintered；Sintering temperature is 1100 DEG C, soaking time 1h；After furnace cooling,
Obtain Al2O3Particle reinforced Al matrix composite.
It is shown through detection, Al obtained by embodiment three2O3The matrix of particle reinforced Al matrix composite is Al-12Si,
Al2O3The volume fraction of particulates reinforcements is 15%.The scanning electron microscope (SEM) photograph of its microstructure is similar to the result of embodiment one.
Example IV:
1) Al powder 26.7g, Si powder 6.7g and Fe are weighed2O3Powder 16.6g, is then mixed to get mixed-powder；
2) mixed-powder that step 1) configures is put into the jar of ball mill, Al is added2O3Mill ball, ball material mass ratio
For 5:1,200mL ethylene glycol is then added；Later, it puts jar well and starts mixed powder, revolving speed 200r/min, Ball-milling Time 6h,
Use sieve by Al after the completion of mixed powder2O3Mill ball sifts out, and obtains mixed liquor.
3) mixed liquor obtained in step 2) is put into Rotary Evaporators, and it is 75 DEG C that water bath temperature, which is arranged, rotation
Speed is 15r/min；The blocky powder of flask inner wall is taken out after the completion of revolving.
4) blocky powder obtained by step 3) is ground into alms bowl with Agate and is ground into uniform powder.
5) uniform powder obtained by step 4) is put into cold stamping die, biscuit is obtained to uniform powder green compact using hydraulic press.
6) the obtained biscuit of step 5) is wrapped in boron nitride ceramics, is then placed in pyrophillite mold, uses six
Face top hydraulic press is pressurized to 5GPa high pressure to it and is sintered；Sintering temperature is 1200 DEG C, soaking time 1h；After furnace cooling,
Obtain Al2O3Particle reinforced Al matrix composite.
It is shown through detection, Al obtained by example IV2O3The matrix of particle reinforced Al matrix composite is Al-12Si,
Al2O3The volume fraction of particulates reinforcements is 20%.The scanning electron microscope (SEM) photograph of its microstructure is similar to the result of embodiment one.
Above-mentioned embodiment is only a preferred solution of the present invention, so it is not intended to limiting the invention.Have
The those of ordinary skill for closing technical field can also make various changes without departing from the spirit and scope of the present invention
Change and modification.Therefore all mode technical solutions obtained for taking equivalent substitution or equivalent transformation, all fall within guarantor of the invention
It protects in range.
Claims (8)
1. a kind of spontaneous Al of situ high pressure2O3The preparation method of particle reinforced Al matrix composite, which is characterized in that including following
Step:
1) Al powder, Si powder and Fe are weighed2O3Powder is simultaneously mixed to get mixed-powder；
2) the resulting mixed-powder of step 1), mill ball and ethylene glycol are put into ball mill and mix powder；Sieve is used after the completion of mixed powder
Net sifts out mill ball, and obtains mixed liquor；
3) the resulting mixed liquor of step 2) is put into revolving in Rotary Evaporators, and obtains blocky powder；
4) the resulting blocky powder of step 3) is ground into uniform powder using Agate grinding alms bowl；
5) the resulting uniform powder of step 4) is put into cold stamping die, and obtains biscuit using hydraulic press green compact；
6) the obtained biscuit of step 5) is wrapped in boron nitride ceramics, is then placed in pyrophillite mold；Reuse six faces
Top hydraulic press is forced into 3-5GPa to pyrophillite grinding tool, is then sintered at a temperature of 1000-1200 DEG C；Keep the temperature later, then with
Furnace is cooling, finally obtains Al2O3Particle reinforced Al matrix composite.
2. Al according to claim 12O3The preparation method of particle reinforced Al matrix composite, which is characterized in that the Al
Powder, Si powder, Fe2O3The partial size of powder is 100-300 μm.
3. Al according to claim 12O3The preparation method of particle reinforced Al matrix composite, which is characterized in that the step
2) in mixed powder operation, the revolving speed of ball mill is 400r/min, mixing time 6h.
4. Al according to claim 12O3The preparation method of particle reinforced Al matrix composite, which is characterized in that the grinding
The ball material mass ratio of ball and mixed-powder is 5:1；The mill ball is Al2O3Ceramic grinding ball；The additional amount of the ethylene glycol is
Every 50g mixed-powder 200mL.
5. Al according to claim 12O3The preparation method of particle reinforced Al matrix composite, which is characterized in that the step
3) in revolving operation, the water bath temperature of Rotary Evaporators is 75 DEG C, rotation speed 15r/min.
6. Al according to claim 12O3The preparation method of particle reinforced Al matrix composite, which is characterized in that the step
6) soaking time in is 1h.
7. Al according to claim 12O3The preparation method of particle reinforced Al matrix composite, which is characterized in that the Al2O3
The mass ratio of simple substance Al and simple substance Si is (65-90): (10-35) in particle reinforced Al matrix composite.
8. Al according to claim 12O3The preparation method of particle reinforced Al matrix composite, which is characterized in that the Al2O3
Al in particle reinforced Al matrix composite2O3The volume fraction of particle is 5-15%.
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Effective date of registration: 20200731 Address after: 1 No. 324022 Zhejiang province Quzhou city Qujiang District Haili Avenue Patentee after: ZHEJIANG HAILI MAKES Co.,Ltd. Address before: 324000 North Road, Quzhou, Zhejiang, No. 78, No. nine Patentee before: QUZHOU University |