CN102676883B - Silicon carbide reinforced aluminum-based composite material and preparation method thereof - Google Patents
Silicon carbide reinforced aluminum-based composite material and preparation method thereof Download PDFInfo
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- CN102676883B CN102676883B CN201110427149.4A CN201110427149A CN102676883B CN 102676883 B CN102676883 B CN 102676883B CN 201110427149 A CN201110427149 A CN 201110427149A CN 102676883 B CN102676883 B CN 102676883B
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Abstract
The invention discloses a silicon carbide reinforced aluminum-based composite material and a preparation method thereof. The silicon carbide reinforced aluminum-based composite material is prepared from the following raw materials in percentage by volume: 20 to 25 percent of 325-mesh silicon carbide powder and the balance of 500-mesh Al-30Si alloy powder. According to the silicon carbide reinforced aluminum-based composite material, the silicon carbide powder and the Al-30Si alloy powder which have properly matched particle sizes are easily combined closely in the pressing and sintering process, defects such as air holes and cracks are avoided and the compactness of the composite material can be improved. In addition, by the preparation method of heating, pressurizing and keeping temperature stepwise according to set programs under the vacuum condition, slowly cooling together with a furnace to room temperature under the vacuum and high pressure conditions and removing the pressure, the metallurgical bonding of the reinforcement and the matrix is further improved, the defects such as air holes and cracks are avoided and the performance is high.
Description
Technical field
The present invention relates to a kind of aluminum matrix composite of SiC reinforcement, relate to a kind of preparation method of this matrix material simultaneously, belong to inorganic composite materials technical field.
Background technology
In recent years, enhancing aluminum-base composite material by silicon carbide particles is with premium propertiess such as its distinctive low expansion, high specific strength, high ratio modulus, high abrasions, progressively approved by aerospace industry, in the field such as piston and brake system of automobile, be also widely used simultaneously.
The enhancing aluminum-base composite material by silicon carbide particles of high-volume fractional is difficult to fine and close.And density is the important factor that determines material mechanical performance.How improving the density of material, is unusual key issue in matrix material preparation.Existing preparation method is broadly divided into liquid phase process and solid state process two classes.
Liquid phase process mainly contains casting, spray deposition and osmose process.In liquid phase process, easily there is harmful surface reaction 3SiC+4Al → Al
4c
3+ 3Si; SiC particle exists in aluminium liquid, and soltion viscosity is improved, and mobility reduces, filling difficulty when casting; And the consistency of silicon-carbide particle and aluminium alloy is poor, proportion differs greatly, and easily in melt, reunites or assembles, and causes size distribution inhomogeneous, affects the performance of aluminum matrix composite.Although control the distribution of reinforced particulate and with the interface wet ability of aluminum substrate aspect can adopt Melt Stirring method, but in follow-up cooled and solidified process, be difficult to control separating out and growing up of primary silicon phase in aluminum silicon alloy matrix, it is serious that large block silicon grain reduces composite property.Conventionally SiCp/Al-30Si matrix material adopts solid state process preparation more.
Solid state process that is powder metallurgic method.We adopted the processing methodes of the base+sintering of colding pressing more in the past.To tentatively in the vacuum of the powder metallurgy compact part of compression moulding in agglomerating plant or protective atmosphere environment, carry out sinter molding.Both made pressure to 600MPa-800MPa, after sintering the porosity of matrix material still very high, density is lower, substantially, in 90%, still needs follow-up hot-pressing densification processing, preparation section complexity.
Hot press forming technology is that the powder being pre-mixed is packed in the mould of integrated heating device, is put into and on pressing device, heats and suppress.Heat pressing process method principal feature is compacting and sintering to carry out simultaneously, makes pressed compact approach theoretical density, can obtain the intensity of needs and the powdered metal parts of physicals.Carry out but this technique concentrates in mould, high moderate pressure can reduce the work-ing life of mould, higher to mold material and structural requirement.Meanwhile, moulding stock difference, mould specific heat capacity is different from accumulation of heat, temperature rise rate in preparation process, soaking time affects uniformity consistency and the microstructure of composite homogeneity of die temperature; Soaking time is long or Heating temperature is too high, and the silicon grain of separating out in microstructure of composite is grown up seriously, also has part metals aluminium to precipitate into pressed compact top layer simultaneously; Soaking time deficiency or Heating temperature are too low, can not form the metallurgical binding of reinforcement particle and aluminum substrate in matrix material; Pressing pressure is larger on matrix material pressed compact density and internal stress impact; Rate of temperature fall and pressure directly affect the safe release of matrix material internal stress and the formation of crack defect.Therefore sintering process is directly connected to physicals and the mechanical property of matrix material.
Because the fusing point of aluminum silicon alloy is lower, in SiCp/Al-30Si matrix material hot pressed sintering preparation technology, the most rambunctious is exactly Heating temperature and soaking time.The metallurgical binding that realizes enhanced granule and matrix needs higher sintering temperature, and high temperature is grown up seriously the silicon grain of separating out in matrix, even causes at pressed compact top layer precipitating metal aluminium.Suitable sintering range is narrow, only has 10 ℃.Meanwhile, the rear internal stress of compacting has proposed stricter requirement to pressing pressure and rate of temperature fall in a vacuum.
Summary of the invention
The object of this invention is to provide the Aluminum Matrix Composites Strengthened by SiC that a kind of density is high.
Another object of the present invention is to provide a kind of Aluminum Matrix Composites Strengthened by SiC, to improve the density of matrix material, avoids the appearance of pore, defects i.e.cracks.
In order to realize above object, the technical scheme that Aluminum Matrix Composites Strengthened by SiC of the present invention adopts is: a kind of Aluminum Matrix Composites Strengthened by SiC, to be made by the raw material of following volume percent: 325 object silicon carbide powder 20-25%, surplus is 500 object Al-30Si powdered alloys.
The preparation method of Aluminum Matrix Composites Strengthened by SiC of the present invention is as follows:
1) in the die cavity of heat-resisting die, apply releasing agent, after silicon carbide powder is mixed with Al-30Si powdered alloy, pack in mould, mould is put into vacuum heating-press sintering equipment and vacuumize, adopt field 40MPa pressure the mixed powder in mould is carried out to precompressed;
2) remain lower to mold heated in vacuum and 40MPa pressure, in 30 minutes, be warming up to 250 ℃ and keep 30 minutes by room temperature; In 30 minutes, be warming up to 400 ℃ and keep 30 minutes by 250 ℃ again; Then in 30 minutes, be warming up to 560-570 ℃ of maintenance by 400 ℃, pressure is adjusted into 60MPa, every pressurization stops pressurizeing 20 minutes in 1 hour, is so repeatedly incubated altogether 3～4 hours, stops heating;
3) by mould cooling naturally in vacuum heating-press sintering equipment, keep 60MPa pressure in temperature-fall period, temperature stops pressurization while being down to 350 ℃ always, continue nature and be cooled to 200 ℃ of insulations, adjusting pressure is 80MPa insulation 30 minutes, stops pressurization, is cooled to room temperature;
4) take out mould, the demoulding obtains matrix material.
Described silicon carbide powder and Al-30Si powdered alloy adopt planetary ball mill to carry out batch mixing.
In described planetary ball mill, ratio of grinding media to material is 1: 1, and mixing time is 2-3h.
Described releasing agent is to be mixed by 75wt% graphite and 25wt% machine oil.
The described vacuum tightness vacuumizing is 0.01～0.02Pa.
Described vacuum heating-press sintering equipment is vacuum brazing machine.
Aluminum Matrix Composites Strengthened by SiC of the present invention is to be formed by silicon carbide powder and Al-30Si powdered alloy mixing compacting sintering, and wherein silicon-carbide particle is too little, in sintering process, easily reunites, and composite material toughness that particle obtains when too large is poor, intensity is low; And aluminum silicon alloy powder particle is when too large, in the matrix material obtaining, can separate out a large amount of primary silicons, be irregular large bulk, performance is reduced; The influence factor of dense structure's maximum is sintering pressure.Therefore select the granularity of silicon carbide powder and Al-30Si powdered alloy to adopt respectively 325 orders and 500 orders, select silicon carbide powder and the Al-30Si powdered alloy of suitable combination of particle size easy of tight in compacting sintering process, avoid the appearance of pore, defects i.e.cracks, can improve the compactness of matrix material.
In addition, the present invention proposes a kind of preparation method who prepares Aluminum Matrix Composites Strengthened by SiC in vacuum heating-press sintering equipment.Mixed powder is put into mould, moulding stock adopts refractory steel, the technique means that adopts stage intensification, stage pressurization compacting and pressurization compacting to combine, be beneficial to composite temperature even, be beneficial to mobile, Shi Qi dense structure, stage cooling is beneficial to stress relief, is unlikely to occur crackle.Preparation technology of the present invention has further improved the compactness of matrix material, further avoid the appearance of matrix material pore, defects i.e.cracks, a difficult problem that solved that in matrix material preparation process, metallic aluminium is separated out, silicon is grown up mutually, reinforcement particle and matrix is difficult for realizing metallurgical binding.
Accompanying drawing explanation
Fig. 1 is the organization chart of embodiment 1;
Fig. 2 is the organization chart of embodiment 2;
Fig. 3 is the organization chart of embodiment 3.
Embodiment
Embodiment 1
The Aluminum Matrix Composites Strengthened by SiC (SiCp/Al-30Si matrix material) of the present embodiment is to be that 325 object SiC powder and 500 object Al-30Si powdered alloys are composited by granularity, silicon carbide powder volume fraction is 20%, and surplus is Al-30Si powdered alloy.
The present embodiment matrix material is prepared in vacuum brazing machine, and step is as follows:
1) on planetary ball mill, will carry out batch mixing and obtain mixed powder, wherein ratio of grinding media to material is 1: 1, and mixing time is 2h;
2, apply releasing agent (75wt% graphite+25wt% machine oil) at the die cavity internal surface of refractory steel sintering mold, mixed powder is packed in mould, mould is put into vacuum brazing machine, opening device, be evacuated down to 0.02Pa, adopt the pressure of 40MPa to carry out precompressed to the mixed powder in mould;
3, remain lower at vacuum and 40MPa pressure the mould in soldering oven is heated, control heat-up rate, in 30 minutes, be warmed up to 250 ℃, be incubated 30 minutes; Continue to heat up, while reaching 400 ℃ after 30 minutes, be incubated 30 minutes; Continue subsequently to heat up, when temperature is raised to 560 ℃ in 30 minutes, stop heating up; Improve pressing pressure to 60MPa, every pressurization 1h stops pressurizeing 20 minutes, is so repeatedly incubated 4 hours, stops heating;
4, mould, with stove cooling in soldering oven, maintains pressure 60MPa always in temperature-fall period, and when temperature drops to 350 ℃, dwell, when temperature drops to 200 ℃, improves pressing pressure to 80MPa, and pressure heat-preserving 30 minutes again, stops pressurization, cools to room temperature;
5, closing device, opens soldering oven and takes out mould, and the matrix material after sintering is deviate from from die cavity.
The composite product homogeneous microstructure obtaining, density is high, flawless and gas hole defect, tensile strength reaches 230MPa, and tissue is shown in Fig. 1.
Embodiment 2
The Aluminum Matrix Composites Strengthened by SiC (SiCp/Al-30Si matrix material) of the present embodiment is to be that 325 object SiC powder and 500 object Al-30Si powdered alloys are composited by granularity, silicon carbide powder volume fraction is 23%, and surplus is Al-30Si powdered alloy.
The present embodiment matrix material is prepared in vacuum brazing machine, and step is as follows:
1, on planetary ball mill, carry out batch mixing and obtain mixed powder, wherein ratio of grinding media to material is 1: 1, and mixing time is 2.5h;
2, apply releasing agent (75wt% graphite+25wt% machine oil) at the die cavity internal surface of refractory steel sintering mold, mixed powder is packed in mould, mould is put into vacuum brazing machine.Opening device, is evacuated down to 0.02Pa, adopts the pressure of 40MPa to carry out precompressed to the mixed powder in mould;
3, remain lower at vacuum and 40MPa pressure the mould in soldering oven is heated, control heat-up rate, in 30 minutes, be warmed up to 250 ℃, be incubated 30 minutes; Continue to heat up, while reaching 400 ℃ after 30 minutes, be incubated 30 minutes; Continue subsequently to heat up, when temperature is raised to 570 ℃ in 30 minutes, stop heating up; Improve pressing pressure to 60MPa, every pressurization 1h stops pressurizeing 20 minutes, is incubated 3 hours, stops heating;
4, mould, with stove cooling in soldering oven, maintains pressure 60MPa always in temperature-fall period, and when temperature drops to 350 ℃, dwell, when temperature drops to 200 ℃, improves pressing pressure to 80MPa, again pressurizes 30 minutes, stops pressurization, cools to room temperature;
5, closing device, opens soldering oven and takes out mould, and the matrix material after sintering is deviate from from die cavity.
The composite product homogeneous microstructure obtaining, density is high, flawless and gas hole defect, tensile strength reaches 197MPa, and tissue is shown in Fig. 2.
Embodiment 3
The Aluminum Matrix Composites Strengthened by SiC (SiCp/Al-30Si matrix material) of the present embodiment is to be that 325 object SiC powder and 500 object Al-30Si powdered alloys are composited by granularity, silicon carbide powder volume fraction is 25%, and surplus is Al-30Si powdered alloy.
The present embodiment matrix material is prepared in vacuum brazing machine, and step is as follows:
1, on planetary ball mill, carry out batch mixing and obtain mixed powder, wherein ratio of grinding media to material is 1: 1, and mixing time is 3h;
2, apply releasing agent (75wt% graphite+25wt% machine oil) at the die cavity internal surface of refractory steel sintering mold, mixed powder is packed in mould, mould is put into vacuum brazing machine.Opening device, is evacuated down to 0.01Pa, adopts the pressure of 40MPa to carry out precompressed to the mixed powder in mould.
3, remain lower at vacuum and 40MPa pressure the mould in soldering oven is heated, control heat-up rate, in 30 minutes, be warmed up to 250 ℃, be incubated 30 minutes; Continue to heat up, while reaching 400 ℃ after 30 minutes, be incubated 30 minutes; Continue subsequently to heat up, when temperature is raised to 565 ℃ in 30 minutes, stop heating up; Improve pressing pressure to 60MPa, every pressurization 1h stops pressurizeing 20 minutes, is incubated 3.5 hours, stops heating;
4, mould, with stove cooling in soldering oven, maintains pressure 60MPa always in temperature-fall period, and when temperature drops to 350 ℃, dwell, when temperature drops to 200 ℃, improves pressing pressure to 80MPa, again pressurizes 30 minutes, stops pressurization, cools to room temperature;
5, closing device, opens soldering oven and takes out mould, and the matrix material after sintering is deviate from from die cavity.
The composite product homogeneous microstructure obtaining, density is high, flawless and gas hole defect, tensile strength reaches 183MPa, and tissue is shown in Fig. 3.
Claims (7)
1. an Aluminum Matrix Composites Strengthened by SiC, is characterized in that: be to be made up of the raw material of following volume percent: 325 object silicon carbide powder 20-25%, and surplus is 500 object Al-30Si powdered alloys;
This Aluminum Matrix Composites Strengthened by SiC is prepared by following methods:
1) in the die cavity of heat-resisting die, apply releasing agent, after silicon carbide powder is mixed with Al-30Si powdered alloy, pack in mould, mould is put into vacuum heating-press sintering equipment and vacuumize, adopt 40MPa pressure to carry out precompressed to the mixed powder in mould;
2) remain lower to mold heated in vacuum and 40MPa pressure, in 30 minutes, be warming up to 250 ℃ and keep 30 minutes by room temperature; In 30 minutes, be warming up to 400 ℃ and keep 30 minutes by 250 ℃ again; Then in 30 minutes, be warming up to 560-570 ℃ of maintenance by 400 ℃, pressure is adjusted into 60MPa, every pressurization stops pressurizeing 20 minutes in 1 hour, is so repeatedly incubated altogether 3～4 hours, stops heating;
3) by mould cooling naturally in vacuum heating-press sintering equipment, keep 60MPa pressure in temperature-fall period, temperature stops pressurization while being down to 350 ℃ always, continue nature and be cooled to 200 ℃ of insulations, adjusting pressure is 80MPa insulation 30 minutes, stops pressurization, is cooled to room temperature;
4) take out mould, the demoulding obtains matrix material.
2. a preparation method for Aluminum Matrix Composites Strengthened by SiC as claimed in claim 1, is characterized in that: its step is as follows:
1) in the die cavity of heat-resisting die, apply releasing agent, after silicon carbide powder is mixed with Al-30Si powdered alloy, pack in mould, mould is put into vacuum heating-press sintering equipment and vacuumize, adopt 40MPa pressure to carry out precompressed to the mixed powder in mould;
2) remain lower to mold heated in vacuum and 40MPa pressure, in 30 minutes, be warming up to 250 ℃ and keep 30 minutes by room temperature; In 30 minutes, be warming up to 400 ℃ and keep 30 minutes by 250 ℃ again; Then in 30 minutes, be warming up to 560-570 ℃ of maintenance by 400 ℃, pressure is adjusted into 60MPa, every pressurization stops pressurizeing 20 minutes in 1 hour, is so repeatedly incubated altogether 3～4 hours, stops heating;
3) by mould cooling naturally in vacuum heating-press sintering equipment, keep 60MPa pressure in temperature-fall period, temperature stops pressurization while being down to 350 ℃ always, continue nature and be cooled to 200 ℃ of insulations, adjusting pressure is 80MPa insulation 30 minutes, stops pressurization, is cooled to room temperature;
4) take out mould, the demoulding obtains matrix material.
3. the preparation method of Aluminum Matrix Composites Strengthened by SiC according to claim 2, is characterized in that: described silicon carbide powder and Al-30Si powdered alloy adopt planetary ball mill to carry out batch mixing.
4. the preparation method of Aluminum Matrix Composites Strengthened by SiC according to claim 3, is characterized in that: in described planetary ball mill, ratio of grinding media to material is 1: 1, and mixing time is 2-3h.
5. the preparation method of Aluminum Matrix Composites Strengthened by SiC according to claim 3, is characterized in that: described releasing agent is to be mixed by 75wt% graphite and 25wt% machine oil.
6. the preparation method of Aluminum Matrix Composites Strengthened by SiC according to claim 3, is characterized in that: described in the vacuum tightness that vacuumizes be 0.01～0.02Pa.
7. according to the preparation method of the Aluminum Matrix Composites Strengthened by SiC described in claim 3-6 any one, it is characterized in that: described vacuum heating-press sintering equipment is vacuum brazing machine.
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| CN109943755B (en) * | 2019-04-19 | 2021-03-23 | 中国兵器科学研究院宁波分院 | Preparation method of aluminum-based composite material for electronic packaging |
| CN112267039B (en) * | 2020-10-10 | 2022-02-01 | 中国科学院金属研究所 | Preparation process of high volume fraction silicon carbide particle reinforced aluminum matrix composite |
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