CN108101520A - Alundum (Al2O3)-composite material of silicon carbide and preparation method thereof - Google Patents
Alundum (Al2O3)-composite material of silicon carbide and preparation method thereof Download PDFInfo
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Abstract
The present invention provides a kind of preparation methods of alundum (Al2O3) composite material of silicon carbide, it is characterised in that：Preparation method includes the following steps：Al is provided2O3Powder, SiC powder and Si3N4Powder；By Al2O3Powder, SiC powder and Si3N4Powder carries out the first ball milling, obtains the first mixed-powder；Ti powder, Ni powder and Co powder are provided；Ti powder, Ni powder and Co powder are subjected to the second ball milling, obtain the second mixed-powder；First reductive heat treatment is carried out to the second mixed-powder, obtains the 3rd mixed-powder；First mixed-powder with the 3rd mixed-powder is mixed and carries out the 3rd ball milling, obtains the 4th mixed-powder, wherein in the 4th mixed-powder, the mass percent of the first mixed-powder is 85 95%；Second reductive heat treatment is carried out to the second mixed-powder, obtains the 5th mixed-powder；Isostatic cool pressing is carried out to the 5th mixed-powder, so as to sheet forming；And microwave sintering is carried out to plate.Fracture toughness, hardness and the bending strength of the alundum (Al2O3) composite material of silicon carbide of the present invention are good, product excellent combination property.
Description
Technical field
The present invention relates to field of compound material, more particularly to a kind of alundum (Al2O3)-composite material of silicon carbide and its preparation
Method.
Background technology
Aluminium oxide ceramics be develop it is relatively early, using a kind of wide ceramic material, it have high temperature resistant, high rigidity,
Corrosion-resistant, wear-resistant, the advantages that density is small, cheap.But aluminium oxide fracture toughness it is relatively low the shortcomings that limit the wide of it
General application.The shortcomings that in order to overcome aluminium oxide fracture toughness relatively low, the prior art propose the toughening side of many aluminium oxide ceramics
Method and principle, wherein it is more representational including：Have yttria stabilizator, fiber and crystal whisker toughened, zirconium oxide transformation toughening,
Composite toughening and self toughening etc..Wherein, alundum (Al2O3)-composite material of silicon carbide be exactly it is a kind of than it is more typical have toughening
The aluminium oxide ceramics of characteristic, for further toughening, some prior arts are proposed is made pottery using mullite crystal whisker toughened aluminum oxide
The defects of technology of porcelain, this technology, is：1st, the mixing of mullite crystal whisker and alundum (Al2O3)-silicon carbide powder is relatively more tired
Difficulty, the two are difficult to be uniformly mixed, this causes unstable product quality；2nd, just because of mullite crystal whisker and alundum (Al2O3)-carbon
The mixing of SiClx powder is difficult, so when powder and whisker quality are larger, the two cannot form uniform mixing substantially, which has limited
The commercial application of this material；3rd, mullite crystal whisker higher price causes production cost higher.
The information for being disclosed in the background section is merely intended to increase the understanding of the general background to the present invention, without answering
When being considered as recognizing or imply that the information structure has been the prior art well known to persons skilled in the art in any form.
The content of the invention
It is an object of the invention to provide a kind of alundum (Al2O3)-composite material of silicon carbide and preparation method thereof, thus gram
The shortcomings that taking the prior art.
To achieve the above object, the present invention provides a kind of preparation method of alundum (Al2O3)-composite material of silicon carbide,
It is characterized in that：Preparation method includes the following steps：Al is provided2O3Powder, SiC powder and Si3N4Powder；By Al2O3Powder, SiC powder and
Si3N4Powder carries out the first ball milling, obtains the first mixed-powder；Ti powder, Ni powder and Co powder are provided；By Ti powder, Ni powder and Co powder
The second ball milling is carried out, obtains the second mixed-powder；First reductive heat treatment is carried out to the second mixed-powder, obtains the 3rd mixed powder
End；First mixed-powder with the 3rd mixed-powder is mixed and carries out the 3rd ball milling, obtains the 4th mixed-powder, wherein the 4th
In mixed-powder, the mass percent of the first mixed-powder is 85-95%；Second mixed-powder is carried out at the second heat of reduction
Reason, obtains the 5th mixed-powder；Isostatic cool pressing is carried out to the 5th mixed-powder, so as to sheet forming；And plate is carried out micro-
Ripple is sintered.
Preferably, in above-mentioned technical proposal, by weight percentage, Al2O3The quality of powder accounts for the first mixed-powder quality
The quality of 40-50%, SiC powder accounts for the 40-45% of the first mixed-powder quality, surplus Si3N4Powder.
Preferably, in above-mentioned technical proposal, the technique of the first ball milling is specially：Drum's speed of rotation is 500-700rpm, ball
It consumes time as 2-3h.
Preferably, in above-mentioned technical proposal, by weight percentage, the quality of Ti powder accounts for the second mixed-powder quality
The quality of 30-40%, Ni powder accounts for the 30-40% of the second mixed-powder quality, and surplus is Co powder.
Preferably, in above-mentioned technical proposal, the technique of the second ball milling is specially：Drum's speed of rotation is 1000-1500rpm,
Ball-milling Time is 15-25h.
Preferably, in above-mentioned technical proposal, the technique of the first reductive heat treatment is specially：Heat-treating atmosphere is hydrogen, heat
Treatment temperature is 600-700 DEG C, heat treatment time 40-70min.
Preferably, in above-mentioned technical proposal, the technique of the 3rd ball milling is specially：Drum's speed of rotation is 1000-1500rpm,
Ball-milling Time is 4-5h.
Preferably, in above-mentioned technical proposal, the technique of the second reductive heat treatment is specially：Heat-treating atmosphere is hydrogen, heat
Treatment temperature is 800-900 DEG C, heat treatment time 40-70min.
Preferably, in above-mentioned technical proposal, the concrete technology of microwave sintering is：Microwave sintering atmosphere is argon gas, and microwave is burnt
Junction temperature is 1200-1350 DEG C, sintering time 20-25min.
The present invention also provides a kind of alundum (Al2O3)-composite material of silicon carbide, which is by such as claim
Prepared by aforementioned preparation process.
Compared with prior art, the present invention has the advantages that：1st, with metal powder instead of mullite crystal whisker, experiment
The mixing for showing metal powder and alundum (Al2O3)-silicon carbide powder is easier, it is possible to which reducing Ball-milling Time simultaneously can be with
Manufacture the larger product of gross mass；2nd, the present invention devises a kind of new technology powder component, and experiment shows this metal mixed
Powder, the fracture toughness of raising alundum (Al2O3)-composite material of silicon carbide that can be by a relatively large margin；3rd, made by reductive heat treatment
Long-time ball milling can be carried out by obtaining, and ensure the exact chemical ingredient of product, improve properties of product；4th, three oxidation of optimization
The ingredient of two aluminum/silicon carbide composite materials improves mechanical property.
Specific embodiment
Unless otherwise explicitly stated, otherwise in entire disclosure and claims, term " comprising " or its change
It changes such as "comprising" or " including " etc. and will be understood to comprise stated element or component, and do not exclude other members
Part or other components.The device of the invention is the device of this field routine, and raw material used in the present invention can be purchased
From chemical products shop, fracture toughness, bending strength, hardness test are carried out with reference to the countries concerned's standard.
Embodiment 1
Alundum (Al2O3)-composite material of silicon carbide is prepared in the following manner：Al is provided2O3Powder, SiC powder and Si3N4
Powder；By Al2O3Powder, SiC powder and Si3N4Powder carries out the first ball milling, obtains the first mixed-powder；Ti powder, Ni powder and Co are provided
Powder；Ti powder, Ni powder and Co powder are subjected to the second ball milling, obtain the second mixed-powder；First is carried out to the second mixed-powder also
Original heat treatment, obtains the 3rd mixed-powder；First mixed-powder with the 3rd mixed-powder is mixed and carries out the 3rd ball milling, is obtained
4th mixed-powder, wherein in the 4th mixed-powder, the mass percent of the first mixed-powder is 85%；To the second mixed powder
End carries out the second reductive heat treatment, obtains the 5th mixed-powder；Isostatic cool pressing is carried out to the 5th mixed-powder, so as to profiled sheeting
Material；And microwave sintering is carried out to plate.By weight percentage, Al2O3The quality of powder accounts for the first mixed-powder quality
The quality of 40%, SiC powder accounts for the 40% of the first mixed-powder quality, surplus Si3N4Powder.The technique of first ball milling is specially：Ball
Mill speed is 500rpm, Ball-milling Time 3h.By weight percentage, the quality of Ti powder accounts for the second mixed-powder quality
The quality of 30%, Ni powder accounts for the 30% of the second mixed-powder quality, and surplus is Co powder.The technique of second ball milling is specially：Ball milling
Machine rotating speed is 1000rpm, Ball-milling Time 25h.The technique of first reductive heat treatment is specially：Heat-treating atmosphere is hydrogen, heat
Treatment temperature is 600 DEG C, heat treatment time 70min.The technique of 3rd ball milling is specially：Drum's speed of rotation is 1000, ball milling
Time is 5h.The technique of second reductive heat treatment is specially：Heat-treating atmosphere is hydrogen, and heat treatment temperature is 800 DEG C, heat treatment
Time is 70min.The concrete technology of microwave sintering is：Microwave sintering atmosphere is argon gas, and microwave sintering temperature is 1200 DEG C, sintering
Time is 25min.
Embodiment 2
Alundum (Al2O3)-composite material of silicon carbide is prepared in the following manner：Al is provided2O3Powder, SiC powder and Si3N4
Powder；By Al2O3Powder, SiC powder and Si3N4Powder carries out the first ball milling, obtains the first mixed-powder；Ti powder, Ni powder and Co are provided
Powder；Ti powder, Ni powder and Co powder are subjected to the second ball milling, obtain the second mixed-powder；First is carried out to the second mixed-powder also
Original heat treatment, obtains the 3rd mixed-powder；First mixed-powder with the 3rd mixed-powder is mixed and carries out the 3rd ball milling, is obtained
4th mixed-powder, wherein in the 4th mixed-powder, the mass percent of the first mixed-powder is 95%；To the second mixed powder
End carries out the second reductive heat treatment, obtains the 5th mixed-powder；Isostatic cool pressing is carried out to the 5th mixed-powder, so as to profiled sheeting
Material；And microwave sintering is carried out to plate.By weight percentage, Al2O3The quality of powder accounts for the first mixed-powder quality
The quality of 50%, SiC powder accounts for the 45% of the first mixed-powder quality, surplus Si3N4Powder.The technique of first ball milling is specially：Ball
Mill speed is 700rpm, Ball-milling Time 2h.By weight percentage, the quality of Ti powder accounts for the second mixed-powder quality
The quality of 40%, Ni powder accounts for the 40% of the second mixed-powder quality, and surplus is Co powder.The technique of second ball milling is specially：Ball milling
Machine rotating speed is 1500rpm, Ball-milling Time 15h.The technique of first reductive heat treatment is specially：Heat-treating atmosphere is hydrogen, heat
Treatment temperature is 700 DEG C, heat treatment time 40min.The technique of 3rd ball milling is specially：Drum's speed of rotation is 1500rpm, ball
It consumes time as 4h.The technique of second reductive heat treatment is specially：Heat-treating atmosphere is hydrogen, and heat treatment temperature is 900 DEG C, at heat
The reason time is 40min.The concrete technology of microwave sintering is：Microwave sintering atmosphere is argon gas, and microwave sintering temperature is 1350 DEG C, is burnt
The knot time is 20min.
Embodiment 3
Alundum (Al2O3)-composite material of silicon carbide is prepared in the following manner：Al is provided2O3Powder, SiC powder and Si3N4
Powder；By Al2O3Powder, SiC powder and Si3N4Powder carries out the first ball milling, obtains the first mixed-powder；Ti powder, Ni powder and Co are provided
Powder；Ti powder, Ni powder and Co powder are subjected to the second ball milling, obtain the second mixed-powder；First is carried out to the second mixed-powder also
Original heat treatment, obtains the 3rd mixed-powder；First mixed-powder with the 3rd mixed-powder is mixed and carries out the 3rd ball milling, is obtained
4th mixed-powder, wherein in the 4th mixed-powder, the mass percent of the first mixed-powder is 90%；To the second mixed powder
End carries out the second reductive heat treatment, obtains the 5th mixed-powder；Isostatic cool pressing is carried out to the 5th mixed-powder, so as to profiled sheeting
Material；And microwave sintering is carried out to plate.By weight percentage, Al2O3The quality of powder accounts for the first mixed-powder quality
The quality of 45%, SiC powder accounts for the 45% of the first mixed-powder quality, surplus Si3N4Powder.The technique of first ball milling is specially：Ball
Mill speed is 600rpm, Ball-milling Time 2.5h.By weight percentage, the quality of Ti powder accounts for the second mixed-powder quality
The quality of 30-40%, Ni powder accounts for the 35% of the second mixed-powder quality, and surplus is Co powder.The technique of second ball milling is specially：Ball
Mill speed is 1200rpm, Ball-milling Time 20h.The technique of first reductive heat treatment is specially：Heat-treating atmosphere is hydrogen,
Heat treatment temperature is 650 DEG C, heat treatment time 60min.The technique of 3rd ball milling is specially：Drum's speed of rotation is 1200rpm,
Ball-milling Time is 4.5h.The technique of second reductive heat treatment is specially：Heat-treating atmosphere is hydrogen, and heat treatment temperature is 850 DEG C,
Heat treatment time is 60min.The concrete technology of microwave sintering is：Microwave sintering atmosphere is argon gas, and microwave sintering temperature is 1300
DEG C, sintering time 20min.
Embodiment 4
First mixed-powder only has Al2O3Powder and SiC powder, Al2O3The quality of powder accounts for the 50% of the first mixed-powder quality,
The quality of SiC powder accounts for the 50% of the first mixed-powder quality, remaining condition, parameter, step, ingredient are same as Example 3.
Embodiment 5
Second mixed-powder only has Ti powder and Ni powder, and the quality of Ti powder accounts for 50%, the Ni powder of the second mixed-powder quality
Quality accounts for the 50% of the second mixed-powder quality, remaining condition, parameter, step, ingredient are same as Example 3.
Embodiment 6
Without the first reductive heat treatment, the 3rd ball milling, remaining condition, parameter, step, ingredient and embodiment are directly carried out
3 is identical.
Embodiment 7
Without the second reductive heat treatment, isostatic cool pressing is directly carried out, remaining condition, parameter, step, ingredient and embodiment
3 is identical.
Embodiment 8
The mass percent of first mixed-powder is 80%, remaining condition, parameter, step, ingredient are same as Example 3.
Embodiment 9
Hot pressed sintering is carried out to plate, specific hot-pressing sintering technique is：1300-1400 DEG C of sintering temperature, pressure 50-
100MPa, sintering time 5-6h, remaining condition, parameter, step, ingredient are same as Example 3.
Embodiment 10
Al2O3The quality of powder accounts for the 35% of the first mixed-powder quality, remaining condition, parameter, step, ingredient and embodiment 3
It is identical.
Embodiment 11
The quality of SiC powder accounts for the 35% of the first mixed-powder quality, remaining condition, parameter, step, ingredient and embodiment 3
It is identical.
Embodiment 12
The technique of first ball milling is specially：Drum's speed of rotation is 400rpm, Ball-milling Time 5h, remaining condition, parameter, step
Suddenly, ingredient is same as Example 3.
Embodiment 13
The quality of Ti powder accounts for the 25% of the second mixed-powder quality, remaining condition, parameter, step, ingredient and 3 phase of embodiment
Together.
Embodiment 14
The quality of Ti powder accounts for the 45% of the second mixed-powder quality, remaining condition, parameter, step, ingredient and 3 phase of embodiment
Together.
Embodiment 15
The quality of Ni powder accounts for the 25% of the second mixed-powder quality, remaining condition, parameter, step, ingredient and 3 phase of embodiment
Together.
Embodiment 16
The quality of Ni powder accounts for the 45% of the second mixed-powder quality, remaining condition, parameter, step, ingredient and 3 phase of embodiment
Together.
Embodiment 17
The technique of second ball milling is specially：Drum's speed of rotation is 800rpm, Ball-milling Time 35h, remaining condition, parameter,
Step, ingredient are same as Example 3.
Embodiment 18
The technique of first reductive heat treatment is specially：Heat-treating atmosphere is hydrogen, and heat treatment temperature is 550 DEG C, heat treatment
Time is 60min.Remaining condition, parameter, step, ingredient are same as Example 3.
Embodiment 19
The technique of first reductive heat treatment is specially：Heat-treating atmosphere is hydrogen, and heat treatment temperature is 750 DEG C, heat treatment
Time is 60min.Remaining condition, parameter, step, ingredient are same as Example 3.
Embodiment 20
The technique of first reductive heat treatment is specially：Heat-treating atmosphere is hydrogen, and heat treatment temperature is 650 DEG C, heat treatment
Time is 30min.Remaining condition, parameter, step, ingredient are same as Example 3.
Embodiment 21
The technique of 3rd ball milling is specially：Drum's speed of rotation is 1700rpm, Ball-milling Time 3h, remaining condition, parameter,
Step, ingredient are same as Example 3.
Embodiment 22
The technique of second reductive heat treatment is specially：Heat-treating atmosphere is hydrogen, and heat treatment temperature is 700 DEG C, heat treatment
Time is 60min.Remaining condition, parameter, step, ingredient are same as Example 3.
Embodiment 23
The technique of second reductive heat treatment is specially：Heat-treating atmosphere is hydrogen, and heat treatment temperature is 1000 DEG C, heat treatment
Time is 60min.Remaining condition, parameter, step, ingredient are same as Example 3.
Embodiment 24
The technique of second reductive heat treatment is specially：Heat-treating atmosphere is hydrogen, and heat treatment temperature is 850 DEG C, heat treatment
Time is 30min.Remaining condition, parameter, step, ingredient are same as Example 3.
Embodiment 25
The technique of second reductive heat treatment is specially：Heat-treating atmosphere is hydrogen, and heat treatment temperature is 850 DEG C, heat treatment
Time is 100min.Remaining condition, parameter, step, ingredient are same as Example 3.
Embodiment 26
The concrete technology of microwave sintering is：Microwave sintering atmosphere is argon gas, and microwave sintering temperature is 1100 DEG C, sintering time
For 100min.Remaining condition, parameter, step, ingredient are same as Example 3.
The test of fracture toughness, bending strength, hardness, test result row are carried out to the composite material of embodiment 1-26 manufactures
In table 1.Compare for convenience, above-mentioned each test result numerical value is normalized on the basis of the numerical value of embodiment 1.
Table 1
The description of the foregoing specific exemplary embodiment to the present invention is in order to illustrate and illustration purpose.These descriptions
It is not wishing to limit the invention to disclosed precise forms, and it will be apparent that according to the above instruction, can much be changed
And variation.The purpose of selecting and describing the exemplary embodiment is that explain that the certain principles of the present invention and its reality should
With so that those skilled in the art can realize and utilize the present invention a variety of exemplary implementation schemes and
Various chooses and changes.The scope of the present invention is intended to be limited by claims and its equivalents.
Claims (10)
1. a kind of preparation method of alundum (Al2O3)-composite material of silicon carbide, it is characterised in that：The preparation method includes as follows
Step：
Al is provided2O3Powder, SiC powder and Si3N4Powder；
By the Al2O3Powder, SiC powder and Si3N4Powder carries out the first ball milling, obtains the first mixed-powder；
Ti powder, Ni powder and Co powder are provided；
The Ti powder, Ni powder and Co powder are subjected to the second ball milling, obtain the second mixed-powder；
First reductive heat treatment is carried out to second mixed-powder, obtains the 3rd mixed-powder；
First mixed-powder with the 3rd mixed-powder is mixed and carries out the 3rd ball milling, obtains the 4th mixed-powder,
Wherein in the 4th mixed-powder, the mass percent of first mixed-powder is 85-95%；
Second reductive heat treatment is carried out to second mixed-powder, obtains the 5th mixed-powder；
Isostatic cool pressing is carried out to the 5th mixed-powder, so as to sheet forming；And
Microwave sintering is carried out to the plate.
2. preparation method as described in claim 1, it is characterised in that：By weight percentage, the Al2O3The quality of powder accounts for
The 40-50% of the first mixed-powder quality, the quality of the SiC powder account for the 40-45% of the first mixed-powder quality,
Surplus is the Si3N4Powder.
3. preparation method as described in claim 1, it is characterised in that：The technique of first ball milling is specially：Ball mill turns
Speed is 500-700rpm, Ball-milling Time 2-3h.
4. preparation method as described in claim 1, it is characterised in that：By weight percentage, the quality of the Ti powder accounts for institute
The 30-40% of the second mixed-powder quality is stated, the quality of the Ni powder accounts for the 30-40% of the second mixed-powder quality, remaining
It measures as the Co powder.
5. preparation method as described in claim 1, it is characterised in that：The technique of second ball milling is specially：Ball mill turns
Speed is 1000-1500rpm, Ball-milling Time 15-25h.
6. preparation method as described in claim 1, it is characterised in that：The technique of first reductive heat treatment is specially：Heat
Processing atmosphere is hydrogen, and heat treatment temperature is 600-700 DEG C, heat treatment time 40-70min.
7. preparation method as described in claim 1, it is characterised in that：The technique of 3rd ball milling is specially：Ball mill turns
Speed is 1000-1500rpm, Ball-milling Time 4-5h.
8. preparation method as described in claim 1, it is characterised in that：The technique of second reductive heat treatment is specially：Heat
Processing atmosphere is hydrogen, and heat treatment temperature is 800-900 DEG C, heat treatment time 40-70min.
9. preparation method as described in claim 1, it is characterised in that：The concrete technology of the microwave sintering is：Microwave sintering
Atmosphere is argon gas, and microwave sintering temperature is 1200-1350 DEG C, sintering time 20-25min.
10. a kind of alundum (Al2O3)-composite material of silicon carbide, it is characterised in that：The composite material is by such as claim 1-9
One of described in preparation method prepare.
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