CN106834870A - Ni‑Al2O3Composite near-net-shape method - Google Patents
Ni‑Al2O3Composite near-net-shape method Download PDFInfo
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- CN106834870A CN106834870A CN201710079953.5A CN201710079953A CN106834870A CN 106834870 A CN106834870 A CN 106834870A CN 201710079953 A CN201710079953 A CN 201710079953A CN 106834870 A CN106834870 A CN 106834870A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
- C22C29/12—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on oxides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/115—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by spraying molten metal, i.e. spray sintering, spray casting
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
- B22F3/15—Hot isostatic pressing
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/001—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides
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Abstract
The invention provides a kind of Ni Al2O3The near-net-shape method of composite, by carbonyl Ni powder, Al2O3、Y2O3Kneaded with binding agent after obtaining mixed material with MgO ball millings, obtain kneading material, injection moulding after mixing material granulation obtains shaping sample, then carries out degreasing, isostatic cool pressing, HIP sintering, obtains Ni Al2O3Composite, degreasing process and isostatic cool pressing, HIP sintering technique of the present invention after using ball-milling technology, calendering process, injection technique and injection prepares Ni Al2O3Composite, obtained Ni Al2O3Composite consistency is up to 99.9%, Vickers hardness 1788HV, bending strength 422MPa, fracture toughness 5.9MPam1/2, can be used to prepare the part of complicated shape, meet that all trades and professions high to precision, complex structure, toughness is high and requirement of complete fine and close part.
Description
Technical field
The present invention relates to ceramic-metal composite technical field, more particularly to a kind of Ni-Al2O3The near net of composite
Manufacturing process.
Background technology
Al2O3One of most abundant ceramics of current resource, with intensity it is high, resistivity is high, electrical insulating property good, hardness and
The base attribute such as fusing point is high, corrosion resistance is good, good in oxidation resistance, thermal coefficient of expansion are small, can bear than metal material and high score
The harsher working environment of sub- material, plays an important role in fields such as machinery, chemical industry, medical science, Aero-Space.But by
In fragility it is big, difficulty of processing is big the shortcomings of, the application of aluminum oxide is limited by very large, and Metal toughened alumina base is compound
Material possesses great application space.
Nickel is one of most widely used metal simple-substance, with fabulous corrosion resistance, toughness, ductility, thermal conductivity and
Electric conductivity.The fusing point of nickel is 1453 DEG C, belongs to medium melting point metals system, and compared to low-melting-point metal, nickel has preferable high temperature
Performance, compared to refractory metal, nickel has preferable toughness in high intensity.Metal nickel particle is introduced into aluminium oxide ceramics matrix
It is interior, can not only in many ways hinder the extension of matrix cracking, such as the extraction of the passivation of crackle, deflection, pinning and metallic
Deng so that the bending strength and fracture toughness of composite ceramics are improved, and also improve the sintering character of aluminium oxide ceramics.
Ni-Al is prepared in the prior art2O3The method of ceramic-metal composite is hot-forming method, such as Liu Xun
Disclose with hot pressing for Ni nanoparticle-Al2O3Metal ceramic powder, Ni particles are evenly distributed on Al2O3In matrix, effective ground resistance
Al is stopped2O3The growing up of matrix grain (referring to《Ni nanoparticle-Al2O3Metal ceramic powder hot-pressing densification process》, Liu Xun etc., in
Southern college journal (natural science edition), 2004,35 (1):21-25)；Gu Sidi is disclosed with Al2O3With Ni (NO3)2·6H2O is
Initial feed, Al is prepared using hot pressed sintering2O3/ Ni metallic toughness reinforcing nano composite ceramics method (referring to《Ni particles are more
Dissipate toughness reinforcing Al2O3The preparation of based nano complex phase ceramic and performance study》, Gu Sidi, Tsing-Hua University, 2004).But these are traditional
It is compressing prepare cermet can only the relatively simple part of shaping form, to produce special-shaped part also needs by follow-up
Machining.
The content of the invention
In view of this, it is an object of the invention to provide a kind of Ni-Al2O3The near-net-shape method of composite, can obtain
To the cermet part of complicated shape, can be used for the fields such as textile machine.
In order to realize foregoing invention purpose, the present invention provides following technical scheme：
A kind of Ni-Al2O3The near-net-shape method of composite, comprises the following steps：
(1) by carbonyl Ni powder, Al2O3、Y2O3With MgO ball millings, mixed material is obtained；
(2) mixed material for obtaining the step (1) is kneaded with binding agent, obtains kneading material；
(3) injection moulding after the mixing material granulation for obtaining the step (2), obtains shaping sample；
(4) the shaping sample degreasing for obtaining the step (3), obtains degreasing idiosome；
(5) the degreasing idiosome that the step (4) is obtained is carried out into isostatic cool pressing, obtains isostatic cool pressing sample；
(6) the isostatic cool pressing sample that the step (5) is obtained is carried out into HIP sintering, obtains Ni-Al2O3Composite wood
Material.
Preferably, mixed material includes the component of following weight/mass percentage composition in the step (1)：Carbonyl Ni powder 8~
12%th, Al2O387~91%, Y2O30.2~0.5% and MgO 0.2~0.5%.
Preferably, binding agent includes the component of following weight/mass percentage composition in the step (2)：60~70% paraffin, 8
~12% ethylene-vinyl acetate copolymer, 18~22% low density polyethylene (LDPE) and 4~6% stearic acid.
Preferably, the temperature of mixing is 145~160 DEG C in the step (2), and the time of the mixing is 1~2h.
Preferably, the temperature of injection moulding is 140~160 DEG C in the step (3), and the pressure of the injection moulding is 80
~100MPa, the time of the injection moulding is 6~10s.
Preferably, the temperature of degreasing degreasing solvent is 30~60 DEG C in the step (4), and the time of the degreasing is 1
~9h.
Preferably, the degreasing in the step (4) includes：The shaping sample is carried out into first paragraph thermal debinding, the successively
Two sections of thermal debindings, the 3rd section of thermal debinding, the 4th section of thermal debinding and the 5th section of thermal debindings；
The first paragraph thermal debinding is that room temperature carries out first paragraph insulation to 200~220 DEG C, is warming up to the first paragraph
The time of thermal debinding is 150~180min, and the time of the first paragraph insulation is 50~70min；
The second segment thermal debinding is warming up to 340~370 DEG C and carries out second segment insulation for 200~220 DEG C, is warming up to described
The heating-up time of second segment thermal debinding is 180~220min, and the time of the second segment insulation is 50~70min；
The 3rd section of thermal debinding is warming up to 415~435 DEG C and carries out the 3rd section of insulation for 340~370 DEG C, is warming up to described
3rd time of thermal debinding is 105~125min, and the time of the 3rd section of insulation is 50~70min；
The 4th section of thermal debinding is warming up to 490~510 DEG C and carries out the 4th section of insulation for 415~435 DEG C, is warming up to described
4th time of thermal debinding is 65~85min, and the time of the 4th section of insulation is 50~70min；
The 5th section of thermal debinding is warming up to 200~220 DEG C and carries out the 5th section of insulation for 490~510 DEG C, is warming up to described
5th time of thermal debinding is 50~70min, and the time of the 5th section of insulation is 20~30min.
Preferably, the pressure of isostatic cool pressing is 250~300MPa in the step (5), and the time of the isostatic cool pressing is 3
~10min.
Preferably, the pressure of HIP sintering is 150~200MPa, the HIP sintering in the step (6)
Temperature be 1350~1450 DEG C, time of the HIP sintering is 1~2h.
Preferably, also include after the completion of HIP sintering in the step (6)：The HIP sintering sample that will be obtained
Cooling, the speed of the cooling is 10~30 DEG C/min.
The invention provides a kind of Ni-Al2O3The near-net-shape method of composite, by carbonyl Ni powder, Al2O3、Y2O3With
MgO ball millings are kneaded after obtaining mixed material with binding agent, obtain kneading material, wherein Y2O3With MgO as sintering aid, have
The effect of crystal grain thinning, acceleration of sintering, injection moulding after mixing material granulation obtains shaping sample, then carries out degreasing, cold etc.
Static pressure, HIP sintering, obtain Ni-Al2O3Composite, the present invention is by using ball-milling technology, calendering process, injection work
Degreasing process and isostatic cool pressing, HIP sintering technique after skill and injection prepare Ni-Al2O3Composite, injection moulding
The defects such as the shaping sample for obtaining is without shorting, crackle, overlap, shaping sample global density than more uniform, blank after degreasing without
Defect.The result of the embodiment of the present invention shows, the Ni-Al that the method that the present invention is provided is obtained2O3The consistency of composite material parts
Up to 99.9%, Vickers hardness 1788HV, bending strength 422MPa, fracture toughness 5.9MPam1/2, can be used in preparing complexity
The part of shape, meets that all trades and professions high to precision, complex structure, small volume, toughness is high and requirement of complete fine and close part.
Brief description of the drawings
The present invention is further detailed explanation with reference to the accompanying drawings and detailed description.
Fig. 1 is Ni-Al of the present invention2O3The flow chart of the near-net-shape method of composite；
Fig. 2 is the ESEM spectrogram of mixed material after the ball milling of the embodiment of the present invention 1；
Fig. 3 is the ESEM spectrogram that the embodiment of the present invention 1 kneads material；
Fig. 4 is the ESEM spectrogram of the degreasing idiosome of the embodiment of the present invention 1；
Fig. 5 is the image of the isostatic cool pressing sample of the embodiment of the present invention 1；
Fig. 6 is Ni-Al obtained in the embodiment of the present invention 12O3The ESEM spectrogram of composite；
Fig. 7 is Ni-Al obtained in the embodiment of the present invention 22O3The ESEM spectrogram of composite；
Fig. 8 is Ni-Al obtained in the embodiment of the present invention 32O3The ESEM spectrogram of composite.
Specific embodiment
The invention provides a kind of Ni-Al2O3The near-net-shape method of composite, comprises the following steps：
(1) by carbonyl Ni powder, Al2O3、Y2O3With MgO ball millings, mixed material is obtained；
(2) mixed material for obtaining the step (1) is kneaded with binding agent, obtains kneading material；
(3) injection moulding after the mixing material granulation for obtaining the step (2), obtains shaping sample；
(4) the shaping sample degreasing for obtaining the step (3), obtains degreasing idiosome；
(5) the degreasing idiosome that the step (4) is obtained is carried out into isostatic cool pressing, obtains isostatic cool pressing sample；
(6) the isostatic cool pressing sample that the step (5) is obtained is carried out into HIP sintering, obtains Ni-Al2O3Composite wood
Material.
The present invention is by carbonyl Ni powder, Al2O3、Y2O3With MgO ball millings, mixed material is obtained.
The present invention is to the carbonyl Ni powder, Al2O3、Y2O3With MgO source without any special limitation, using ability
Rule of origin or commercial goods known to field technique personnel.
In the present invention, the Al2O3Specific surface area be preferably 5.8~7.6m2/ g, more preferably 6.7~7.5m2/ g,
Most preferably 6.9~7.3m2/g；The Al2O3Particle mean size be preferably 0.36~0.84 μm, more preferably 0.48~0.6 μ
m；The Al in embodiments of the present invention2O3Performance it is as shown in table 1.
The inventive embodiments Al of table 12O3Performance parameter
In the present invention, the Fisher particle size of the carbonyl Ni powder is preferably 3~7 μm, more preferably 4~5 μm；In the present invention
The performance of the powder of carbonyl Ni described in embodiment is as shown in table 2.
The embodiment of the present invention of table 2 performance parameter of carbonyl Ni powder
In the present invention, the Y2O3Particle mean size be preferably 30~50nm, more preferably 35~40nm.
In the present invention, the Fisher particle size of the MgO is preferably 30~50nm, more preferably 35~40nm.
In the present invention, the mixed material preferably includes the component of following weight/mass percentage composition：Carbonyl Ni powder 8~
12%th, Al2O387~91%, Y2O30.2~0.5% and MgO 0.2~0.5%；More preferably include carbonyl Ni powder 9~11%,
Al2O388~90%, Y2O30.2~0.5% and MgO 0.2~0.5%.
The present invention is by carbonyl Ni powder, Al2O3、Y2O3, ball milling after MgO mixing, the present invention do not appoint to the mode of the ball milling
What special restriction, using ball milling method well known to those skilled in the art；In embodiments of the present invention preferably in agate
Ball milling is carried out in tank with agate ball, the agate ball is preferably 10~40 with the mass ratio of mixed material: 1, more preferably 20~
30：1；The medium that the ball milling is used preferably absolute ethyl alcohol or acetone, the medium are preferably 5~20 with the mass ratio of raw material
: 1, more preferably 8~16：1, most preferably 10~12：1.
In the present invention, the rotating speed of the ball milling is preferably 260~360r/min, more preferably 280~340r/min, most
Preferably 300~320r/min；The time of the ball milling be preferably 5~35h, more preferably 15~30h, most preferably 20~
25h。
After obtaining mixed material, the present invention kneads the mixed material and binding agent, obtains kneading material.
In the present invention, the mixed material is preferably 5~20 with the mass ratio of binding agent：1, more preferably 8~17：1,
Most preferably 9~15：1.
In the present invention, the binding agent preferably includes the component of following weight/mass percentage composition：60~70% paraffin, 8
~12% ethylene-vinyl acetate copolymer, 18~22% low density polyethylene (LDPE) and 4~6% stearic acid；More preferably wrap
Include：62~68% paraffin, 9~11% ethylene-vinyl acetate copolymer, 18.5~21.5% low density polyethylene (LDPE) and
4.5~5.5% stearic acid.
In the present invention, the low density polyethylene (LDPE) decomposition temperature is high, is difficult to be reacted with organic solvent, is typically chosen heat point
Solution is removed.
In the present invention, the preparation method of the binding agent preferably includes following steps：By the ethylene-vinyl acetate
Copolymer and low density polyethylene (LDPE) melt under the conditions of 130~150 DEG C, obtain high-melting-point fused materials；By the paraffin and firmly
Resin acid melts under the conditions of 55~70 DEG C, obtains molten low melting point material；By the high-melting-point fused materials and molten low melting point
Material mixes, that is, obtain binding agent.
In the present invention, the melt temperature of the ethylene-vinyl acetate copolymer and low density polyethylene (LDPE) is preferably 134
~145 DEG C, more preferably 135~144 DEG C；The paraffin and stearic melt temperature are preferably 58~66 DEG C, more preferably
60~62 DEG C；The high-melting-point fused materials are preferably 139~147 DEG C with the mixing temperature of molten low melting point material, more preferably
It is 140~145 DEG C.
The present invention does not have any special restriction to the mode of the mixing, using mixing well known to those skilled in the art
Mode；Carried out preferably in feeding machine in embodiments of the present invention, specifically mix the mixed material with binding agent
After be added in feeding machine.
In the present invention, the temperature of the mixing is preferably 145~160 DEG C, more preferably 146~157 DEG C.The mixing
Time be preferably 1~2h, more preferably 1.2~1.8h.
The present invention does not have any special restriction to the hybrid mode and charging sequence of the mixed material and binding agent, adopts
With hybrid mode well known to those skilled in the art and charging sequence；The binding agent is preferably pressed in embodiments of the present invention
Weight is divided into two parts, is added at twice in the mixed material.
After obtaining mixing material, injection moulding after the mixing material granulation is obtained shaping sample by the present invention.
The present invention does not have special restriction to the method for the granulation, using granulation mode well known to those skilled in the art
；Carried out preferably in comminutor in the present invention.
In the present invention, the particle diameter that the granulation obtains granule materials is preferably 1~5mm, more preferably 1.5~2.5mm.
It is of the invention by the granule materials injection moulding after obtaining granule materials.In the present invention, the injection moulding
Temperature is preferably 140~160 DEG C, more preferably 148~158 DEG C；The pressure of the injection moulding is preferably 80~100MPa, more
Preferably 85~95MPa；The time of the injection moulding is preferably 6~10s, more preferably 7~9s.
In the present invention, preferred pair mould is preheated in the injection moulding, and the preheating temperature of the mould is preferably
40~55 DEG C, more preferably 48~52 DEG C；The shape to the mould does not have any special limitation in the present invention, according to need
Voluntarily to select the mould of suitable shape.
After obtaining shaping sample, the shaping sample degreasing is obtained degreasing idiosome by the present invention.In the present invention, it is described
Degreasing preferably uses solvent-thermal debinding method.
In the present invention, the temperature of the degreasing degreasing solvent is preferably 30~60 DEG C, more preferably 35~50 DEG C；Institute
The time for stating degreasing is preferably 1~9h, more preferably 2~7h.
In the present invention, the degreasing solvent is preferably the one kind in normal heptane, trichloro ethylene and n-hexane；The degreasing
Solvent is preferably 10~20 with the mass ratio of shaping sample：1, more preferably 14~18：1, most preferably 15~17：1.
In the present invention, the degreasing preferably specifically includes following steps：The shaping sample is carried out into first paragraph successively
Thermal debinding, second segment thermal debinding, the 3rd section of thermal debinding, the 4th section of thermal debinding and the 5th section of thermal debinding；
The first paragraph thermal debinding is that room temperature carries out first paragraph insulation to 200~220 DEG C, is warming up to the first paragraph
The time of thermal debinding is preferably 150~180min, more preferably 160~170min, and the time of first insulation is preferably 50
~70min, more preferably 60~65min；
The second segment thermal debinding is warming up to 340~370 DEG C and carries out second segment insulation for 200~220 DEG C, is warming up to described
The heating-up time of second segment thermal debinding is preferably 180~220min, more preferably 200~210min, the second segment insulation
Time is preferably 50~70min, more preferably 55~65min；
The 3rd section of thermal debinding is warming up to 415~435 DEG C and carries out the 3rd section of insulation for 340~370 DEG C, is warming up to described
The time of the 3rd section of thermal debinding is preferably 105~125min, more preferably 110~120min, the time of the 3rd section of insulation
It is 50~70min, more preferably 55~65min；
The 4th section of thermal debinding is warming up to 490~510 DEG C and carries out the 4th section of insulation for 415~435 DEG C, is warming up to described
The time of the 4th section of thermal debinding is preferably 65~85min, more preferably 70~75min, and the time of the 4th section of insulation is 50
~70min, more preferably 55~65min；
The 5th section of thermal debinding is warming up to 200~220 DEG C and carries out the 5th section of insulation for 490~510 DEG C, is warming up to described
The time of the 5th section of thermal debinding is preferably 50~70min, more preferably 55~65min, and the time of the 5th section of insulation is preferred
It is 20~30min, more preferably 23~28min.
In the present invention, the degreasing blank that will preferably be obtained after the degreasing is cooled to room temperature, and the present invention is to the cooling
Mode there is no any special limitation, using the type of cooling well known to those skilled in the art；In the embodiment of the present invention
In preferably by the way of natural cooling.
After obtaining degreasing idiosome, the degreasing idiosome is carried out isostatic cool pressing by the present invention, obtains isostatic cool pressing sample.
In the present invention, the pressure of the isostatic cool pressing is preferably 250~300MPa, more preferably 255~288MPa, most
Preferably 257~284MPa；The time of the isostatic cool pressing is preferably 3~10min, more preferably 4~8min.
After obtaining isostatic cool pressing sample, the isostatic cool pressing sample is carried out HIP sintering by the present invention, obtains Ni-
Al2O3Composite.
In the present invention, the pressure of the HIP sintering is preferably 150~200MPa, more preferably 160~
180MPa；The temperature of the HIP sintering is preferably 1350~1450 DEG C, more preferably 1380~1440 DEG C；Described heat etc.
The time of static pressure sintering is preferably 1~2h, more preferably 1.2~1.8h.
In the present invention, the high temperature insostatic pressing (HIP) sample cooling that will preferably be obtained after the HIP sintering, obtains Ni-Al2O3
Composite.In the present invention, the speed of the cooling is preferably 10~30 DEG C/min, more preferably 13~28 DEG C/min, most
Preferably 15~27 DEG C/min.
Fig. 1 is Ni-Al of the present invention2O3The flow chart of the near-net-shape method of composite, by carbonyl Ni powder, Al2O3、Y2O3
Kneaded with binding agent after obtaining mixed material with MgO ball millings, obtain kneading material, injection moulding after mixing material granulation is obtained
Shaping sample, then carries out degreasing, isostatic cool pressing, HIP sintering, obtains Ni-Al2O3Composite.
The invention provides a kind of Ni-Al2O3The near-net-shape method of composite, by carbonyl Ni powder, Al2O3、Y2O3With
MgO ball millings are kneaded after obtaining mixed material with binding agent, obtain kneading material, wherein Y2O3With MgO as sintering aid, have
The effect of crystal grain thinning, acceleration of sintering, injection moulding after mixing material granulation obtains shaping sample, then carries out degreasing, cold etc.
Static pressure, HIP sintering, obtain Ni-Al2O3Composite, the present invention is by using ball-milling technology, calendering process, injection work
Degreasing process and isostatic cool pressing, HIP sintering technique after skill and injection prepare Ni-Al2O3Composite, injection moulding
The defects such as the shaping sample for obtaining is without shorting, crackle, overlap, shaping sample global density than more uniform, blank after degreasing without
Defect.The result of the embodiment of the present invention shows, the Ni-Al that the method that the present invention is provided is obtained2O3The consistency of composite material parts
Up to 99.9%, Vickers hardness 1788HV, bending strength 422MPa, fracture toughness 5.9MPam1/2, can be used in preparing complexity
The part of shape, meets that all trades and professions high to precision, complex structure, small volume, toughness is high and requirement of complete fine and close part.
With reference to the Ni-Al that embodiment is provided the present invention2O3The near-net-shape method of composite is carried out specifically
It is bright, but they can not be interpreted as limiting the scope of the present invention.
Embodiment 1
According to carbonyl Ni powder 8%, Al2O391%th, Y2O30.5% and MgO 0.5% mixes raw material, and carbonyl Ni powder takes
Family name's granularity is 3 μm, Al2O3Specific surface area be 5.8m2/ g, particle mean size is preferably 0.36 μm, Y2O3Particle mean size be 30nm,
The Fisher particle size of MgO is 30nm, and mixed material is carried out into ball milling in agate pot, using alcohol as ball-milling medium, selected ball
Grinding process parameter is：Ratio of grinding media to material：10：1；Rotational speed of ball-mill：260r/min；Ball-milling Time：35h.Mixed-powder after ball milling is entered
Row scanning electron microscope analysis, as a result as shown in fig. 2, it can be seen that carbonyl Ni powder is in Al2O3In be well mixed.
Binding agent is wax-based binder system, and binder formula is：60% paraffin, 12% ethylene-vinyl acetate copolymerization
Thing, 22% low density polyethylene (LDPE), 6% stearic acid, first by ethylene-vinyl acetate copolymer in binding agent and low density polyethylene (LDPE)
Component is melted, and then again melts paraffin and stearic acid, and binding agent is obtained after mixing, is taken binding agent 20g and is divided into two parts
It is separately added into the mixed material 200g after fusing, obtains kneading material, Fig. 3 is the ESEM spectrogram for kneading material, by Fig. 3
As can be seen that each component is well mixed in mixing material.
Mixed material obtains the material that particle diameter is 1mm in adding comminutor, then in 140 DEG C of temperature, pressure 80MPa, note
Time 6s, dwell pressure 50MPa are penetrated, then injection moulding at 40 DEG C of mold preheating temperature carries out solvent-thermal debinding, degreasing
Time is 9h, and trichloro ethylene skimming temp is 30 DEG C, and the heating curve of thermal debinding is：200 DEG C are warming up to through 150min at room temperature,
50min is incubated at 200 DEG C, then 340 DEG C are warming up to by 180min, 50min is incubated at 340 DEG C, then by 105min liters
Temperature is incubated 50min to 415 DEG C at 415 DEG C, then is warming up to 490 DEG C by 65min, 50min is incubated at 490 DEG C, then pass through
50min is warming up to 560 DEG C, and 20min is incubated at 560 DEG C, finally naturally cools to room temperature, obtains degreasing idiosome, and Fig. 4 is degreasing
The scanning electron microscope image of blank afterwards, as seen from Figure 4, the blank zero defect after degreasing.
To degreasing idiosome in isostatic cool pressing is carried out under pressurize 3min under 250MPa, Fig. 5 is blank after isostatic cool pressing treatment
Image, as seen from Figure 5, the surface zero defect of the blank after isostatic cool pressing treatment, then in 1350 DEG C, the work of 150MPa
Then pressure, soaking time 1h is cooled to room temperature with 10 DEG C/min, obtains Ni-Al2O3Composite, Fig. 6 burns for high temperature insostatic pressing (HIP)
The scanning electron microscope image of sample section after knot, as seen from Figure 6, sample tissue is fine and close after HIP sintering, is evenly distributed.
To the Ni-Al for obtaining2O3Composite carries out microstructure observation and is measured with mechanical property, Ni-Al2O3Composite wood
Material consistency is 99.9%, and Vickers hardness is up to 1788HV, and bending strength is 422MPa, fracture toughness 5.9MPam1/2。
Embodiment 2
According to carbonyl Ni powder 12%, Al2O387%th, Y2O30.5% and MgO 0.5% mixes raw material, and carbonyl Ni powder takes
Family name's granularity is 7 μm, Al2O3Specific surface area be 7.6m2/ g, particle mean size is preferably 0.84 μm, Y2O3Particle mean size be 50nm,
The Fisher particle size of MgO is 50nm, and mixed material is carried out into ball milling in agate pot, using acetone as ball-milling medium, selected ball
Grinding process parameter is：Ratio of grinding media to material：40：1；Rotational speed of ball-mill：360r/min；Ball-milling Time：5h.
Binding agent is wax-based binder system, and binder formula is：70% paraffin, 8% ethylene-vinyl acetate copolymerization
Thing, 18% low density polyethylene (LDPE), 4% stearic acid, first by ethylene-vinyl acetate copolymer in binding agent and low density polyethylene (LDPE)
Component is melted, and then again melts paraffin and stearic acid, and binding agent is obtained after mixing, is taken binding agent 18g and is divided into two parts
It is separately added into the mixed material 200g after fusing, obtains kneading material.
Mixed material obtains the material that particle diameter is 5mm in adding comminutor, then in 160 DEG C of temperature, pressure 100MPa, note
Time 10s, dwell pressure 80MPa are penetrated, then injection moulding at 55 DEG C of mold preheating temperature carries out solvent-thermal debinding, degreasing
Time is 1h, and normal heptane skimming temp is 60 DEG C, and the heating curve of thermal debinding is：220 DEG C are warming up to through 180min at room temperature,
70min is incubated at 220 DEG C, then 370 DEG C are warming up to by 220min, 70min is incubated at 370 DEG C, then heat up by 125min
To 435 DEG C, 70min is incubated at 435 DEG C, then 510 DEG C are warming up to by 85min, 70min is incubated at 510 DEG C, then pass through
70min is warming up to 700 DEG C, and 30min is incubated at 700 DEG C, finally naturally cools to room temperature, obtains degreasing idiosome.
To degreasing idiosome in isostatic cool pressing is carried out under pressurize 10min under 300MPa, then in 1450 DEG C, the work of 200MPa
Then pressure, soaking time 2h is cooled to room temperature with 30 DEG C/min, obtains Ni-Al2O3Composite, Fig. 7 burns for high temperature insostatic pressing (HIP)
The scanning electron microscope image of sample section after knot, as seen from Figure 7, sample tissue is fine and close after HIP sintering, is evenly distributed.
To the Ni-Al for obtaining2O3Composite carries out microstructure observation and is measured with mechanical property, Ni-Al2O3Composite wood
Material consistency is 99.1%, and Vickers hardness is up to 1781HV, and bending strength is 420MPa, fracture toughness 5.79MPam1/2。
Embodiment 3
According to carbonyl Ni powder 10%, Al2O389%th, Y2O30.5% and MgO 0.5% mixes raw material, and carbonyl Ni powder takes
Family name's granularity is 3.5 μm, Al2O3Specific surface area be 6.8m2/ g, particle mean size is preferably 0.4 μm, Y2O3Particle mean size be
The Fisher particle size of 35nm, MgO is 40nm, and mixed material is carried out into ball milling in agate pot, using acetone as ball-milling medium, is selected
Milling parameters be：Ratio of grinding media to material：20：1；Rotational speed of ball-mill：300r/min；Ball-milling Time：28h.
Binding agent is wax-based binder system, and binder formula is：66% paraffin, 9% ethylene-vinyl acetate copolymerization
Thing, 20% low density polyethylene (LDPE), 5% stearic acid, first by ethylene-vinyl acetate copolymer in binding agent and low density polyethylene (LDPE)
Component is melted, and then again melts paraffin and stearic acid, and binding agent is obtained after mixing, is taken binding agent 21g and is divided into two parts
It is separately added into the mixed material 200g after fusing, obtains kneading material.
Mixed material obtains the material that particle diameter is 3mm in adding comminutor, then in 150 DEG C of temperature, pressure 90MPa, note
Time 8s, dwell pressure 70MPa are penetrated, then injection moulding at 50 DEG C of mold preheating temperature carries out solvent-thermal debinding, degreasing
Time is 2h, and normal heptane skimming temp is 50 DEG C, and the heating curve of thermal debinding is：210 DEG C are warming up to through 160min at room temperature,
70min is incubated at 210 DEG C, then 350 DEG C are warming up to by 210min, 40min is incubated at 350 DEG C, then heat up by 115min
To 410 DEG C, 50min is incubated at 410 DEG C, then 500 DEG C are warming up to by 80min, 60min is incubated at 500 DEG C, then pass through
60min is warming up to 690 DEG C, and 40min is incubated at 690 DEG C, finally naturally cools to room temperature, obtains degreasing idiosome.
To degreasing idiosome in isostatic cool pressing is carried out under pressurize 8min under 280MPa, then in 1400 DEG C, the work of 180MPa
Then pressure, soaking time 1.5h is cooled to room temperature with 20 DEG C/min, obtains Ni-Al2O3Composite, Fig. 8 is high temperature insostatic pressing (HIP)
The scanning electron microscope image of sample section after sintering, as seen from Figure 8, sample tissue is fine and close after HIP sintering, and distribution is equal
It is even.
To the Ni-Al for obtaining2O3Composite carries out microstructure observation and is measured with mechanical property, Ni-Al2O3Composite wood
Material consistency is 99.4%, and Vickers hardness is up to 1779HV, and bending strength is 419MPa, fracture toughness 5.85MPam1/2。
The above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (10)
1. a kind of Ni-Al2O3The near-net-shape method of composite, comprises the following steps：
(1) by carbonyl Ni powder, Al2O3、Y2O3With MgO ball millings, mixed material is obtained；
(2) mixed material for obtaining the step (1) is kneaded with binding agent, obtains kneading material；
(3) injection moulding after the mixing material granulation for obtaining the step (2), obtains shaping sample；
(4) the shaping sample degreasing for obtaining the step (3), obtains degreasing idiosome；
(5) the degreasing idiosome that the step (4) is obtained is carried out into isostatic cool pressing, obtains isostatic cool pressing sample；
(6) the isostatic cool pressing sample that the step (5) is obtained is carried out into HIP sintering, obtains Ni-Al2O3Composite.
2. near-net-shape method according to claim 1, it is characterised in that in the step (1) mixed material include with
The component of lower weight/mass percentage composition：Carbonyl Ni powder 8~12%, Al2O387~91%, Y2O30.2~0.5% and MgO 0.2~
0.5%.
3. near-net-shape method according to claim 1, it is characterised in that binding agent includes following in the step (2)
The component of weight/mass percentage composition：60~70% paraffin, 8~12% ethylene-vinyl acetate copolymer, 18~22% it is low
Density polyethylene and 4~6% stearic acid.
4. the near-net-shape method according to claim 1 or 3, it is characterised in that the temperature of mixing is in the step (2)
145~160 DEG C, the time of the mixing is 1~2h.
5. near-net-shape method according to claim 1, it is characterised in that the temperature of injection moulding in the step (3)
It it is 140~160 DEG C, the pressure of the injection moulding is 80~100MPa, and the time of the injection moulding is 6~10s.
6. near-net-shape method according to claim 1, it is characterised in that degreasing degreasing solvent in the step (4)
Temperature be 30~60 DEG C, time of the degreasing is 1~9h.
7. method according to claim 6, it is characterised in that the degreasing in the step (4) includes：The shaping is tried
Sample carries out first paragraph thermal debinding, second segment thermal debinding, the 3rd section of thermal debinding, the 4th section of thermal debinding and the 5th section of thermal debinding successively；
The first paragraph thermal debinding is that room temperature carries out first paragraph insulation to 200~220 DEG C, is warming up to the first paragraph heat de-
The time of fat is 150~180min, and the time of the first paragraph insulation is 50~70min；
The second segment thermal debinding is warming up to 340~370 DEG C and carries out second segment insulation for 200~220 DEG C, is warming up to described second
The heating-up time of section thermal debinding is 180~220min, and the time of the second segment insulation is 50~70min；
The 3rd section of thermal debinding for 340~370 DEG C be warming up to 415~435 DEG C carry out the 3rd section insulation, be warming up to the described 3rd
The time of section thermal debinding is 105~125min, and the time of the 3rd section of insulation is 50~70min；
The 4th section of thermal debinding for 415~435 DEG C be warming up to 490~510 DEG C carry out the 4th section insulation, be warming up to the described 4th
The time of section thermal debinding is 65~85min, and the time of the 4th section of insulation is 50~70min；
The 5th section of thermal debinding for 490~510 DEG C be warming up to 200~220 DEG C carry out the 5th section insulation, be warming up to the described 5th
The time of section thermal debinding is 50~70min, and the time of the 5th section of insulation is 20~30min.
8. method according to claim 1, it is characterised in that in the step (5) pressure of isostatic cool pressing be 250~
300MPa, the time of the isostatic cool pressing is 3~10min.
9. near-net-shape method according to claim 1, it is characterised in that HIP sintering in the step (6)
Pressure is 150~200MPa, and the temperature of the HIP sintering is 1350~1450 DEG C, the time of the HIP sintering
It is 1~2h.
10. the near-net-shape method according to claim 1 or 9, it is characterised in that high temperature insostatic pressing (HIP) burns in the step (6)
Also include after knot：The HIP sintering sample cooling that will be obtained, the speed of the cooling is 10~30 DEG C/min.
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