CN110202135A - Nanostructure bimetallic oxide enhances NiAl base high strength at high temperature lubricating composite preparation method - Google Patents
Nanostructure bimetallic oxide enhances NiAl base high strength at high temperature lubricating composite preparation method Download PDFInfo
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- 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
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- 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
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Abstract
The invention discloses a kind of nanostructure bimetallic oxides to enhance NiAl base high strength at high temperature lubricating composite preparation method, nanostructure mixed-powder is prepared using high-energy ball milling method, nanostructure NiAl-BaO/TiO is then prepared using cold pressing treatment and vacuum heating-press sintering2Composite material, NiAl-BaO/TiO2The microhardness of composite material is 380~450HV, and compression strength is 1500~1700MPa.The present invention effectively improves the wetability between metal oxide and NiAl matrix using the composite material of vacuum hot pressing sintering technique preparation, improves the bond strength between oxide and matrix.BaO and TiO2It can react in high-temperature sintering process and generate BaTiO3High temperature solid lubricant realizes the high temperature lubrication property of material.Meanwhile tiny nano particle has the function of refined crystalline strengthening in composite material, can effectively increase the intensity of composite material, is successfully prepared a kind of high-strength lightweight high temperature lubricating composite material of nanostructure.
Description
Technical field
The invention belongs to high strength at high temperature lubricating composite technical fields, and in particular to a kind of nanostructure bimetallic oxidation
Object enhances NiAl base high strength at high temperature lubricating composite preparation method.
Background technique
In recent years, with the fast development of the new high-tech industries such as China's aerospace, nuclear industry, to high temperature, high load, height
More stringent requirements are proposed for the mechanics of military service material and tribological property under the extreme harsh working condition such as speed, such as: lightweight, resistance to
Higher temperature and wear-resisting, relative motion component intensity under severe conditions, wear-resisting and lubrication problem have become the entire dress of influence
The key problem in technology of standby reliability of operation and service life.Therefore, there is an urgent need to construct higher temperature with the rudimentary knowledge of materialogy
Under the conditions of high-strength lightweight high temperature lubricating composite material, to meet the hair of the new high-tech industries such as China's aerospace, nuclear industry
Exhibition demand.
The fusing point of NiAl intermetallic compound is higher, is 1638 DEG C, about 300 DEG C higher than common nickel base superalloy, than
Ni3Al intermetallic compound is about 250 DEG C high.Meanwhile lower (the 5.9g/cm of density of NiAl intermetallic compound3, it is nickel-base alloy
2/3), excellent performance meets China's new high-tech industry and proposes resistance to higher temperature and light-weighted to high-temperature composite material
It is required that.The use temperature of metal oxide high-temperature solid lubricant is higher, is with a wide range of applications.The interaction of BaO is joined
Number is smaller, and the greasy property under high temperature is preferable.But wetability of the metal oxide generally between metallic matrix is poor, material
Intensity it is generally lower, this largely will affect the application of material.
Summary of the invention
In view of the above-mentioned deficiencies in the prior art, the technical problem to be solved by the present invention is that providing a kind of nanostructure
Bimetallic oxide enhances NiAl base high strength at high temperature lubricating composite preparation method, utilizes BaO and TiO2During the sintering process
Reaction, generate BaTiO3High-temperature lubricant further increases the high temperature lubrication property of composite material, while can be effectively improved gold
The problem for belonging to wetability difference between oxide and NiAl matrix, improves the intensity of composite material.Nanometer in composite material simultaneously
Particle has the function of refined crystalline strengthening, can further improve the intensity of composite material.
The invention adopts the following technical scheme:
Nanostructure bimetallic oxide enhances NiAl base high strength at high temperature lubricating composite preparation method, and feature exists
In using high-energy ball milling method preparation nanostructure mixed-powder, then using cold pressing treatment and vacuum heating-press sintering preparation nanometer
Structure NiAl-BaO/TiO2Composite material, NiAl-BaO/TiO2The microhardness of composite material is 380~450HV, compression strength
For 1500~1700MPa.
Specifically, the following steps are included:
S1, by NiAl and BaO/TiO2Mixing is added ethyl alcohol and carries out ball-milling treatment；
S2, the powder of step S1 ball-milling treatment is fitted into graphite grinding tool, cold pressing treatment is then carried out on cold press, it is right
Powder carries out cold moudling；
S3, the powder after step S2 cold pressing treatment is subjected to vacuum heating-press sintering, obtains the uniform NiAl- of dense structure
BaO/TiO2High temperature lubricating composite material.
Further, in step S1, by mass percentage, NiAl is 75%~90%, BaO/TiO2For 10%~
25%.
Further, TiO2Molar ratio with BaO is 1:1.
Further, in step S1, ball-milling technology are as follows: ball material mass ratio is (8~12): 1, revolving speed is 200~300r/
Min, Ball-milling Time are 10~20h, the mixed-powder that sieve powder and drying and processing obtain.
Further, the partial size of mixed-powder is 10~50nm, and the temperature of drying and processing is 80~100 DEG C, the time 1
~2h.
Further, in step S2, the pressure of cold pressing treatment is 5~13MPa.
Further, in step S3, the vacuum degree of vacuum heating-press sintering is 1 × 10-2Pa~3 × 10-2Pa。
Further, sintering temperature be 1200~1400 DEG C, heating rate be 5~15 DEG C/min, soaking time be 1~
3h, pressure are 15~30MPa.
Specifically, the NiAl-BaO/TiO of preparation2Coefficient of friction of the composite material under 800 DEG C of hot conditions is 0.35,
Wear rate is 3.9 × 10-5mm3/Nm。
Compared with prior art, the present invention at least has the advantages that
A kind of preparation side of nanostructure bimetallic oxide enhancing NiAl base high strength at high temperature lubricating composite of the present invention
Method prepares nanostructure NiAl-BaO/TiO using vacuum hot pressing sintering technique2Composite material not only improves NiAl-BaO/
TiO2The institutional framework of composite material, realizes the high temperature lubrication property of composite material, and effectively increases composite material
Intensity, meanwhile, meet the light-weighted requirement of high-temperature lubricating material.
Further, BaO and TiO that the present invention adds in NiAl matrix2It can occur in high-temperature sintering process anti-
BaTiO should be generated3, it can be achieved that the high temperature lubrication property of composite material, while metal oxide and NiAl matrix can be effectively improved
Between wetability, improve the intensity of composite material.
Further, raw material powder is calculated as mass fraction, and NiAl is 75~90%, BaO/TiO2It is 10~25%,
Middle TiO2Molar ratio with BaO is that 1:1 can get high-strength high-temperature composite material compared with traditional same type composite material.
Further, by high-energy ball milling, the partial size of the mixed-powder of preparation is 10~50nm, and one side high-energy ball milling can
So that powder is uniformly mixed, it is ensured that microstructure of composite is uniform；On the other hand tiny nano particle has refined crystalline strengthening
Effect, can effectively improve the intensity of composite material.
Further, the present invention first by uniformly mixed powder on cold press cold pressing treatment, powder hot-pressing can be made to burn
First simple molding before knot, while excluding the gas in powder.
Further, on the one hand vacuum hot pressing sintering technique of the present invention can prevent material during the sintering process
The oxidation of material；On the other hand the finer and close material of tissue can be prepared, the consistency of material, Jin Erti can be significantly improved
The intensity of high material.
In conclusion the present invention has prepared a kind of nanostructure bimetallic oxide increasing using vacuum hot pressing sintering technique
Strong NiAl base high strength at high temperature lubricating composite.Compared with other metal oxides enhance metal-base composites, system of the present invention
Standby composite material effectively improves the wetability between metal oxide and NiAl matrix, improves between oxide and matrix
Bond strength.BaO and TiO2It can react in high-temperature sintering process and generate BaTiO3High temperature solid lubricant is realized
The high temperature lubrication property of material.Meanwhile tiny nano particle has the function of refined crystalline strengthening in composite material, can effectively improve
The intensity of composite material, is successfully prepared a kind of high-strength lightweight high temperature lubricating composite material of nanostructure.
Below by drawings and examples, technical scheme of the present invention will be described in further detail.
Detailed description of the invention
Fig. 1 is the institutional framework of composite material；
Fig. 2 is the compression curve of composite material；
Fig. 3 is the friction curve of composite material.
Specific embodiment
The present invention provides a kind of nanostructure bimetallic oxides to enhance NiAl base high strength at high temperature lubricating composite system
Preparation Method is prepared for the uniformly mixed powder of nanostructure using the method for high-energy ball milling, then uses cold pressing treatment and vacuum
Hot pressing and sintering technique is prepared for nanostructure NiAl-BaO/TiO2Composite material effectively improves metal oxide and NiAl base
The problem of wetability difference, significantly improves the compression strength of composite material between body.BaO and TiO2It can in high-temperature sintering process
BaTiO is generated to react3High temperature solid lubricant, and then realize the high temperature lubrication property of material.Composite material it is micro-
Hardness is 380~450HV, and compression strength reaches 1500~1700MPa, and the coefficient of friction under 800 DEG C of hot conditions is 0.35,
Wear rate is 3.9 × 10-5mm3/ Nm, has successfully prepared a kind of high-strength lightweight high temperature lubricating composite material, and the present invention utilizes
Refined crystalline strengthening theory and BaO and TiO2Reaction in-situ during the sintering process realizes the high temperature lubrication property of composite material, together
When effectively improve the institutional framework of wetability and composite material between metal oxide and NiAl matrix, effectively increase gold
Belong to the bond strength between oxide and NiAl matrix, significantly improves the compression strength of composite material, realize composite material
High-strength, lightweight and high temperature lubrication property.
A kind of nanostructure bimetallic oxide of the present invention enhances NiAl base high strength at high temperature lubricating composite preparation method,
Nanostructure mixed-powder is prepared by high-energy ball milling, is successfully prepared the nanostructure composite material that each object is mutually evenly distributed,
Utilize BaO and TiO2It reacts in high-temperature sintering process and generates BaTiO3High temperature solid lubricant realizes composite material
High temperature lubrication property, meanwhile, the problem of wetability difference between metal oxide and NiAl matrix is effectively improved, is significantly improved
The microhardness and compression strength of composite material, while realizing the performance of composite material high strength, lightweight and high temperature lubricating.Tool
Steps are as follows for body:
S1, mixed-powder are with when ball milling
Powder is weighed by the ingredient design proportion of composite material, is calculated by mass percentage, NiAl is 75%~90%,
BaO/TiO2It is 10%~25%, wherein TiO2Molar ratio with BaO is 1:1；
The mixed-powder weighed up is placed in zirconium dioxide ball grinder, a certain amount of ethyl alcohol is added, on high energy ball mill
Carry out ball milling；
Ball-milling technology are as follows: ball material mass ratio is (8~12): 1,200~300r/min of revolving speed, and Ball-milling Time is 10~20h,
After ball milling, sieve powder simultaneously carries out drying and processing, and the partial size of mixed-powder is 10~50nm, and the temperature of drying and processing is 80~
100 DEG C, the time is 1~2h；
S2, cold moudling
The good powder of ball milling mixing is fitted into graphite grinding tool first, cold pressing treatment is then carried out on cold press, to powder
End carries out cold moudling；The pressure of cold pressing treatment is 5~13MPa.
S3, vacuum heating-press sintering
Powder after cold pressing treatment is subjected to vacuum heating-press sintering in vacuum sintering funace, vacuum sintering funace
Vacuum degree is 1 × 10-2Pa~3 × 10-2Pa, sintering temperature are 1200~1400 DEG C, and heating rate is 5~15 DEG C/min, heat preservation
Time is 1~3h, and pressure is 15~30MPa, and acquisition dense structure is uniform, and microhardness is high, high-strength, lightweight high temperature lubricating is multiple
Condensation material.
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with the embodiment of the present invention
In attached drawing, technical scheme in the embodiment of the invention is clearly and completely described, it is clear that described embodiment is
A part of the embodiment of the present invention, instead of all the embodiments.The present invention being described and shown in usually here in attached drawing is real
The component for applying example can be arranged and be designed by a variety of different configurations.Therefore, below to the present invention provided in the accompanying drawings
The detailed description of embodiment be not intended to limit the range of claimed invention, but be merely representative of of the invention selected
Embodiment.Based on the embodiments of the present invention, those of ordinary skill in the art are obtained without creative efforts
The every other embodiment obtained, shall fall within the protection scope of the present invention.
Embodiment 1
Using the uniformly mixed nanostructure mixed-powder of the method preparation of high-energy ball milling；By mass percent 75%
The BaO/TiO of NiAl and 25%2It is put into zirconium dioxide ball grinder and carries out high-energy ball milling, ball material mass ratio is 8:1, and revolving speed is
200r/min, Ball-milling Time 10h, the partial size of mixed-powder are 10nm, and the temperature of drying and processing is 80 DEG C, time 1h, system
The powder mixed, is then fitted into graphite grinding tool by standby uniformly mixed nanostructure mixed-powder.
Before filling powder, one layer of graphite paper is first spread on graphite grinding tool wall, prevents powder viscous with graphite grinding tool during the sintering process
It is connected together.The mixed-powder of nanostructure has the function of refined crystalline strengthening, can effectively improve the intensity of composite material.Composite wood
The BaO/TiO added in material2On the one hand bimetallic oxide can effectively improve the intensity of composite material；On the other hand sintered
It can react in journey and generate BaTiO3High temperature solid lubricant is realized the high temperature lubrication property of composite material, while can be had
Effect improves the problem of wetability difference between oxide and NiAl matrix, effectively improves the intensity of composite material.
The pressure for controlling cold pressing treatment is 5MPa, and the vacuum degree of vacuum heating-press sintering is 1 × 10-2Pa, sintering temperature are
1200 DEG C, heating rate is 5 DEG C/min, soaking time 1h, pressure 15MPa, and composite material is made.
Each object is mutually distributed relatively uniform in the composite material of preparation, as shown in Figure 1.Add BaO/TiO2Bimetallic oxide
Afterwards, it is 429.8HV that the microhardness of composite material is increased by 251.6HV, has obtained significant raising, compression strength is
1500MPa.Compared with similar high temperature lubricating composite material, the microhardness of the composite material of preparation is also higher.
Embodiment 2
Using the uniformly mixed nanostructure mixed-powder of the method preparation of high-energy ball milling.By mass percent 85%
The BaO/TiO of NiAl and 15%2It is put into zirconium dioxide ball grinder and carries out high-energy ball milling, ball material mass ratio is 10:1, and revolving speed is
250r/min, Ball-milling Time 15h, the partial size of mixed-powder are 30nm, and the temperature of drying and processing is 90 DEG C, time 1.5h,
The powder mixed, is then fitted into graphite grinding tool by the uniformly mixed nanostructure mixed-powder of preparation.
Before filling powder, one layer of graphite paper is first spread on graphite grinding tool wall, prevents powder viscous with graphite grinding tool during the sintering process
It is connected together.The mixed-powder of nanostructure has the function of refined crystalline strengthening, can effectively improve the intensity of composite material.Composite wood
The BaO/TiO added in material2On the one hand bimetallic oxide can effectively improve the intensity of composite material；On the other hand sintered
It can react in journey and generate BaTiO3High temperature solid lubricant is realized the high temperature lubrication property of composite material, while can be had
Effect improves the problem of wetability difference between oxide and NiAl matrix, effectively improves the intensity of composite material.
The pressure for controlling cold pressing treatment is 9MPa, and the vacuum degree of vacuum heating-press sintering is 2 × 10-2Pa, sintering temperature are
1300 DEG C, heating rate is 10 DEG C/min, soaking time 2h, pressure 25MPa, and composite material is made.
Each object is mutually distributed relatively uniform in the composite material of preparation.Add BaO/TiO2After bimetallic oxide, composite wood
The microhardness of material is 380HV, has obtained significant raising, compression strength 1600MPa.With similar high temperature lubricating composite material
It compares, the microhardness of the composite material of preparation is also higher.
Embodiment 3
Using the uniformly mixed nanostructure mixed-powder of the method preparation of high-energy ball milling.By mass percent 90%
The BaO/TiO of NiAl and 10%2It is put into zirconium dioxide ball grinder and carries out high-energy ball milling, ball material mass ratio is 12:1, and revolving speed is
300r/min, Ball-milling Time 20h, the partial size of mixed-powder are 50nm, and the temperature of drying and processing is 100 DEG C, time 2h, system
The powder mixed, is then fitted into graphite grinding tool by standby uniformly mixed nanostructure mixed-powder.
Before filling powder, one layer of graphite paper is first spread on graphite grinding tool wall, prevents powder viscous with graphite grinding tool during the sintering process
It is connected together.The mixed-powder of nanostructure has the function of refined crystalline strengthening, can effectively improve the intensity of composite material.Composite wood
The BaO/TiO added in material2On the one hand bimetallic oxide can effectively improve the intensity of composite material；On the other hand sintered
It can react in journey and generate BaTiO3High temperature solid lubricant is realized the high temperature lubrication property of composite material, while can be had
Effect improves the problem of wetability difference between oxide and NiAl matrix, effectively improves the intensity of composite material.
The pressure for controlling cold pressing treatment is 13MPa, and the vacuum degree of vacuum heating-press sintering is 3 × 10-2Pa, sintering temperature are
1400 DEG C, heating rate is 15 DEG C/min, soaking time 3h, pressure 30MPa, and composite material is made.
Each object is mutually distributed relatively uniform in the composite material of preparation.Add BaO/TiO2After bimetallic oxide, composite wood
The microhardness of material is 450HV, has obtained significant raising, compression strength 1700MPa.With similar high temperature lubricating composite material
It compares, the microhardness of the composite material of preparation is also higher.
Embodiment 4
The composite material prepared to embodiment 1 is cut into compression sample, and specimen size isCompression examination
It tests and is carried out on universal testing machine, reliable and stable for guarantee test data, test is repeated 5 times.
Compression speed during compression test is 0.05mm/s.The addition of metal oxide effectively increases composite material
Compression strength, the compression strength of composite material is increased to 1486MPa by 1365MPa, as shown in Figure 2.With similar high temperature lubricating
Composite material is compared, and the composite material compression strength of preparation is even more to be significantly improved.
Embodiment 5
The composite material prepared to embodiment 1 is cut into high temperature friction sample, and specimen size isIt is high
Warm friction test carries out on UMT high-temperature friction testing machine, and friction test uses ball-disc type, and ball selects fusing point height, high-temperature stable
The good Al of property2O3, friction testing temperature is 800 DEG C, radius 5mm, revolving speed 200r/min, and the friction testing time is 1h.BaO
With TiO2It can react in high-temperature sintering process and generate BaTiO3High temperature solid lubricant realizes the high temperature of composite material
Greasy property.
It is 0.35 that test, which measures coefficient of friction of the composite material under 800 DEG C of hot conditions, and wear rate is 3.9 × 10- 5mm3/ Nm has apparent reduction compared with NiAl material, as shown in Figure 3.Compared with similar high temperature lubricating composite material, preparation is answered
The friction and wear behavior of condensation material at high temperature is more excellent.
The above content is merely illustrative of the invention's technical idea, and this does not limit the scope of protection of the present invention, all to press
According to technical idea proposed by the present invention, any changes made on the basis of the technical scheme each falls within claims of the present invention
Protection scope within.
Claims (10)
1. nanostructure bimetallic oxide enhances NiAl base high strength at high temperature lubricating composite preparation method, which is characterized in that
Nanostructure mixed-powder is prepared using high-energy ball milling method, nanostructure is then prepared using cold pressing treatment and vacuum heating-press sintering
NiAl-BaO/TiO2Composite material, NiAl-BaO/TiO2The microhardness of composite material is 380~450HV, and compression strength is
1500~1700MPa.
2. preparation method according to claim 1, which comprises the following steps:
S1, by NiAl and BaO/TiO2Mixing is added ethyl alcohol and carries out ball-milling treatment；
S2, the powder of step S1 ball-milling treatment is fitted into graphite grinding tool, cold pressing treatment is then carried out on cold press, to powder
Carry out cold moudling；
S3, the powder after step S2 cold pressing treatment is subjected to vacuum heating-press sintering, obtains the uniform NiAl-BaO/ of dense structure
TiO2High temperature lubricating composite material.
3. preparation method according to claim 2, which is characterized in that in step S1, by mass percentage, NiAl is
75%~90%, BaO/TiO2It is 10%~25%.
4. preparation method according to claim 3, which is characterized in that TiO2Molar ratio with BaO is 1:1.
5. preparation method according to claim 2, which is characterized in that in step S1, ball-milling technology are as follows: ball material mass ratio is
(8~12): 1, revolving speed is 200~300r/min, and Ball-milling Time is 10~20h, the mixed-powder that sieve powder and drying and processing obtain.
6. preparation method according to claim 5, which is characterized in that the partial size of mixed-powder is 10~50nm, at drying
The temperature of reason is 80~100 DEG C, and the time is 1~2h.
7. preparation method according to claim 2, which is characterized in that in step S2, the pressure of cold pressing treatment is 5~
13MPa。
8. preparation method according to claim 2, which is characterized in that in step S3, the vacuum degree of vacuum heating-press sintering is 1
×10-2Pa~3 × 10-2Pa。
9. preparation method according to claim 8, which is characterized in that sintering temperature is 1200~1400 DEG C, heating rate
For 5~15 DEG C/min, soaking time is 1~3h, and pressure is 15~30MPa.
10. preparation method according to claim 1, which is characterized in that the NiAl-BaO/TiO of preparation2Composite material is 800
Coefficient of friction under DEG C hot conditions is 0.35, and wear rate is 3.9 × 10-5mm3/Nm。
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