CN107699764A - A kind of method of fabricated in situ Nano diamond enhancing iron nickel-base composite material and its resulting materials and application - Google Patents

A kind of method of fabricated in situ Nano diamond enhancing iron nickel-base composite material and its resulting materials and application Download PDF

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CN107699764A
CN107699764A CN201710906498.1A CN201710906498A CN107699764A CN 107699764 A CN107699764 A CN 107699764A CN 201710906498 A CN201710906498 A CN 201710906498A CN 107699764 A CN107699764 A CN 107699764A
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CN107699764B (en
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张法明
赵佩佩
刘腾飞
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Southeast University
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C26/00—Alloys containing diamond or cubic or wurtzitic boron nitride, fullerenes or carbon nanotubes
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/05—Mixtures of metal powder with non-metallic powder
    • C22C1/058—Mixtures of metal powder with non-metallic powder by reaction sintering (i.e. gasless reaction starting from a mixture of solid metal compounds)
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C33/00—Making ferrous alloys
    • C22C33/02—Making ferrous alloys by powder metallurgy
    • C22C33/0257—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements
    • C22C33/0278—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements with at least one alloying element having a minimum content above 5%
    • C22C33/0285—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements with at least one alloying element having a minimum content above 5% with Cr, Co, or Ni having a minimum content higher than 5%
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/08—Ferrous alloys, e.g. steel alloys containing nickel
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C26/00—Alloys containing diamond or cubic or wurtzitic boron nitride, fullerenes or carbon nanotubes
    • C22C2026/002—Carbon nanotubes

Abstract

The invention discloses a kind of method of fabricated in situ Nano diamond enhancing iron-nickel alloy based composites, for the composite as made by CNT and Fe-Ni Alloy Powder as raw material, preparation technology is discharge plasma sintering technique.CNT is mutually changed into Nano diamond in the catalysis of Fe-Ni Alloy Powder with the DC pulse electric field action lower part of discharge plasma sintering, transformation ratio is 50 80%, and CNT and Nano diamond play the collaboration enhancing effect of fiber reinforcement and particle strengthening in the composite.Relative to prior art, cooperate with the Strengthening and Toughening effect of enhancing more excellent, iron-nickel alloy based composites obtained by the present invention can be widely applied to precision instrument and high-technology field with hardness, intensity and the anti-wear performance higher than pure iron nickel alloy and with lower thermal coefficient of expansion.

Description

A kind of method of fabricated in situ Nano diamond enhancing iron nickel-base composite material and its institute Obtain material and application
Technical field
The present invention relates to the method and its gained of a kind of fabricated in situ Nano diamond enhancing iron nickel-base composite material Material and application, belong to metal-base composites technical field.
Background technology
Iron-nickel alloy refers to the higher iron-nickel alloy of nickel content including invar alloy, and nickel content is in 30%-36%.Invar alloy Maximum is characterized in that thermal coefficient of expansion is very low, i.e., as the change of temperature, alloy size are almost unchanged.Low-heat based on its protrusion Expansion characteristics, volume vary with temperature very small, and with ductility is good, the feature easily welded, invar alloy extensively should For precision instrument, bimetal leaf, mechanical equipment component etc., it is mainly used to manufacturer's standard part, slide measure, gravity in laboratory Instrument, fine measuring instrument accessory etc., also there is wide development in liquefied petroleum gas container, the frontier such as long-haul transmission cable Prospect, and have important application in fields such as aerospace field, global positioning systems.Obvious invar alloy is led in new and high technology Very important status has been occupied in domain.But the alloy has the problems such as hardness and low intensity, anti-wear performance difference, up for solution Certainly.
Most common metal strengthening mode mainly has four kinds, including solution strengthening, working hardening, refined crystalline strengthening and precipitation are by force Change.Above-mentioned four kinds of mechanism can effectively lift the mechanical property of iron-nickel alloy, but simultaneously also can be to the swollen feature of low-heat of material There is harmful effect.Therefore, we need to explore a kind of new schedule of reinforcement, while the low-heat of guarantee alloy swollen characteristic, carry Its high comprehensive mechanical property.It is a kind of very effective solution route to prepare iron nickel-base composite material, in particular by nano-sized carbon Material is as enhancing phase.
Nano diamond is one of nano-carbon material, is that one kind has in machinery, calorifics, optics, chemistry, electronics etc. The material of property.Nano diamond composite has very excellent performance and is widely applied：(1) superelevation The wearability that hardness, intensity are become reconciled, become important removing material；(2) high thermal conductivity, relatively low thermal coefficient of expansion It is set to be had a wide range of applications in heat dissipation element, high temperature semiconductors.The preparation method of Nano diamond composite is main at present Nano diamond powder and metal dust are blended under certain temperature, pressure and prepared, but under such preparation technology The matrix and interface binding power of reinforcement is poor and the skewness of reinforcement, so as to cause the mechanical property of composite Decline.
The content of the invention
Goal of the invention：In order to solve iron-nickel alloy hardness and low intensity, the technical problem of anti-wear performance difference, the present invention provides A kind of preparation method of fabricated in situ Nano diamond enhancing iron nickel-base composite material.Wherein, CNT has high Intensity, under the catalysis of Fe-Ni Alloy Powder catalyst with SPS DC pulse electric field action can partial phase change be nanogold Hard rock, transformation ratio are 50-80%, therefore obtain both CNT and Nano diamond the collaboration enhancing Ni-based composite wood of iron Material, makes it have excellent mechanical property, and composite is kept lower thermal coefficient of expansion.
Technical scheme：In order to realize foregoing invention purpose, the invention discloses a kind of enhancing of fabricated in situ Nano diamond The method of iron nickel-base composite material, mainly it is made up of CNT and iron nickel base alloy powder, CNT is as synthesis nanometer The carbon source of diamond, is evenly dispersed in iron nickel base alloy.
Fabricated in situ Nano diamond enhancing iron nickel-base composite material of the present invention is by finely dispersed carbon nanometer Pipe is added in iron nickel base alloy, and CNT has high intensity and good toughness, part iron-nickel alloy as catalyst, CNT meeting partial phase change under catalyst and SPS DC pulse electric field action is Nano diamond, finally obtains nanometer Both diamond and CNT collaboration enhancing iron nickel base alloy composite, its have excellent mechanical property and keep compared with Low thermal coefficient of expansion.
Preferably, by quality ratio, the adding proportion of the CNT is the 0.01-2.0% of iron-nickel alloy quality.
As it is another preferably, the caliber of the CNT is 1-100nm, the particle chi of the iron nickel base alloy powder Very little is 1-300 μm.
As another kind preferably, the content of nickel is 30-36wt.% in iron nickel (FeNi) based composites, and is contained 0-10wt.% trace element cobalt, than more typically having FeNi30, FeNi36, FeNi32Co4, FeNi31Co5.
The method of fabricated in situ diamond enhancing iron nickel-base composite material of the present invention, specifically includes following steps：
(1) liquid phase chemical mixes：Take dispersant (TNADIS) powder, add absolute ethyl alcohol, supersonic oscillations 10-30min, Form dispersant solution；Then carbon nanotube powder is added, vibrates 10-60min；Fe-Ni Alloy Powder is finally added, then 20-60min is vibrated, what is obtained is the solution of CNT and iron-nickel alloy.
(2) mechanical mill mixes：By resulting solution in step (1) with ratio of grinding media to material 5:1-20:1 ratio is placed in ball grinder In, the rotating speed using rotating speed as 100-400r/min, alternately rotating, ball milling 2-10h.
(3) dry：Powder after ball milling mixing is vacuumized into dry 5-24h, drying temperature is 40-120 DEG C, is completely dried The sieve of the 100-400 mesh of powder afterwards.
(4) sinter molding：According to the dimensional parameters of required product, the powder in step (3) is taken, is burnt by plasma discharging It is prepared by knot.
Preferably, in step (4)：
Pressure used in the discharge plasma sintering is 20-100MPa, and temperature is 1000-1300 DEG C, is sintered in highest The temperature time is 5-60min.
Specific preparation flow is as follows：
(1) calculate and weigh starting powder：Weigh the carbon nanotube powder and Fe-Ni Alloy Powder of respective quality, CNT The adding proportion of powder is the 0.01-2.0% of two kinds of powder gross masses.
(2) liquid phase chemical mixes：Take dispersant (TNADIS) powder, add absolute ethyl alcohol, supersonic oscillations 10-30min, Form dispersant solution；Then the carbon nanotube powder weighed is added in (1), vibrates 10-60min；Finally add in (1) The Fe-Ni Alloy Powder weighed, then 20-60min is vibrated, what is obtained is the solution of CNT and iron-nickel alloy.
(3) mechanical mill mixes：By resulting solution in step (2) with ratio of grinding media to material 5:1-20:1 ratio is placed in ball grinder In, the rotating speed using rotating speed as 100-400r/min, alternately rotating, ball milling 2-10h.
(4) dry：Powder after ball milling mixing is vacuumized into dry 5-24h, drying temperature is 40-120 DEG C, is completely dried The sieve of the 100-400 mesh of powder afterwards.
(5) sinter molding：According to the dimensional parameters of required product, the powder in step (4) is taken, plasma discharging can be passed through It is prepared by sintering.
Discharge plasma sintering forming method：Powder in (4) is poured into graphite jig, is fitted into push-down head, is put Sinter molding in discharge plasma sintering stove is inserted, under vacuum or inert atmosphere protection, pressure 20-100MPa, temperature is 1000-1400 DEG C, thermometric mode is infrared or thermocouple temperature measurement, and heating rate is 20-300 DEG C/min, and temperature is sintered in highest Degree insulation 5-60min.Natural stove is cold, and the demoulding obtains product.
(6) contextual analysis of organization and performance test：The starting powder in (4) is carried out first with SEM Morphology characterization, XRD material phase analysis then is carried out to the sample of sinter molding in (5), carbon is identified using transmission electron microscope The structure of nanotube and diamond, measure microhardness using microhardness testers, microcomputer controlled electronic universal tester is pressed Contracting test measurement compressive strength, thermal coefficient of expansion is measured using thermal analyzer, finally using SEM to fracture shape Looks are observed analysis.
Discharge plasma sintering (SPS) is also known as DC pulse electric field sintering (PECS) and field helps the sintering technology (FAST) to be The advanced sintering technology based on the activation of ON-OFF DC pulses electric field and pressure activated.SPS sintering mechanism has：Joule adds Heat, local melting and evaporation, particle surface activation, pressure activated and plastic deformation, field help diffusion, plasma attack pressure, Particle surface cleans and plasma sintering.
Although Chinese patent CN201610302136.7 discloses a kind of system of Nano diamond enhancing titanium matrix composite Preparation Method, but it is by additional Nano diamond particles reiforced metal-base composition, and the present invention is in-situ authigenic receives Rice diamond reinforced metal-base composite material, ferronickel is the custom catalystses of diamond synthesizing, and CNT is added into ferronickel In alloy, under the DC pulse electric field action of discharge plasma sintering, CNT can be changed into Nano diamond particle, turn Variability is 50-80%, still there is a small amount of CNT residual, and the Nano diamond for foring CNT and in-situ authigenic is assisted With enhancing ferronickel based composites.
The inventive method fabricated in situ Nano diamond strengthen iron nickel-base composite material, due to Nano diamond have it is excellent Mechanical performance and stable thermodynamic property, then diamond composite be widely used in cutter, drill bit, fin and electricity Sub- encapsulating material.Fabricated in situ Nano diamond technology can make that the combination of diamond and matrix is closer, and wetability is more preferable, and two The interface of person is cleaner, and makes diamond particles more tiny, plays a part of dispersion-strengtherning, and be evenly distributed in matrix In, and Nano diamond and unreacted CNT collaboration enhancing iron nickel base alloy, it is excellent finally make it that composite has Different combination property.
The beneficial effects of the invention are as follows：It is carbon source using CNT, iron nickel base alloy is as catalyst, in the straight of SPS Carbon nanotube portion is changed into Nano diamond under stream Electro-pulsing Field, change ratio 50-80%, then both collaboration enhancings Iron nickel-base composite material, largely improve the hardness, intensity and anti-wear performance of iron nickel base alloy.Simultaneously as carbon The thermal coefficient of expansion very little of nanotube and diamond in itself so that composite keeps relatively low thermal coefficient of expansion again, therefore opens up Wide application of the iron-nickel alloy in fields such as precision instrumentations.
Technique effect：Relative to prior art, the inventive method is simple and easy, can overcome that existing to prepare diamond compound The matrix and reinforcement wetability that material occurs are bad, and the shortcomings of reinforcement skewness, gained fabricated in situ is diamond intensified The hardness strength of strong iron nickel-base composite material is enhanced, and keeps lower thermal coefficient of expansion.
Brief description of the drawings
Fig. 1 content of carbon nanotubes is the transmission electron microscope pattern of Nano diamond particle in 1.0wt.% composites With diffraction spot point diagram (a) and the transmission electron microscope shape appearance figure (b) of unreacted CNT；
Fig. 2 is the composite of different content of carbon nanotubes and pure FeNi30 X ray diffracting spectrum；
Fig. 3 is the composite of different content of carbon nanotubes and pure FeNi30 microhardness tendency chart；
Fig. 4 is that the composite of different content of carbon nanotubes and pure FeNi30 stress-strain diagram and compressive strength become Gesture figure：Wherein, A is the compression curve figure of different content of carbon nanotubes composites；B is yield strength tendency chart；
Fig. 5 content of carbon nanotubes is the SEM shape appearance figure of the compression fracture of 0.75wt.% composites；
Fig. 6 is the thermal coefficient of expansion tendency chart of the composite of different content of carbon nanotubes；
Embodiment
The technical solution of the present invention is further described below in conjunction with the accompanying drawings.The present embodiment is with technical solution of the present invention Premised under implemented, give detailed implementation process, but protection scope of the present invention is not limited to following embodiments.
Embodiment 1
Discharge plasma sintering prepares fabricated in situ Nano diamond enhancing FeNi30 based composites, using CNT Powder and FeNi30 powder are raw material (purity 99%), and the wherein caliber of CNT is 20nm, the particle of FeNi30 powder Size is 45 μm (325 mesh).Prepare a diameter of 10mm, highly the cylindrical composite material sintered body for 10mm.
Comprise the following steps that：
(1) 10g FeNi30 powder (purity 99%) is weighed and the carbon nanotube powder that mass fraction is 0.25wt%, Carbon nano-tube dispersant (TNADIS) is placed in beaker first, absolute ethyl alcohol is added, 20min is vibrated by supersonic oscillations instrument Solution is formed, then the carbon nanotube powder weighed is added thereto shaken well 35min, the FeNi30 powder that will finally weigh End adds above solution, repeats above-mentioned oscillating operation 40min.
(2) powder solution that will tentatively be mixed in (1), it is 14 by ratio of grinding media to material：1 ratio is placed in ball grinder, anhydrous Ethanol is as protective agent, and the program of 250r/min rotating speed, successively rotating 2.5h, Ball-milling Time are on planetary ball mill 5h, abundant ball milling, makes it uniformly mix.
(3) the good starting powder of ball milling being placed in vacuum drying chamber to vacuumize and dried 8 hours, drying temperature is 100 DEG C, With the sieve of 325 mesh after being completely dried.
(4) dimensional parameters of the product after sintering are determined：A diameter of 10mm, it is highly 10mm.Calculated according to density formula Required powder quality is 6.28g.
(5) the powder 6.28g being sieved is weighed, it is Ni-based multiple to prepare fabricated in situ diamond enhancing iron with discharge plasma sintering Condensation material, sintering parameter are：Under vacuum protection atmosphere, pressure 80MPa, sintering temperature is 1050 DEG C, soaking time 5min, Thermometric mode is infrared measurement of temperature.Wherein heating rate is 100 DEG C/min, the sample application Archimedes method sintered is surveyed relative Density, calculate consistency be 98.7%.
Embodiment 2
Discharge plasma sintering prepares fabricated in situ Nano diamond enhancing FeNi36 invar alloy based composites, uses CNT and FeNi36 powder are raw material (purity 99%), and the wherein caliber of CNT is 50nm, FeNi36 powder Granular size is 25 μm (500 mesh).Prepare a diameter of 12mm, highly the cylindrical composite material sintered body for 32mm.
(1) 50g FeNi36 powder (purity 99%) is weighed and the carbon nanotube powder that mass fraction is 0.5wt%, it is first First Carbon nano-tube dispersant (TNADIS) is placed in beaker, adds absolute ethyl alcohol, 10min shapes are vibrated by supersonic oscillations instrument Shaken well 60min is added thereto into solution, then by the carbon nanotube powder weighed, the FeNi36 powder that will finally weigh Above solution is added, repeats above-mentioned oscillating operation 20min.
(2) powder solution that will tentatively be mixed in (1), it is 10 by ratio of grinding media to material:1 ratio is placed in ball grinder, anhydrous Ethanol is as protective agent, and the program of 300r/min rotating speed, successively rotating 2.5h, Ball-milling Time are on planetary ball mill 5h, abundant ball milling, makes it uniformly mix.
(3) the good starting powder of ball milling being placed in vacuum drying chamber to vacuumize and dried 8 hours, drying temperature is 100 DEG C, With the sieve of 400 mesh after being completely dried.
(4) dimensional parameters of the product after sintering are determined：A diameter of 12mm, it is highly 32mm.Calculated according to density formula Required powder quality is 30.07g.
(5) the powder 30.07g being sieved is weighed, it is Ni-based to prepare fabricated in situ diamond enhancing iron with discharge plasma sintering Composite, sintering parameter are：Under vacuum protection atmosphere, pressure 100MPa, sintering temperature is 1100 DEG C, soaking time 10min, thermometric mode are infrared measurement of temperature.Wherein heating rate is 50 DEG C/min, the sample application Archimedes method that will be sintered Survey relative density, calculate consistency be 99.1%.
Embodiment 3
For method with embodiment 1, difference is as follows：
CNT caliber is 2nm single-walled carbon nanotube, and matrix selects FeNi32Co4 super Invar alloy powder, its powder The particle size at end is 1 μm, and the adding proportion of the CNT is the 1.0% of matrix nickel quality.
By the sample after sintering with Archimedes method survey relative density, calculate consistency be 99.5%.
Embodiment 4
For method with embodiment 3, difference is as follows：
CNT caliber is 10nm, and matrix selects FeNi31Co5 super Invar alloy powder, and the particle size of its powder is 300 μm, the adding proportion of the CNT is the 2.0% of matrix weight of iron.
By the sample after sintering with Archimedes method survey relative density, calculate consistency be 99.7%.
Embodiment 5
For method with embodiment 1, difference is as follows：
CNT caliber is 100nm single-walled carbon nanotube, and matrix selects FeNi32Co4 super Invar alloy powder, its The particle size of powder is 150 μm, and the adding proportion of the CNT is the 0.1% of matrix nickel quality.
The concussion time is respectively 30min, 10min, 60min in step (1)；
Each parameter is respectively in step (2)：Ratio of grinding media to material 5:1, rotating speed 100r/min, ball milling 2h.
Each parameter is respectively in step (3)：5h is dried in vacuo, drying temperature is 40 DEG C, the sieving of 100-400 mesh sieve；
Each parameter is respectively in step (5) discharge plasma sintering：Pressure is 20MPa, and temperature is 1000 DEG C, in most high fever Junction temperature soaking time is 30min；
By the sample after sintering with Archimedes method survey relative density, calculate consistency be 99.6%.
Embodiment 6
For method with embodiment 2, difference is as follows：
CNT caliber is 80nm single-walled carbon nanotube, and matrix selects FeNi32Co4 super Invar alloy powder, its powder The particle size at end is 200 μm, and the adding proportion of the CNT is the 0.05% of matrix nickel quality.
The concussion time is respectively 20min, 250min, 45min in step (1)；
Each parameter is respectively in step (2)：Ratio of grinding media to material 20:1, rotating speed 400r/min, ball milling 10h.
Each parameter is respectively in step (3)：24h is dried in vacuo, drying temperature is 120 DEG C, the sieving of 300 mesh sieve；
Each parameter is respectively in step (5) discharge plasma sintering：Pressure is 60MPa, and temperature is 1000 DEG C, in most high fever Junction temperature soaking time is 60min；
By the sample after sintering with Archimedes method survey relative density, calculate consistency be 99.4%.
Figure of description Fig. 1 is the transmission electron microscope figure that content of carbon nanotubes is 1.0wt.%, by calculating diffraction Spot can obtain CNT phase transformation for diamond, and the particle of black is Nano diamond particle in figure, and is had unreacted CNT is present, then the enhancing mechanism for further demonstrating the composite cooperates with for Nano diamond particle with CNT Strengthen iron nickel-base composite material.Fig. 2 is the XRD of different content of carbon nanotubes composites, and three peaks are all iron-nickel alloy Peak, due to added CNT amount very little, then can not detect CNT and diamond thing phase peak.Fig. 3 is that different carbon are received The microhardness tendency chart of nanotube content composite, it is seen that with the increase of content of carbon nanotubes, hardness is in rising trend, but When content of carbon nanotubes is 1.0wt.%, hardness reduces, and reason is that the reunion of CNT causes the surface of composite Hardness declines.A is the compression curve figure of different content of carbon nanotubes composites in Fig. 4, does not have to see material from figure Phenomenon of rupture, then the toughness of the composite is fine；, can be with addition, obtain yield strength tendency chart B by calculating yield strength It was found that with the increase of content of carbon nanotubes, the yield strength of composite is increasing.Fig. 5 is that content of carbon nanotubes is The scanning fracture apperance figure of 0.75wt.% composites, it can be seen that incision position has the presence of many dimples, then judges the material Fracture mode be ductile rupture.Fig. 6 is the thermal coefficient of expansion curve map of different content of carbon nanotubes, it is seen that with CNT The increase of content, the thermal coefficient of expansion of the composite is on a declining curve, therefore the composite can apply to precision instrument With high-technology field.

Claims (7)

  1. A kind of 1. method of fabricated in situ Nano diamond enhancing iron-nickel alloy based composites, it is characterised in that described compound Material is mainly as made by CNT and iron-nickel alloy；Wherein, the CNT is as in-situ authigenic Nano diamond Carbon source, be evenly distributed in iron-nickel alloy matrix.
  2. 2. the method for fabricated in situ Nano diamond enhancing iron nickel-base composite material according to claim 1, its feature exist In by quality ratio, the adding proportion of the CNT is 0.01%-2.0%.
  3. 3. the method for fabricated in situ Nano diamond enhancing iron nickel-base composite material according to claim 1, its feature exist In the caliber of the CNT is 1-100nm, and the particle diameter of iron nickel base alloy powder is 1-300 μm.
  4. 4. the method for fabricated in situ Nano diamond enhancing iron nickel-base composite material according to claim 1, its feature exist In comprising the following steps：
    (1) liquid phase chemical mixes：Dispersant powder is taken, absolute ethyl alcohol is added, supersonic oscillations 10-30min, it is molten to form dispersant Liquid；Then carbon nanotube powder is added, vibrates 10-60min；Fe-Ni Alloy Powder is finally added, then vibrates 20-60min, What is obtained is the solution of CNT and iron-nickel alloy；
    (2) mechanical mill mixes：By resulting solution in step (1) with ratio of grinding media to material 5:1-20:1 ratio is placed in ball grinder, with Rotating speed is 100-400r/min rotating speed, replaces rotating, ball milling 2-10h；
    (3) dry：Powder after ball milling mixing is vacuumized into dry 5-24h, drying temperature is 40-120 DEG C, after being completely dried The sieve of powder 100-400 mesh；
    (4) sinter molding：According to the dimensional parameters of required product, the powder in step (3) is taken, by discharge plasma sintering side Method sinters, and produces.
  5. 5. the method for fabricated in situ Nano diamond enhancing iron nickel-base composite material according to claim 4, its feature exist In in step (4)：
    Pressure used in the discharge plasma sintering is 20-100MPa, and temperature is 1000-1300 DEG C, in maximum sintering temperature Soaking time is 5-60min.
  6. 6. the Nano diamond enhancing iron nickel-base composite material obtained by any one of claim 1-5 methods described.
  7. 7. application of the composite described in claim 6 in precision instrumentation is prepared.
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CN112008087A (en) * 2020-08-30 2020-12-01 中南大学 Method for improving comprehensive performance of carbon nano material reinforced nickel-based high-temperature alloy
CN112759408A (en) * 2021-01-04 2021-05-07 苏州第一元素纳米技术有限公司 Boron carbide ceramic and preparation method and application thereof
CN113005323A (en) * 2021-01-16 2021-06-22 西安交通大学 Diamond/copper composite heat conduction material and preparation method thereof

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112008087A (en) * 2020-08-30 2020-12-01 中南大学 Method for improving comprehensive performance of carbon nano material reinforced nickel-based high-temperature alloy
CN112759408A (en) * 2021-01-04 2021-05-07 苏州第一元素纳米技术有限公司 Boron carbide ceramic and preparation method and application thereof
CN112759408B (en) * 2021-01-04 2022-12-23 苏州第一元素纳米技术有限公司 Boron carbide ceramic and preparation method and application thereof
CN113005323A (en) * 2021-01-16 2021-06-22 西安交通大学 Diamond/copper composite heat conduction material and preparation method thereof

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