CN108031841A - A kind of manufacturing process of metal-base nanometer composite material part - Google Patents

A kind of manufacturing process of metal-base nanometer composite material part Download PDF

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Publication number
CN108031841A
CN108031841A CN201711050358.5A CN201711050358A CN108031841A CN 108031841 A CN108031841 A CN 108031841A CN 201711050358 A CN201711050358 A CN 201711050358A CN 108031841 A CN108031841 A CN 108031841A
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metal
composite material
manufacturing process
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nanometer composite
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CN108031841B (en
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赵晓明
徐天文
许海嫚
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Bolite (Weinan) additive manufacturing Co.,Ltd.
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Xian Bright Laser Technologies Co Ltd
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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
    • B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
    • 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
    • B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/10—Formation of a green body
    • 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
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
    • B22F1/107—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material containing organic material comprising solvents, e.g. for slip casting
    • 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
    • B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/30—Process control
    • B22F10/32—Process control of the atmosphere, e.g. composition or pressure in a building chamber
    • 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
    • B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/30—Process control
    • B22F10/34—Process control of powder characteristics, e.g. density, oxidation or flowability
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y10/00—Processes of additive manufacturing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y70/00—Materials specially adapted for additive manufacturing
    • 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
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10—Processes characterised by the sequence of their steps
    • 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
    • B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/25—Process efficiency

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Automation & Control Theory (AREA)
  • Powder Metallurgy (AREA)

Abstract

A kind of manufacturing process of metal-base nanometer composite material part disclosed by the invention, comprises the following steps：Step 1, the pretreatment of nano material and metal material；Step 2, the preparation of nanometer enhancing metal-based compound photocuring slurry；Step 3, optical soliton interaction is carried out；Step 4, it is degreasing sintered.The manufacturing process of the present invention uses high-energy ultrasound, effectively alleviates the reunion of nano particle in forming process by the pretreatment to metal dust and nano material, whole process；Strengthen combining for metal-based compound photocuring slurry and photocuring technology by preparing nanometer, improve the complexity of formation of parts；By carrying out Fast Sintering in the temperature less than interfacial reaction, the nano particle interfacial reaction of whole process is reduced；Step is simple, there is good practical value.

Description

A kind of manufacturing process of metal-base nanometer composite material part
Technical field
The invention belongs to optical soliton interaction method and technology field, and in particular to a kind of metal-base nanometer composite material part Manufacturing process.
Background technology
Metal-base nanometer composite material is due to having the characteristics that intensity height, good toughness, good heat stability, in aviation, boat My god, automation etc. high-technology field have a wide range of applications.The shaping side of current metal-base nanometer composite material part Method mainly has two kinds：Liquid cast method and solid-state sintering.Liquid cast method can obtain near net-shaped complex parts, but need mould Tool while Presence of an interface react and component is difficult to control；Solid-state sintering component is easily controllable, but particle agglomeration and only easily occurs Simple miniature parts can be obtained.Therefore, there is presently no one kind can realize high-performance complexity metal-base nanometer composite material The method of part Quick-forming.
The content of the invention
The object of the present invention is to provide a kind of manufacturing process of metal-base nanometer composite material part, existing Metal Substrate is solved Part of nanometer composite material manufacturing process median surface is reacted and agglomeration is strong, the problem of being not easy to prepare complex parts.
The technical solution adopted in the present invention is a kind of manufacturing process of metal-base nanometer composite material part, including with Lower step：
Step 1, the pretreatment of metal dust and nano material
Step 2, the preparation of nanometer enhancing metal-based compound photocuring slurry
Step 2.1, it will be put into through the processed metal dust of step 1 in planetary ball mill, while add suitable point Powder and phase solvent, using absolute ethyl alcohol as medium, 1:Ball milling 2-8h under 1 ratio of grinding media to material, then filtering and the drying at 120 DEG C 10h, obtains mixed-powder；
Step 2.2, take quantity of resin to be put into mixer, then the mixed-powder of step 2.1 point is no less than and is added three times Enter wherein, add suitable diluent at the same time in each add, stirring is uniformly mixed it, obtains mixture；
Step 2.3, under the conditions of lucifuge, suitable free radical photo-initiation and warp are added into the mixture of step 2.2 Nano material after step 1 processing, carries out ultrasonic wave and disperses to handle with mechanical agitation, obtains nanometer enhancing metal after mixing Base complex light cure pastes；
Step 2.4, under lucifuge, the condition of negative pressure no more than -0.06MPa, the nanometer enhancing Metal Substrate to step 2.3 is answered Closing light cure pastes continue high-energy ultrasound and handle 8-12h, spare；
Step 3, optical soliton interaction
The three-dimensional part model information to be formed handled well is imported in optical soliton interaction equipment, utilizes receiving for step 2.4 Meter Zeng Qiang metal-based compound photocuring slurries shape the blank of required part, and always to optical soliton interaction in forming process Uncured slurry in equipment in feeding device carries out high-energy ultrasound processing；
Step 4, it is degreasing sintered
Step 4.1, degreasing
The blank of step 3 is placed in roaster, under normal pressure, ar gas environment, is warming up to the speed of 3-5 DEG C/min 350-600 DEG C, keep the temperature 1-10h；Then vacuumize, keep the temperature furnace cooling after same time；
Step 4.2, sinter
Blank after step 4.1 is handled, environment in argon gas protection, under the conditions of gas pressure 10-200MPa, with 5-10 DEG C/heating rate of min is raised to 600-1300 DEG C, insulation 0.5-3h obtains required metal-base nanometer composite material part.
It is of the invention to be further characterized in that,
The pretreatment of metal dust is specially in step 1：Choose particle diameter d50For the parent metal powder of 1-10um, in temperature 200-250 DEG C, dry 2-10h under vacuum environment of the atmospheric pressure no more than -0.06MPa；
The pretreatment of nano material is specially in step 1：Ultrasonic wave disperse with the conditions of churned mechanically collective effect, Disperse and clean nano particle, it is then dry under the vacuum environment of 100-180 DEG C of temperature, atmospheric pressure no more than -0.06MPa 20-30h。
Resin is free radical type resin in step 2.2, is specially unsaturated polyester (UP) or esters of acrylic acid, diluent is propylene Esters of gallic acid, vinyl-based or vinyl ethers；Dispersant is ammonium polyacrylate or ammonium citrate in step 2.1, and phase solvent is hard Resin acid or polyalcohol；
Free radical photo-initiation is benzoin derivatives, acylphosphine oxide or sulfur-containing organic compound in step 2.3；
Wherein resin, dispersant, diluent, phase solvent and free radical photo-initiation are both needed to drying process before use.
The Volume fraction of metal dust and resin is 1-3 in mixed-powder in step 2.2:1；
Dispersant total amount of adding is the 0.1-1% of metal dust quality, and phase solvent total amount of adding is metal dust quality 0.18-2%；Each secondary diluent total amount of adding is the 0.1-1.5% of metal dust quality.
Temperature is 25-35 DEG C when being mixed in step 2.2；Mixing parametric：Rotating speed 280-600rad/min under normal pressure, during stirring Between 4-8h.
The quality of free radical photo-initiation is the 0.5-3% of resin gross mass in step 2.2 in step 2.3；
The quality of nano material is the 0.5-5% of metal dust gross mass in step 2.2 mixed-powder in step 2.3.
Stir speed (S.S.) 300-600rad/min in step 2.3, mixing time 1-4h.
The parameter of optical soliton interaction equipment is in step 3：The a length of 200-400nm of light wave used, when shaping, layering used was thick Spend for 10-100um.
Step 4.2 needs to judge whether to pre-burning according to the characteristic of part material therefor before sintering, if carrying out pre-burning Then design parameter is：Under the conditions of environment, gas pressure 10-200MPa in argon gas protection, it is warming up to the speed of 3-5 DEG C/min 800-900 DEG C, keep the temperature 0.5-2h.
The beneficial effects of the invention are as follows：A kind of manufacturing process of metal-base nanometer composite material part of the present invention passes through to gold Belong to the pretreatment of powder and nano material, whole process uses high-energy ultrasound, effectively alleviates nano particle in forming process Reunite；Strengthen combining for metal-based compound photocuring slurry and photocuring technology by preparing nanometer, improve formation of parts Complexity；By carrying out Fast Sintering in the temperature less than interfacial reaction, the nano particle interface for reducing whole process is anti- Should；Step is simple, there is good practical value.
Embodiment
The manufacturing process of the present invention is described in detail below by embodiment.
A kind of manufacturing process of metal-base nanometer composite material part of the present invention, specifically includes following steps：
Step 1, the pretreatment of metal dust and nano material
The pretreatment of metal dust is specially：Choose particle diameter d50For the parent metal powder of 1-10um, in temperature 200-250 DEG C, dry 2-10h under vacuum environment of the atmospheric pressure no more than -0.06MPa；
The pretreatment of nano material is specially：Ultrasonic wave disperse with the conditions of churned mechanically collective effect, it is scattered simultaneously Nano particle is cleaned, then the dry 20-30h under the vacuum environment of 100-180 DEG C of temperature, atmospheric pressure no more than -0.06MPa.
Step 2, the preparation of nanometer enhancing metal-based compound photocuring slurry
Step 2.1, it will be put into through the processed metal dust of step 1 in planetary ball mill, while add suitable warp The dispersant and phase solvent of drying process, using absolute ethyl alcohol as medium, 1:Ball milling 2-8h under 1 ratio of grinding media to material, is then filtered simultaneously Dry 10h, obtains mixed-powder at 120 DEG C,
Dispersant is ammonium polyacrylate or ammonium citrate, and phase solvent is stearic acid or polyalcohol；
Step 2.2, take in right amount the resin through drying process be put into mixer, then by the mixed-powder of step 2.1 point No less than being added thereto three times, suitable diluent is added when adding every time at the same time, stirring is uniformly mixed it, is mixed Thing；
Wherein resin is free radical type resin, is specially unsaturated polyester (UP) or esters of acrylic acid, diluent is acrylate Class, vinyl-based or vinyl ethers；Dispersant total amount of adding is the 0.1-1% of metal dust quality in mixed-powder；Dilution Agent total amount of adding is the 0.1-1.5% of metal dust quality in mixed-powder；Phase solvent total amount of adding is metal dust quality 0.18-2%；Temperature is 25-35 DEG C during mixing；Mixing parametric：Rotating speed 280-600rad/min under normal pressure, mixing time 4-8h；
Step 2.3, under the conditions of lucifuge, suitable free radical through drying process is added into the mixture of step 2.2 Photoinitiator and the nano material after step 1 processing, carry out ultrasonic wave and disperse to handle with mechanical agitation, with 300-600rad/ The speed stirring 1-4h of min is uniformly mixed it, obtains nanometer enhancing metal-based compound photocuring slurry；
Wherein free radical photo-initiation is benzoin derivatives, acylphosphine oxide or sulfur-containing organic compound；Free radical The 0.5-5% that the quality of photoinitiator is the 0.5-3% of resin gross mass, the quality of nano material is metal dust gross mass；
Step 2.4, under lucifuge, the condition of negative pressure no more than -0.06MPa, the nanometer enhancing Metal Substrate to step 2.3 is answered Closing light cure pastes continue high-energy ultrasound processing 8-12h, and bubble therein is excluded to exclude bubble therein, spare.
Step 3, optical soliton interaction
The three-dimensional part model information to be formed handled well is imported in optical soliton interaction equipment, utilizes receiving for step 2.4 Meter Zeng Qiang metal-based compound photocuring slurries shape the blank of required part, and always to optical soliton interaction in forming process Uncured slurry in equipment in feeding device carries out high-energy ultrasound processing；The a length of 200- of light wave used in optical soliton interaction equipment 400nm, lift height used is 10-100um during shaping.
Step 4, it is degreasing sintered
Step 4.1, degreasing
The blank of step 3 is placed in roaster, under normal pressure, ar gas environment, is warming up to the speed of 3-5 DEG C/min 350-600 DEG C, keep the temperature furnace cooling after 1-10h；Then vacuumize, keep the temperature furnace cooling after same time；
Step 4.2, sinter
Blank after step 4.1 is handled, according to the demand of different parts, chooses whether pre-burning, pre-burning tool before sintering Body parameter is：Under the conditions of environment, gas pressure 10-200MPa in argon gas protection, 800- is warming up to the speed of 3-5 DEG C/min 900 DEG C, keep the temperature 0.5-2h；
Then the environment in argon gas protection, under the conditions of gas pressure 10-200MPa, with the heating rate liter of 5-10 DEG C/min To 600-1300 DEG C, insulation 0.5-3h obtains required metal-base nanometer composite material part.
The manufacturing process of the present invention uses high-energy ultrasound by the pretreatment to metal dust and nano material, whole process, The effective reunion for alleviating nano particle in forming process；Strengthen metal-based compound photocuring slurry and light by preparing nanometer The joint of curing technology, improves the complexity of formation of parts；By carrying out Fast Sintering in the temperature less than interfacial reaction, Reduce the nano particle interfacial reaction of whole process；Step is simple, there is good practical value.
Embodiment 1：Carbon nanotubes-aluminum composites part
(1) pretreatment of metal dust and nano material
The pretreatment of metal dust is specially：By d50The AlSi10Mg powder of=1um, 200 DEG C, atmospheric pressure no more than- Dry 5h under the vacuum environment of 0.06MPa；
The pretreatment of nano material is specially：Disperseed with alcohol in ultrasonic wave with locating under the conditions of churned mechanically collective effect Carbon nanotubes is managed, then the dry 20h under the vacuum environment of 100 DEG C of temperature, atmospheric pressure no more than -0.06MPa.
(2) preparation of nanometer enhancing metal-based compound photocuring slurry
Drying process 1,6- hexanediyl esters；Dispersants ammonium polyacrylate, diluent isobornyl acrylate, phase Solvent polyalcohol, radical photoinitiator benzoin dimethylether.
The AlSi10Mg metal dusts of 1620g are fitted into planetary ball mill, while add 8.1g dispersant polypropylene Sour ammonium and 16.2g phase solvent polyalcohols, are medium 1 using absolute ethyl alcohol:Ball milling 2h under 1 ratio of grinding media to material, after filtering at 120 DEG C Dry 10h；
By 1, the 6- hexanediyl ester free radical type resins through the processed metal dust of above step and 400ml (Volume fraction of metal dust and free radical type resin is 3:2), adding in three times in mixer is uniformly mixed it, obtains Mixture；Diluent isobornyl acrylate is all added in each add, each time addition isobornyl acrylate total amount is 16.2g, 35 DEG C of mixing temperature, mixing parametric are to stir 8h under normal pressure with the rotating speed of 400rad/min；
Under conditions of lucifuge, the benzoin dimethylether of 12g and the carbon nanotubes of 56.7g are continuously added in the mixture, Be stirred with high-energy ultrasound processing, stir speed (S.S.) 350rad/min, processing time 4h make its be uniformly mixed received so that carbon is made Mitron/aluminum-base composite photocuring slurry；
Under lucifuge, the condition of negative pressure no more than -0.06MPa, carbon nanotubes/aluminum-base composite photocuring slurry is continued into The high-energy ultrasound processing of row 8h, it is spare to exclude bubble therein.
(3) optical soliton interaction
The three-dimensional part model information to be formed handled well is imported in optical soliton interaction equipment, utilizes carbon nanotubes/aluminium Base complex light cure pastes shape the blank of required part；The a length of 355nm of light wave used in optical soliton interaction equipment, shaping when institute It is 20um with lift height, high-energy ultrasound processing is carried out to uncured slurry in feeding device always in forming process.
(4) it is degreasing sintered
The blank of step 3 is placed in roaster and carries out ungrease treatment.Degreasing process is：Under normal pressure, ar gas environment, 350 DEG C are warming up to the speed of 3 DEG C/min, after keeping the temperature 10h；Then vacuumize, undergo furnace cooling after equal soaking time.
Then it is sintered, sintering process：In the environment of argon gas protection, gas pressure 200MPa, with 10 DEG C/min's Speed is warming up to 630 DEG C, and insulation 2h obtains required carbon nanotubes-aluminum composites part.
Embodiment 2：Carbon nano tube/copper base composite material parts
(1) pretreatment of metal dust and nano material
The pretreatment of metal dust is specially：By d50The H65 powder of=10um, 200 DEG C, atmospheric pressure no more than- Dry 2h under the vacuum environment of 0.06MPa；
The pretreatment of nano material is specially：Disperseed with alcohol in ultrasonic wave with locating under the conditions of churned mechanically collective effect Carbon nanotubes is managed, then the dry 20h under the vacuum environment of 100 DEG C of temperature, atmospheric pressure no more than -0.06MPa.
(2) preparation of nanometer enhancing metal-based compound photocuring slurry
Drying process 1,6- hexanediyl esters；Dispersant ammonium citrate, diluent vinyl ethers, phase solvent are polynary Alcohol, radical photoinitiator benzoin dimethylether.
4275g H65 metal dusts are fitted into planetary ball mill, at the same add 4.275g dispersants ammonium citrate with 7.695g phase solvent polyalcohols, are medium 1 using absolute ethyl alcohol:Ball milling 2h under 1 ratio of grinding media to material is dry at 120 DEG C after filtering 10h；
By 1, the 6- hexanediyl ester free radical type resins through the processed metal dust of above step and 500ml (metal dust and free radical type resin volume score ratio are 1:1), adding in three times in mixer is uniformly mixed it；Each All add diluent vinyl ethers during addition, it is 4.275g to add vinyl ethers total amount for each time, 20 DEG C of mixing temperature, mixing parametric To stir 8h under normal pressure with the rotating speed of 280rad/min；
Under conditions of lucifuge, the benzoin dimethylether of 15g and the carbon nanometer of 21.375g are continuously added in the mixture Pipe, be stirred makes it be uniformly mixed so that carbon is made with high-energy ultrasound processing, stir speed (S.S.) 280rad/min, processing time 4h Nanotube/copper-based complex light cure pastes；
Under lucifuge, the condition of negative pressure no more than -0.06MPa, carbon nano tube/copper base complex light cure pastes are continued into The high-energy ultrasound processing of row 8h, it is spare to exclude bubble therein.
(3) optical soliton interaction
The three-dimensional part model information to be formed handled well is imported in optical soliton interaction equipment, utilizes carbon nano tube/copper Base complex light cure pastes shape the blank of required part；The a length of 355nm of light wave used in optical soliton interaction equipment, shaping when institute It is 10um with lift height, high-energy ultrasound processing is carried out to uncured slurry in feeding device always in forming process.
(4) it is degreasing sintered
The blank of step 3 is placed in roaster and carries out ungrease treatment.Degreasing process is：Under normal pressure, ar gas environment, 400 DEG C are warming up to the speed of 5 DEG C/min, keeps the temperature 1h；Then vacuumize, undergo furnace cooling after equal soaking time.
Then it is sintered, sintering process：In the environment of argon gas protection, gas pressure 100MPa, with the speed of 5 DEG C/min Rate is warming up to 600 DEG C, and insulation 2h obtains required carbon nano tube/copper base composite material parts.
Embodiment 3：TiC/ titanium alloy composite material parts
(1) pretreatment of metal dust and nano material
The pretreatment of metal dust is specially：By d50The TC4 powder of=8um, 250 DEG C, atmospheric pressure no more than- Dry 6h under the vacuum environment of 0.06MPa；
The pretreatment of nano material is specially：Disperseed with alcohol in ultrasonic wave with locating under the conditions of churned mechanically collective effect TiC nano particles are managed, then the dry 30h under the vacuum environment of 100 DEG C of temperature, atmospheric pressure no more than -0.06MPa.
(2) preparation of nanometer enhancing metal-based compound photocuring slurry
Drying process 1,6- hexanediyl esters；Dispersant ammonium citrate, diluent vinyl ethers, phase solvent are polynary Alcohol, radical photoinitiator benzoin dimethylether.
3382.5g TC4 powder is fitted into planetary ball mill, at the same add 33.825g dispersants ammonium citrate with 67.65g phase solvent polyalcohols, are medium 1 using absolute ethyl alcohol:Ball milling 8h under 1 ratio of grinding media to material is dry at 120 DEG C after filtering 10h；
By 1, the 6- hexanediyl ester free radical type resins through the processed metal dust of above step and 250ml (metal dust and free radical type resin volume score ratio are 3:1), adding in three times in mixer is uniformly mixed it；Each Diluent vinyl ethers is all added during addition, it is 50.7375g that each time, which adds vinyl ethers total amount, and 35 DEG C of mixing temperature, stirs ginseng Number is to stir 6h under normal pressure with the rotating speed of 600rad/min；
Under conditions of lucifuge, the TiC of the benzoin dimethylether and 169.125g that continuously add 7.5g in the mixture receives Rice grain, be stirred makes it be uniformly mixed with system with high-energy ultrasound processing, stir speed (S.S.) 280rad/min, processing time 4h Into TiC nano particles/TC4 complex light cure pastes；
Under lucifuge, the condition of negative pressure no more than -0.06MPa, TiC nano particles/TC4 complex lights cure pastes are continued The high-energy ultrasound processing of 8h is carried out, it is spare to exclude bubble therein.
(3) optical soliton interaction
By the three-dimensional part model information to be formed handled well import optical soliton interaction equipment in, using TiC nano particles/ TC4 complex light cure pastes shape the blank of required part；The a length of 355nm of light wave used in optical soliton interaction equipment, during shaping Lift height used is 60um, and high-energy ultrasound processing is carried out to uncured slurry in feeding device always in forming process.
(4) it is degreasing sintered
The blank of step 3 is placed in roaster and carries out ungrease treatment.Degreasing process is：Under normal pressure, ar gas environment, 600 DEG C are warming up to the speed of 3 DEG C/min, keeps the temperature 5h；Then vacuumize, go through furnace cooling again after equal soaking time.
Then it is sintered, is divided into the completion of two steps：1. pre-burning, in the environment of argon gas protection, gas pressure 10MPa, with 5 DEG C/speed of min is warming up to 800 DEG C, keep the temperature 0.5h；2. sinter, after the completion for the treatment of pre-burning, at the same pressure, with 5 DEG C/min Speed be warming up to 1200 DEG C, insulation 3h obtains required TiC nano particles/TC4 composite material parts.
Embodiment 4：Graphene/nickel based high-temperature alloy composite material parts
(1) pretreatment of metal dust and nano material
The pretreatment of metal dust is specially：By d50The FGH4095 powder of=1um, 250 DEG C, atmospheric pressure no more than- Dry 10h under the vacuum environment of 0.06MPa；
The pretreatment of nano material is specially：Disperseed with alcohol in ultrasonic wave with locating under the conditions of churned mechanically collective effect Graphene nano particle is managed, then the dry 20h under the vacuum environment of 180 DEG C of temperature, atmospheric pressure no more than -0.06MPa.
(2) preparation of nanometer enhancing metal-based compound photocuring slurry
Drying process polyester acrylate；Dispersants ammonium polyacrylate, diluent vinyl ethers, phase solvent polyalcohol, from By fundamental mode photoinitiator Irgacure 250.
5544g FGH4095 metal dusts are fitted into planetary ball mill, while add 27.22g dispersant polypropylene Sour ammonium and 11.088g phase solvent polyalcohols, are medium 1 using absolute ethyl alcohol:Ball milling 6h under 1 ratio of grinding media to material, at 120 DEG C after filtering Lower dry 10h；
By the polyester acrylate free radical type resin (metal powder through the processed metal dust of above step and 400ml End and free radical type resin volume score ratio are 3:2), adding in three times in mixer is uniformly mixed it；Added each time When all add diluent vinyl ethers, it is 5.544g to add vinyl ethers total amount for each time, 30 DEG C of mixing temperature, and mixing parametric is, 8h is stirred with the rotating speed of 350rad/min under normal pressure；
Under conditions of lucifuge, the graphene of the benzoin dimethylether and 110.88g that continuously add 8g in the mixture is received Rice grain, be stirred makes it be uniformly mixed with system with high-energy ultrasound processing, stir speed (S.S.) 600rad/min, processing time 4h Into graphene nano particle/nickel base superalloy complex light cure pastes；
Under lucifuge, the condition of negative pressure no more than -0.06MPa, to graphene nano particle/nickel base superalloy complex light Cure pastes continue the high-energy ultrasound processing of 12h, spare to exclude bubble therein.
(3) optical soliton interaction
The three-dimensional part model information to be formed handled well is imported in optical soliton interaction equipment, utilizes graphene nano Grain/nickel base superalloy complex light cure pastes shape the blank of required part；Light wave used in optical soliton interaction equipment is a length of 355nm, lift height used is 100um during shaping, uncured slurry in feeding device is carried out always in forming process high Can ultrasonication.
(4) it is degreasing sintered
The blank of step 3 is placed in roaster and carries out ungrease treatment.Degreasing process is：Under normal pressure, ar gas environment, 660 DEG C are warming up to the speed of 3 DEG C/min, keeps the temperature 2h；Then vacuumize, undergo after equal soaking time again with furnace cooling But.
Then it is sintered, is divided into the completion of two steps：1. pre-burning, in the environment of argon gas protection, gas pressure 100MPa, with The speed of 5 DEG C/min is warming up to 8900 DEG C, keeps the temperature 2h；2. sinter, after the completion for the treatment of pre-burning, at the same pressure, with 5 DEG C/min Speed be warming up to 1300 DEG C, insulation 2h obtains graphene nano particle/nickel base superalloy composite material parts.

Claims (9)

1. a kind of manufacturing process of metal-base nanometer composite material part, it is characterised in that comprise the following steps：
Step 1, the pretreatment of metal dust and nano material
Step 2, the preparation of nanometer enhancing metal-based compound photocuring slurry
Step 2.1, it will be put into through the processed metal dust of step 1 in planetary ball mill, while add suitable dispersant With phase solvent, using absolute ethyl alcohol as medium, 1:Ball milling 2-8h under 1 ratio of grinding media to material, subsequent filtering and the dry 10h at 120 DEG C, Obtain mixed-powder；
Step 2.2, take quantity of resin to be put into mixer, then the mixed-powder of step 2.1 point is no less than and adds it three times In, suitable diluent is added when adding every time at the same time, stirring is uniformly mixed it, obtains mixture；
Step 2.3, under the conditions of lucifuge, suitable free radical photo-initiation is added into the mixture of step 2.2 and through step 1 Nano material after processing, carries out ultrasonic wave and disperses to handle with mechanical agitation, obtains nanometer enhancing Metal Substrate after mixing and answers Closing light cure pastes；
Step 2.4, under lucifuge, the condition of negative pressure no more than -0.06MPa, metal-based compound light is strengthened to the nanometer of step 2.3 Cure pastes continue high-energy ultrasound and handle 8-12h, spare；
Step 3, optical soliton interaction
The three-dimensional part model information to be formed handled well is imported in optical soliton interaction equipment, is increased using the nanometer of step 2.4 Strong metal base complex light cure pastes shape the blank of required part, and always to optical soliton interaction equipment in forming process Uncured slurry in middle feeding device carries out high-energy ultrasound processing；
Step 4, it is degreasing sintered
Step 4.1, degreasing
The blank of step 3 is placed in roaster, under normal pressure, ar gas environment, 350- is warming up to the speed of 3-5 DEG C/min 600 DEG C, keep the temperature 1-10h；Then vacuumize, keep the temperature furnace cooling after same time；
Step 4.2, sinter
Blank after step 4.1 is handled, environment in argon gas protection, under the conditions of gas pressure 10-200MPa, with 5-10 DEG C/ The heating rate of min is raised to 600-1300 DEG C, and insulation 0.5-3h obtains required metal-base nanometer composite material part.
2. the manufacturing process of a kind of metal-base nanometer composite material part according to claim 1, it is characterised in that described The pretreatment of metal dust is specially in step 1：Choose particle diameter d50For the parent metal powder of 1-10um, in temperature 200-250 DEG C, dry 2-10h under vacuum environment of the atmospheric pressure no more than -0.06MPa；
The pretreatment of nano material is specially in the step 1：Ultrasonic wave disperse with the conditions of churned mechanically collective effect, Disperse and clean nano particle, it is then dry under the vacuum environment of 100-180 DEG C of temperature, atmospheric pressure no more than -0.06MPa 20-30h。
3. the manufacturing process of a kind of metal-base nanometer composite material part according to claim 1, it is characterised in that described Resin is free radical type resin in step 2.2, be specially unsaturated polyester (UP) or esters of acrylic acid, diluent for esters of acrylic acid, Vinyl-based or vinyl ethers；Dispersant is ammonium polyacrylate or ammonium citrate in step 2.1, and phase solvent is stearic acid or more First alcohol；
Free radical photo-initiation is benzoin derivatives, acylphosphine oxide or sulfur-containing organic compound in the step 2.3；
Wherein resin, dispersant, diluent, phase solvent and free radical photo-initiation are both needed to drying process before use.
4. the manufacturing process of a kind of metal-base nanometer composite material part according to claim 1, it is characterised in that described The Volume fraction of metal dust and resin is 1-3 in mixed-powder in step 2.2:1；
Dispersant total amount of adding is the 0.1-1% of metal dust quality, and phase solvent total amount of adding is the 0.18- of metal dust quality 2%, each secondary diluent total amount of adding is the 0.1-1.5% of metal dust quality.
5. the manufacturing process of a kind of metal-base nanometer composite material part according to claim 1, it is characterised in that described Temperature is 25-35 DEG C when being mixed in step 2.2；Mixing parametric：Rotating speed 280-600rad/min under normal pressure, mixing time 4-8h.
6. the manufacturing process of a kind of metal-base nanometer composite material part according to claim 1, it is characterised in that described The quality of free radical photo-initiation is the 0.5-3% of resin gross mass in step 2.2 in step 2.3；
The quality of nano material is the 0.5-5% of metal dust gross mass in step 2.2 mixed-powder in the step 2.3.
7. the manufacturing process of a kind of metal-base nanometer composite material part according to claim 1, it is characterised in that described Stir speed (S.S.) 300-600rad/min in step 2.3, mixing time 1-4h.
8. the manufacturing process of a kind of metal-base nanometer composite material part according to claim 1, it is characterised in that described The parameter of optical soliton interaction equipment is in step 3：The a length of 200-400nm of light wave used, lift height used is 10- during shaping 100um。
9. the manufacturing process of a kind of metal-base nanometer composite material part according to claim 1, it is characterised in that described Step 4.2 needs to judge whether to pre-burning according to the characteristic of part material therefor before sintering, specifically joins if pre-burning is carried out Number is：Under the conditions of environment, gas pressure 10-200MPa in argon gas protection, 800-900 is warming up to the speed of 3-5 DEG C/min DEG C, keep the temperature 0.5-2h.
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