CN108031841B - Forming method of metal-based nano composite material part - Google Patents

Forming method of metal-based nano composite material part Download PDF

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CN108031841B
CN108031841B CN201711050358.5A CN201711050358A CN108031841B CN 108031841 B CN108031841 B CN 108031841B CN 201711050358 A CN201711050358 A CN 201711050358A CN 108031841 B CN108031841 B CN 108031841B
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metal
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CN108031841A (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

Abstract

The invention discloses a forming method of a metal-based nano composite material part, which comprises the following steps: step 1, preprocessing a nano material and a metal material; step 2, preparing nano enhanced metal-based composite photo-curing slurry; step 3, carrying out photocuring forming; and 4, degreasing and sintering. The forming method of the invention effectively reduces the agglomeration of nano particles in the forming process by pre-treating the metal powder and the nano material and using high-energy ultrasonic waves in the whole process; the complexity of the formed part is improved by the combination of the preparation of the nano enhanced metal-based composite photo-curing slurry and the photo-curing technology; the rapid sintering is carried out at the temperature lower than the interface reaction, so that the interface reaction of the nano particles in the whole process is reduced; simple steps and good practical value.

Description

Forming method of metal-based nano composite material part
Technical Field
The invention belongs to the technical field of photocuring forming methods, and particularly relates to a forming method of a metal-based nano composite material part.
Background
The metal-based nano composite material has the characteristics of high strength, good toughness, excellent thermal stability and the like, and has wide application prospect in high and new technical fields of aviation, aerospace, automation and the like. The current forming method of metal-based nano composite material parts mainly comprises two methods: liquid casting methods and solid state sintering methods. The liquid casting method can obtain a near-net-shape complex part, but needs a mould, has interface reaction and is difficult to control the components; the solid state sintering method is easy to control the components, but particle agglomeration is easy to occur and only simple and small parts can be obtained. Therefore, at present, no method for realizing rapid forming of high-performance complex metal-based nanocomposite parts exists.
Disclosure of Invention
The invention aims to provide a forming method of a metal-based nano composite part, which solves the problems of strong interface reaction and agglomeration and difficulty in preparing complex parts in the existing forming method of the metal-based nano composite part.
The technical scheme adopted by the invention is that the forming method of the metal-based nano composite material part comprises the following steps:
step 1, pretreatment of metal powder and nano material
Step 2, preparation of nano enhanced metal-based composite photo-curing slurry
Step 2.1, putting the metal powder treated in the step 1 into a planetary ball mill, simultaneously adding a proper amount of dispersing agent and phase solvent, taking absolute ethyl alcohol as a medium, carrying out ball milling for 2-8h at a ball-to-material ratio of 1:1, then filtering and drying for 10h at 120 ℃ to obtain mixed powder;
2.2, putting a proper amount of resin into a stirrer, adding the mixed powder obtained in the step 2.1 into the stirrer at least three times, adding a proper amount of diluent into the mixed powder at the same time during each addition, and stirring the mixture to uniformly mix the diluent to obtain a mixture;
step 2.3, under the condition of keeping out of the sun, adding a proper amount of free radical photoinitiator and the nano material treated in the step 1 into the mixture obtained in the step 2.2, performing ultrasonic dispersion and mechanical stirring treatment, and uniformly mixing to obtain nano enhanced metal-based composite photo-curing slurry;
step 2.4, under the conditions of light shielding and negative pressure not greater than-0.06 MPa, continuing high-energy ultrasonic treatment on the nano enhanced metal-based composite photo-curing slurry obtained in the step 2.3 for 8-12 hours for later use;
step 3, photocuring forming
Guiding the processed three-dimensional model information of the part to be formed into a photocuring forming device, forming a blank of the required part by using the nano enhanced metal-based composite photocuring slurry obtained in the step 2.4, and carrying out high-energy ultrasonic treatment on uncured slurry in a feeding device in the photocuring forming device all the time in the forming process;
step 4, degreasing and sintering
Step 4.1, degreasing
Placing the blank in the step 3 in a roasting furnace, heating to 350-600 ℃ at the speed of 3-5 ℃/min under the normal pressure and argon environment, and preserving heat for 1-10 h; then vacuumizing, preserving heat for the same time, and cooling along with the furnace;
step 4.2, sintering
And (3) heating the blank treated in the step (4.1) to 600-1300 ℃ at the heating rate of 5-10 ℃/min under the conditions of the argon protection environment and the gas pressure of 10-200MPa, and preserving the heat for 0.5-3h to obtain the required metal-based nanocomposite part.
The present invention is also characterized in that,
the pretreatment of the metal powder in the step 1 specifically comprises the following steps: selecting the particle diameter d501-10um matrix metal powder, and drying for 2-10h in a vacuum environment with the temperature of 200-250 ℃ and the atmospheric pressure of not more than-0.06 MPa;
the pretreatment of the nano material in the step 1 specifically comprises the following steps: dispersing and cleaning the nano particles under the combined action of ultrasonic dispersion and mechanical stirring, and then drying for 20-30h under a vacuum environment with the temperature of 100-180 ℃ and the atmospheric pressure of not more than-0.06 MPa.
2.2, the resin is free radical resin, specifically unsaturated polyester or acrylate, and the diluent is acrylate, vinyl or vinyl ether; in the step 2.1, the dispersant is ammonium polyacrylate or ammonium citrate, and the phase solvent is stearic acid or polyalcohol;
in the step 2.3, the free radical photoinitiator is benzoin derivatives, acyl phosphine oxides or organic sulfur-containing compounds;
wherein the resin, the dispersant, the diluent, the phase solvent and the free radical photoinitiator are dried before use.
In the step 2.2, the volume fraction ratio of the metal powder to the resin in the mixed powder is 1-3: 1;
the total adding amount of the dispersing agent is 0.1-1% of the mass of the metal powder, and the total adding amount of the phase solvent is 0.18-2% of the mass of the metal powder; the total amount of the diluent added in each time is 0.1-1.5% of the mass of the metal powder.
The temperature is 25-35 ℃ when mixing in the step 2.2; stirring parameters: the rotation speed under normal pressure is 280 plus 600rad/min, and the stirring time is 4-8 h.
In the step 2.3, the mass of the free radical photoinitiator is 0.5-3% of the total mass of the resin in the step 2.2;
the mass of the nano material in the step 2.3 is 0.5-5% of the total mass of the metal powder in the mixed powder in the step 2.2.
In the step 2.3, the stirring speed is 300- & lt 600rad/min, and the stirring time is 1-4 h.
In step 3, the parameters of the photocuring forming equipment are as follows: the wavelength of the used light is 200-400nm, and the thickness of the used lamination is 10-100 um.
Step 4.2, before sintering, judging whether to perform pre-sintering according to the characteristics of the material used by the part, wherein if the pre-sintering is performed, the specific parameters are as follows: under the condition of argon protection and gas pressure of 10-200MPa, the temperature is raised to 800-900 ℃ at the speed of 3-5 ℃/min, and the temperature is maintained for 0.5-2 h.
The invention has the beneficial effects that: according to the forming method of the metal-based nano composite material part, high-energy ultrasonic waves are used in the whole process through the pretreatment of metal powder and nano materials, so that the agglomeration of nano particles in the forming process is effectively reduced; the complexity of the formed part is improved by the combination of the preparation of the nano enhanced metal-based composite photo-curing slurry and the photo-curing technology; the rapid sintering is carried out at the temperature lower than the interface reaction, so that the interface reaction of the nano particles in the whole process is reduced; simple steps and good practical value.
Detailed Description
The molding method of the present invention will be described in detail below with reference to specific embodiments.
The invention relates to a forming method of a metal-based nano composite material part, which specifically comprises the following steps:
step 1, pretreatment of metal powder and nano material
The pretreatment of the metal powder comprises the following specific steps: selecting the particle diameter d501-10um matrix metal powder, and drying for 2-10h in a vacuum environment with the temperature of 200-250 ℃ and the atmospheric pressure of not more than-0.06 MPa;
the pretreatment of the nano material comprises the following specific steps: dispersing and cleaning the nano particles under the combined action of ultrasonic dispersion and mechanical stirring, and then drying for 20-30h under a vacuum environment with the temperature of 100-180 ℃ and the atmospheric pressure of not more than-0.06 MPa.
Step 2, preparation of nano enhanced metal-based composite photo-curing slurry
Step 2.1, putting the metal powder treated in the step 1 into a planetary ball mill, simultaneously adding a proper amount of dried dispersing agent and phase solvent, ball-milling for 2-8h at a ball-to-material ratio of 1:1 by using absolute ethyl alcohol as a medium, filtering and drying for 10h at 120 ℃ to obtain mixed powder,
the dispersant is ammonium polyacrylate or ammonium citrate, and the phase solvent is stearic acid or polyalcohol;
2.2, putting a proper amount of dried resin into a stirrer, adding the mixed powder obtained in the step 2.1 into the stirrer for at least three times, adding a proper amount of diluent into the mixed powder at the same time when adding the diluent each time, and stirring the mixture to uniformly mix the diluent to obtain a mixture;
wherein the resin is free radical type resin, specifically unsaturated polyester or acrylate, and the diluent is acrylate, vinyl or vinyl ether; the total adding amount of the dispersing agent is 0.1-1% of the mass of the metal powder in the mixed powder; the total amount of the diluent is 0.1-1.5% of the mass of the metal powder in the mixed powder; the total addition amount of the phase solvent is 0.18-2% of the mass of the metal powder; the temperature is 25-35 ℃ during mixing; stirring parameters: the rotation speed under normal pressure is 280 plus 600rad/min, and the stirring time is 4-8 h;
step 2.3, under the condition of keeping out of the sun, adding a proper amount of free radical photoinitiator subjected to drying treatment and the nano material treated in the step 1 into the mixture obtained in the step 2.2, performing ultrasonic dispersion and mechanical stirring treatment, and stirring at the speed of 300-600rad/min for 1-4h to uniformly mix the mixture to obtain nano enhanced metal-based composite photocuring slurry;
wherein the free radical photoinitiator is benzoin derivative, acyl phosphine oxide or organic sulfur-containing compound; the mass of the free radical photoinitiator is 0.5-3% of the total mass of the resin, and the mass of the nano material is 0.5-5% of the total mass of the metal powder;
and 2.4, under the conditions of light shielding and negative pressure not greater than-0.06 MPa, continuing high-energy ultrasonic treatment on the nano enhanced metal-based composite photo-curing slurry obtained in the step 2.3 for 8-12h to remove bubbles in the slurry and remove bubbles in the slurry for later use.
Step 3, photocuring forming
Guiding the processed three-dimensional model information of the part to be formed into a photocuring forming device, forming a blank of the required part by using the nano enhanced metal-based composite photocuring slurry obtained in the step 2.4, and carrying out high-energy ultrasonic treatment on uncured slurry in a feeding device in the photocuring forming device all the time in the forming process; the light wavelength used by the light curing forming equipment is 200-400nm, and the thickness of the layer used during forming is 10-100 um.
Step 4, degreasing and sintering
Step 4.1, degreasing
Placing the blank in the step 3 in a roasting furnace, heating to 350-600 ℃ at the speed of 3-5 ℃/min under the normal pressure and argon environment, preserving heat for 1-10h, and cooling along with the furnace; then vacuumizing, preserving heat for the same time, and cooling along with the furnace;
step 4.2, sintering
And (3) selecting whether to pre-sinter the blank treated in the step 4.1 before sintering according to the requirements of different parts, wherein the specific pre-sintering parameters are as follows: under the condition of argon protection and gas pressure of 10-200MPa, heating to 800-900 ℃ at the speed of 3-5 ℃/min, and preserving heat for 0.5-2 h;
then, under the condition of argon protection and gas pressure of 10-200MPa, the temperature is raised to 600-1300 ℃ at the heating rate of 5-10 ℃/min, and the temperature is preserved for 0.5-3h to obtain the required metal-based nanocomposite part.
The forming method of the invention effectively reduces the agglomeration of nano particles in the forming process by pre-treating the metal powder and the nano material and using high-energy ultrasonic waves in the whole process; the complexity of the formed part is improved by the combination of the preparation of the nano enhanced metal-based composite photo-curing slurry and the photo-curing technology; the rapid sintering is carried out at the temperature lower than the interface reaction, so that the interface reaction of the nano particles in the whole process is reduced; simple steps and good practical value.
Example 1: carbon nanotube/aluminum-based composite material part
(1) Pretreatment of metal powders and nanomaterials
The pretreatment of the metal powder comprises the following specific steps: will d501um AlSi10Mg powder, drying at 200 deg.C under vacuum condition with atmospheric pressure no greater than-0.06 MPa for 5 h;
the pretreatment of the nano material comprises the following specific steps: treating the carbon nano tube by alcohol under the combined action of ultrasonic dispersion and mechanical stirring, and then drying for 20 hours in a vacuum environment at the temperature of 100 ℃ and the atmospheric pressure of not more than-0.06 MPa.
(2) Preparation of nano reinforced metal-based composite photo-curing slurry
Drying the 1, 6-hexanediol diacrylate; dispersant ammonium polyacrylate, diluent isobornyl acrylate, phase solvent polyol and free radical photoinitiator benzoin dimethyl ether.
1620g of AlSi10Mg metal powder is loaded into a planetary ball mill, 8.1g of dispersant ammonium polyacrylate and 16.2g of phase solvent polyalcohol are added simultaneously, ball milling is carried out for 2h under the ball-material ratio of 1:1 by taking absolute ethyl alcohol as a medium, and drying is carried out for 10h at 120 ℃ after filtration;
adding the metal powder treated in the steps and 400ml of 1, 6-hexanediol diacrylate radical type resin (the volume fraction ratio of the metal powder to the radical type resin is 3:2) into a stirrer for three times to be uniformly mixed to obtain a mixture; adding a diluent of isobornyl acrylate in each addition, wherein the total amount of isobornyl acrylate added in each addition is 16.2g, the mixing temperature is 35 ℃, the stirring parameters are as follows, and stirring is carried out for 8 hours at the rotating speed of 400rad/min under normal pressure;
under the condition of keeping out of the sun, continuously adding 12g of benzoin dimethyl ether and 56.7g of carbon nano tubes into the mixture, stirring and carrying out high-energy ultrasonic treatment, wherein the stirring speed is 350rad/min, and the treatment time is 4h, so that the materials are uniformly mixed to prepare the carbon nano tube/aluminum-based composite photo-curing slurry;
and under the conditions of light shielding and negative pressure not greater than-0.06 MPa, continuously carrying out high-energy ultrasonic treatment on the carbon nano tube/aluminum-based composite photocuring slurry for 8 hours to remove air bubbles in the slurry for later use.
(3) Photocuring forming
Guiding the processed three-dimensional model information of the part to be formed into a photocuring forming device, and forming a blank of the required part by using the carbon nano tube/aluminum-based composite photocuring slurry; the light wavelength used by the light curing forming equipment is 355nm, the layering thickness used during forming is 20um, and the high-energy ultrasonic treatment is always carried out on the uncured slurry in the feeding device during the forming process.
(4) Degreasing and sintering
And (4) placing the blank in the step (3) in a roasting furnace for degreasing treatment. The degreasing process comprises the following steps: heating to 350 ℃ at the speed of 3 ℃/min under the normal pressure and argon environment, and preserving heat for 10 hours; then vacuumizing, and cooling along with the furnace after the same heat preservation time.
And then sintering, wherein the sintering process comprises the following steps: under the protection of argon, the gas pressure is 200MPa, the temperature is raised to 630 ℃ at the speed of 10 ℃/min, and the temperature is kept for 2h to obtain the required carbon nano tube/aluminum matrix composite part.
Example 2: carbon nanotube/copper-based composite material part
(1) Pretreatment of metal powders and nanomaterials
The pretreatment of the metal powder comprises the following specific steps: will d50H65 powder of 10um, drying for 2H at 200 deg.C under vacuum condition with atmospheric pressure not greater than-0.06 MPa;
the pretreatment of the nano material comprises the following specific steps: treating the carbon nano tube by alcohol under the combined action of ultrasonic dispersion and mechanical stirring, and then drying for 20 hours in a vacuum environment at the temperature of 100 ℃ and the atmospheric pressure of not more than-0.06 MPa.
(2) Preparation of nano reinforced metal-based composite photo-curing slurry
Drying the 1, 6-hexanediol diacrylate; dispersant ammonium citrate, diluent vinyl ether, phase solvent polyalcohol and free radical photoinitiator benzoin dimethyl ether.
4275g H65 metal powder is put into a planetary ball mill, 4.275g of dispersant ammonium citrate and 7.695g of phase solvent polyalcohol are added at the same time, the mixture is ball milled for 2 hours at the ball-to-material ratio of 1:1 by taking absolute ethyl alcohol as a medium, and the mixture is dried for 10 hours at 120 ℃ after being filtered;
adding the metal powder treated in the steps and 500ml of 1, 6-hexanediol diacrylate radical type resin (the volume fraction ratio of the metal powder to the radical type resin is 1:1) into a stirrer for three times to be uniformly mixed; adding diluent vinyl ether during each addition, wherein the total amount of the added vinyl ether is 4.275g, the mixing temperature is 20 ℃, the stirring parameters are that stirring is carried out for 8h at the rotation speed of 280rad/min under normal pressure;
under the condition of keeping out of the sun, continuously adding 15g of benzoin dimethyl ether and 21.375g of carbon nano tubes into the mixture, stirring and carrying out high-energy ultrasonic treatment, wherein the stirring speed is 280rad/min, and the treatment time is 4h, so that the materials are uniformly mixed to prepare the carbon nano tube/copper-based composite photocuring slurry;
and under the conditions of light shielding and negative pressure not greater than-0.06 MPa, continuing to perform high-energy ultrasonic treatment on the carbon nanotube/copper-based composite photocuring slurry for 8 hours to remove air bubbles in the slurry for later use.
(3) Photocuring forming
Guiding the processed three-dimensional model information of the part to be formed into a photocuring forming device, and forming a blank of the required part by using the carbon nano tube/copper-based composite photocuring slurry; the light wavelength used by the light curing forming equipment is 355nm, the layering thickness used during forming is 10um, and the high-energy ultrasonic treatment is always carried out on the uncured slurry in the feeding device during the forming process.
(4) Degreasing and sintering
And (4) placing the blank in the step (3) in a roasting furnace for degreasing treatment. The degreasing process comprises the following steps: heating to 400 ℃ at the speed of 5 ℃/min under the normal pressure and argon environment, and preserving heat for 1 h; then vacuumizing, and cooling along with the furnace after the same heat preservation time.
And then sintering, wherein the sintering process comprises the following steps: under the protection of argon, the gas pressure is 100MPa, the temperature is raised to 600 ℃ at the speed of 5 ℃/min, and the temperature is kept for 2h to obtain the required carbon nano tube/copper-based composite material part.
Example 3: TiC/titanium alloy composite material part
(1) Pretreatment of metal powders and nanomaterials
The pretreatment of the metal powder comprises the following specific steps: will d50Drying 8um TC4 powder at 250 deg.C under vacuum of no more than-0.06 MPa for 6 hr;
the pretreatment of the nano material comprises the following specific steps: and (2) treating the TiC nano particles by using alcohol under the combined action of ultrasonic dispersion and mechanical stirring, and then drying for 30 hours at the temperature of 100 ℃ under a vacuum environment with the atmospheric pressure of not more than-0.06 MPa.
(2) Preparation of nano reinforced metal-based composite photo-curing slurry
Drying the 1, 6-hexanediol diacrylate; dispersant ammonium citrate, diluent vinyl ether, phase solvent polyalcohol and free radical photoinitiator benzoin dimethyl ether.
3382.5g of TC4 powder is loaded into a planetary ball mill, 33.825g of dispersant ammonium citrate and 67.65g of phase solvent polyalcohol are added simultaneously, the mixture is ball milled for 8 hours under the ball-material ratio of 1:1 by taking absolute ethyl alcohol as a medium, and the mixture is dried for 10 hours at 120 ℃ after being filtered;
adding the metal powder treated by the steps and 250ml of 1, 6-hexanediol diacrylate radical type resin (the volume fraction ratio of the metal powder to the radical type resin is 3:1) into a stirrer for three times to be uniformly mixed; adding diluent vinyl ether during each addition, wherein the total amount of the added vinyl ether is 50.7375g, the mixing temperature is 35 ℃, the stirring parameters are that stirring is carried out for 6h at the normal pressure and the rotating speed of 600 rad/min;
under the condition of keeping out of the sun, continuously adding 7.5g of benzoin dimethyl ether and 169.125g of TiC nano-particles into the mixture, stirring and performing high-energy ultrasonic treatment, wherein the stirring speed is 280rad/min, and the treatment time is 4h, so that the materials are uniformly mixed to prepare TiC nano-particles/TC 4 composite photocuring slurry;
and under the conditions of light shielding and negative pressure not greater than-0.06 MPa, carrying out high-energy ultrasonic treatment on the TiC nano-particles/TC 4 composite photocuring slurry for 8 hours to remove air bubbles in the slurry for later use.
(3) Photocuring forming
Guiding the processed three-dimensional model information of the part to be formed into a photocuring forming device, and forming a blank of the required part by utilizing TiC nano-particle/TC 4 composite photocuring slurry; the light wavelength used by the light curing forming equipment is 355nm, the layering thickness used during forming is 60um, and the high-energy ultrasonic treatment is always carried out on the uncured slurry in the feeding device during the forming process.
(4) Degreasing and sintering
And (4) placing the blank in the step (3) in a roasting furnace for degreasing treatment. The degreasing process comprises the following steps: heating to 600 ℃ at the speed of 3 ℃/min under the environment of normal pressure and argon, and preserving heat for 5 hours; then vacuumizing, and cooling along with the furnace again after the same heat preservation time.
And (3) sintering, namely, ① presintering, heating to 800 ℃ at the speed of 5 ℃/min under the condition of argon protection and under the gas pressure of 10MPa, and preserving heat for 0.5h, ② sintering, heating to 1200 ℃ at the speed of 5 ℃/min under the same pressure after presintering is finished, and preserving heat for 3h to obtain the required TiC nano-particle/TC 4 composite material part.
Example 4: graphene/nickel-based superalloy composite part
(1) Pretreatment of metal powders and nanomaterials
The pretreatment of the metal powder comprises the following specific steps: will d50FGH4095 powder of 1um is dried for 10h at 250 deg.C under vacuum condition with atmospheric pressure not more than-0.06 MPa;
the pretreatment of the nano material comprises the following specific steps: treating the graphene nanoparticles with alcohol under the combined action of ultrasonic dispersion and mechanical stirring, and then drying for 20h in a vacuum environment at the temperature of 180 ℃ and the atmospheric pressure of not more than-0.06 MPa.
(2) Preparation of nano reinforced metal-based composite photo-curing slurry
Drying the polyester acrylate; dispersant ammonium polyacrylate, diluent vinyl ether, phase solvent polyalcohol and free radical photoinitiator Irgacure 250.
Loading 5544g of FGH4095 metal powder into a planetary ball mill, simultaneously adding 27.22g of dispersant ammonium polyacrylate and 11.088g of phase solvent polyol, ball-milling for 6h at a ball-to-material ratio of 1:1 by using absolute ethyl alcohol as a medium, filtering, and drying at 120 ℃ for 10 h;
adding the metal powder treated by the steps and 400ml of polyester acrylate free radical type resin (the volume fraction ratio of the metal powder to the free radical type resin is 3:2) into a stirrer for three times to be uniformly mixed; adding diluent vinyl ether during each addition, wherein the total amount of the added vinyl ether is 5.544g each time, the mixing temperature is 30 ℃, the stirring parameters are that stirring is carried out for 8 hours at the normal pressure and at the rotating speed of 350 rad/min;
under the condition of keeping out of the sun, continuously adding 8g of benzoin dimethyl ether and 110.88g of graphene nano-particles into the mixture, stirring and performing high-energy ultrasonic treatment at the stirring speed of 600rad/min for 4h, and uniformly mixing to prepare graphene nano-particle/nickel-based high-temperature alloy composite photo-curing slurry;
and under the conditions of light shielding and negative pressure not greater than-0.06 MPa, continuously carrying out high-energy ultrasonic treatment on the graphene nanoparticle/nickel-based superalloy composite photocuring slurry for 12 hours to remove air bubbles in the slurry for later use.
(3) Photocuring forming
Guiding the processed three-dimensional model information of the part to be formed into a photocuring forming device, and forming a blank of the required part by using the graphene nanoparticle/nickel-based superalloy composite photocuring slurry; the light wavelength used by the light curing forming equipment is 355nm, the layering thickness used during forming is 100um, and the uncured slurry in the feeding device is always subjected to high-energy ultrasonic treatment in the forming process.
(4) Degreasing and sintering
And (4) placing the blank in the step (3) in a roasting furnace for degreasing treatment. The degreasing process comprises the following steps: heating to 660 ℃ at the speed of 3 ℃/min under the normal pressure and argon environment, and preserving heat for 2 h; then vacuumizing, and cooling along with the furnace again after the same heat preservation time.
And sintering, namely ① presintering, heating to 8900 ℃ at the speed of 5 ℃/min under the condition of argon protection and the gas pressure of 100MPa, and keeping the temperature for 2h, ② sintering, heating to 1300 ℃ at the speed of 5 ℃/min under the same pressure after presintering, and keeping the temperature for 2h to obtain the graphene nanoparticle/nickel-based high-temperature alloy composite part.

Claims (4)

1. A method of forming a metal matrix nanocomposite part, comprising the steps of:
step 1, pretreating metal powder and nano materials:
the pretreatment of the metal powder comprises the following specific steps: selecting the particle diameter d501-10um matrix metal powder, and drying for 2-10h in a vacuum environment with the temperature of 200-250 ℃ and the atmospheric pressure of not more than-0.06 MPa;
the pretreatment of the nano material comprises the following specific steps: dispersing and cleaning the nano particles under the combined action of ultrasonic dispersion and mechanical stirring, and then drying for 20-30h under a vacuum environment with the temperature of 100-180 ℃ and the atmospheric pressure of not more than-0.06 MPa;
step 2, preparation of nano enhanced metal-based composite photo-curing slurry
Step 2.1, putting the metal powder treated in the step 1 into a planetary ball mill, adding a dispersing agent and a phase solvent at the same time, ball-milling for 2-8h at a ball-to-material ratio of 1:1 by taking absolute ethyl alcohol as a medium, filtering and drying for 10h at 120 ℃ to obtain mixed powder;
step 2.2, putting the resin into a stirrer, adding the mixed powder obtained in the step 2.1 into the stirrer at least three times, adding the diluent into the mixed powder at the same time when adding the diluent each time, and stirring the mixture to uniformly mix the diluent and the diluent to obtain a mixture;
the volume fraction ratio of the metal powder to the resin in the mixed powder in the step 2.2 is 1-3: 1; the total adding amount of the dispersing agent is 0.1-1% of the mass of the metal powder, the total adding amount of the phase solvent is 0.18-2% of the mass of the metal powder, and the total adding amount of the diluents in each time is 0.1-1.5% of the mass of the metal powder;
step 2.3, adding a free radical photoinitiator and the nano material treated in the step 1 into the mixture obtained in the step 2.2 under a dark condition, performing ultrasonic dispersion and mechanical stirring treatment, and uniformly mixing to obtain nano enhanced metal-based composite photo-curing slurry;
the mass of the free radical photoinitiator in the step 2.3 is 0.5-3% of the total mass of the resin in the step 2.2; the mass of the nano material in the step 2.3 is 0.5-5% of the total mass of the metal powder in the mixed powder in the step 2.2;
step 2.4, under the conditions of light shielding and negative pressure not greater than-0.06 MPa, continuing high-energy ultrasonic treatment on the nano enhanced metal-based composite photo-curing slurry obtained in the step 2.3 for 8-12 hours for later use;
step 3, photocuring forming
Guiding the processed three-dimensional model information of the part to be formed into a photocuring forming device, forming a blank of the required part by using the nano enhanced metal-based composite photocuring slurry obtained in the step 2.4, and carrying out high-energy ultrasonic treatment on uncured slurry in a feeding device in the photocuring forming device all the time in the forming process;
the parameters of the photocuring forming equipment are as follows: the wavelength of the used light is 200-400nm, and the thickness of the used layering is 10-100um during forming;
step 4, degreasing and sintering
Step 4.1, degreasing
Placing the blank in the step 3 in a roasting furnace, heating to 350-600 ℃ at the speed of 3-5 ℃/min under the normal pressure and argon environment, and preserving heat for 1-10 h; then vacuumizing, preserving heat for the same time, and cooling along with the furnace;
step 4.2, sintering
Raising the temperature of the blank treated in the step 4.1 to 600-1300 ℃ at the temperature rise rate of 5-10 ℃/min under the conditions of the argon protection environment and the gas pressure of 10-200MPa, and preserving the heat for 0.5-3h to obtain the required metal-based nanocomposite part;
step 4.2, before sintering, whether to perform pre-sintering is judged according to the characteristics of the material used by the part, and if the pre-sintering is performed, the specific parameters are as follows: under the condition of argon protection and gas pressure of 10-200MPa, the temperature is raised to 800-900 ℃ at the speed of 3-5 ℃/min, and the temperature is maintained for 0.5-2 h.
2. The method of claim 1, wherein in step 2.2 the resin is a free radical resin, specifically an unsaturated polyester, and the diluent is an acrylate or vinyl; in the step 2.1, the dispersant is ammonium polyacrylate or ammonium citrate, and the phase solvent is stearic acid or polyalcohol;
the free radical photoinitiator in the step 2.3 is benzoin derivative, acyl phosphine oxide or organic sulfur-containing compound;
wherein the resin, the dispersant, the diluent, the phase solvent and the free radical photoinitiator are dried before use.
3. The method for forming a metal-matrix nanocomposite part according to claim 1, wherein the temperature of the mixing in the step 2.2 is 25 to 35 ℃; stirring parameters: the rotation speed under normal pressure is 280 plus 600rad/min, and the stirring time is 4-8 h.
4. The method as claimed in claim 1, wherein the stirring speed in step 2.3 is 300-600rad/min, and the stirring time is 1-4 h.
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