CN109128149A - The method for preparing three-dimensional carbon nanomaterial in aluminium powder surface in situ using sodium chloride template - Google Patents
The method for preparing three-dimensional carbon nanomaterial in aluminium powder surface in situ using sodium chloride template Download PDFInfo
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- CN109128149A CN109128149A CN201810962953.4A CN201810962953A CN109128149A CN 109128149 A CN109128149 A CN 109128149A CN 201810962953 A CN201810962953 A CN 201810962953A CN 109128149 A CN109128149 A CN 109128149A
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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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/16—Metallic particles coated with a non-metal
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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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/06—Metallic powder characterised by the shape of the particles
- B22F1/065—Spherical particles
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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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
Abstract
The present invention relates to a kind of methods for preparing three-dimensional carbon nanomaterial in aluminium powder surface in situ using sodium chloride template, including following procedure: (1) sodium chloride template primary reconstruction three-dimensional carbon nanomaterial presoma；(2) aluminium powder surface ball milling loads self assembled three-dimensional carbon nanomaterial presoma；(3) calcining reduction in situ synthesizes three-dimensional carbon nanomaterial/aluminium composite powder: three-dimensional carbon nanomaterial presoma/aluminium composite powder that step (2) is obtained is placed in tube furnace, argon gas is passed through as carrier gas, 600 DEG C are warming up to 10 DEG C/min, 60min；Then high-temperature calcination reduction is carried out using argon gas, hydrogen gas mixture as carrier gas, filtered, washing obtains three-dimensional carbon nanomaterial/aluminium composite powder after removing sodium chloride template；(4) cold pressing-sinter molding of three-dimensional carbon nanomaterial/aluminium composite material block: the extrusion deformation processing of (5) three-dimensional carbon nanomaterial/aluminium composite material block.
Description
Technical field
It the present invention relates to the use of the method that sodium chloride template prepares three-dimensional carbon nanomaterial in aluminium powder surface in situ, and relate to
And composite powder forming technique and composite materials property, belong to powder metallurgical technology.
Background technique
Metal-base composites have high specific strength, specific modulus, good thermally conductive, electric conductivity, wearability, high-temperature behavior,
The excellent properties such as low thermal expansion coefficient and high dimensional stability have it in fields such as aerospace, electronics and automobiles
Have wide practical use.In numerous metal-base composites, aluminum matrix composite is with fastest developing speed, because of aluminum-base composite material
Material is with density is small, corrosion-resistant, processing performance is good, matrix alloy range of choice is wide, heat treatment performance is good and preparation process spirit
The advantages that living.According to the difference of reinforced phase and matrix composite pathway, additional reinforcement and In-sltu reinforcement body can be divided into.
Carbon nanomaterial is the ideal nanometer activeness and quietness material of metal-base composites, is attracted attention by scientific research personnel, tool
There are critically important researching value and application prospect.In recent years, carbon nanomaterial reinforced aluminum matrix composites are rapidly developed,
Traditional preparation method is to be dispersed in it in aluminum substrate by additional mode to obtain composite material, ball is usually used
Grinding process is dispersed, and what good dispersion effect was often obtained by prolonged mechanical milling process, therefore high-energy ball milling meeting
Destroy the structural intergrity of carbon nanomaterial, therefore researcher begins one's study and carries out carbon by way of growth in situ and receive
Dispersion of the rice material in metal powder surface.
Due to the limitation of the intrinsic scale of carbon nanomaterial, making it difficult to, which improves composite material obdurability, is inverted relationship
Bottleneck problem.Three-dimensional carbon nanometer network shape structure is integrated with unique spatial structure characteristic and the unique physics of carbon nanomaterial
Chemical property not only has the design feature for being not easy stacking reunion, high-specific surface area, but also has excellent mechanical property.
If the excellent mechanical property such as its high intensity, high elastic modulus can be introduced into aluminum matrix composite, and designed in configuration
On make carbon nanomaterial present three-dimensional network-like structure, theoretically will greatly improve alumina-base material mechanical property.
This invents the series methods using " template cladding-calcining reduction-shaping and deformation ", as sodium chloride template
In the method that aluminium powder surface in situ prepares three-dimensional carbon nanomaterial, and it is related to composite powder forming technique and Compound Material Engineering
Energy method, can make three-dimensional carbon nano material evenly dispersed on aluminium powder surface, and composite block material after molding is by subsequent
Hot extrusion deformation processing, can be further improved compactness, obtain the excellent mechanical performance of obdurability collaboration enhancing.
Summary of the invention
The purpose of the present invention is to provide a kind of powder metallurgy fabricated in situ three-dimensional carbon nanomaterial/aluminium of simple process is multiple
The method of condensation material.This method can effectively overcome the problems, such as that this method process is simple brought by the additional carbon nanomaterial of tradition
Easy, obtained composite materials property is excellent.To achieve the above object, the present invention is to be subject to reality by the following technical programs
Existing,
A method of three-dimensional carbon nanomaterial, including following mistake are prepared in aluminium powder surface in situ using sodium chloride template
Journey:
(1) sodium chloride template primary reconstruction three-dimensional carbon nanomaterial presoma:
According to quality proportioning it is 10:0.2-0.5 by sodium chloride and DEXTROSE ANHYDROUS, is dissolved in appropriate ionized water, freezes
It is lyophilized again afterwards, grinding obtains three-dimensional carbon nanomaterial precursor powder after freeze-drying；
(2) aluminium powder surface ball milling loads self assembled three-dimensional carbon nanomaterial presoma:
The ball aluminum powder that three-dimensional carbon nanomaterial precursor powder made from step (1) and 400 mesh are sieved is subjected to ball milling
Mixing obtains three-dimensional carbon nanomaterial presoma/aluminium composite powder；
(3) calcining reduction in situ synthesizes three-dimensional carbon nanomaterial/aluminium composite powder:
Three-dimensional carbon nanomaterial presoma/aluminium composite powder that step (2) is obtained is placed in tube furnace, is passed through argon gas work
For carrier gas, 600 DEG C are warming up to 10 DEG C/min, 60min；Then high-temperature calcination is carried out using argon gas, hydrogen gas mixture as carrier gas
Reduction filters, washing obtains three-dimensional carbon nanomaterial/aluminium composite powder after removing sodium chloride template；
(4) cold pressing-sinter molding of three-dimensional carbon nanomaterial/aluminium composite material block:
Three-dimensional carbon nanomaterial made from step (3)/aluminium composite powder is subjected to cold moudling, then sintering processes, obtain
To three-dimensional carbon nanomaterial/aluminium composite material block；
(5) the extrusion deformation processing of three-dimensional carbon nanomaterial/aluminium composite material block:
Three-dimensional carbon nanomaterial/aluminium composite material block made from step (4) is put into box type heater and is heated, then
Hot extrusion deformation processing is carried out, As-extruded composite material block is obtained.
Preferably, the process conditions of step (4) are as follows: carry out 600MPa cold moudling, be then sintered in tube furnace
Processing, sintering temperature are set in 630 DEG C, and sintering time 1h, protective atmosphere is argon gas.When step (5) hot extrusion, box heating
Furnace set temperature is 550 DEG C, extrusion ratio 16:1.
The invention has the following advantages that preparing three-dimensional carbon nanomaterial presoma by template of sodium chloride first, pass through ball
Presoma is supported on aluminium powder surface by mill dispersing technology, and three-dimensional carbon nanomaterial/aluminium composite powder is obtained after calcining reduction, in conjunction with
PM technique prepares composite material block.Three-dimensional carbon nanomaterial/the aluminium composite material prepared using this method is stretched
Performance realizes the collaboration enhancing of obdurability.
The present invention using sodium chloride template in aluminium powder surface in situ growing three-dimensional carbon nanometer reinforcement, and by molding and
Deformation technique realizes the design to microstructure of composite structure, optimizes the performance of composite material, before showing preferable application
Scape.
Detailed description of the invention
Fig. 1 is the scanned photograph of aluminium powder before and after ball milling in embodiment 1.
Fig. 2 is the scanned photograph of surfactant aluminium powder before and after the processing in embodiment 1.
Fig. 3 is to be compounded in spherical and Flake Aluminum Powder Coated three-dimensional carbon nanomaterial using liquid phase wet process in embodiment 1
The scanned photograph of presoma.
Fig. 4 is the microregion element energy spectrum diagram of aluminium powder surface coating layer in embodiment 1.
Fig. 5 is that three-dimensional carbon nanomaterial/aluminium composite powder erodes the transmission photo after aluminum substrate in embodiment 1.
Fig. 6 is to coat sweeping for three-dimensional carbon nanomaterial presoma on aluminium powder surface using solid phase dry ball milling in embodiment 2
Retouch photo.
Fig. 7 is to coat three-dimensional carbon nanomaterial in aluminium powder surface in situ after precursor powder calcining reduction in embodiment 2
Scanned photograph.
Fig. 8 is the tensile stress strain curve of composite material and fine aluminium block sample in embodiment 2,3,4.
Fig. 9 is composite material Fracture scan photo in embodiment 3.
Figure 10 is the X-ray diffraction spectrum of Composite Sintering state and As-extruded in embodiment 3.
Specific embodiment
Technology path of the invention is as follows:
Three-dimensional carbon nanomaterial is prepared in aluminium powder surface in situ using sodium chloride template, and block is prepared by composite powder
Composite material；Its feature includes following procedure:
(1) sodium chloride template primary reconstruction three-dimensional carbon nanomaterial presoma:
According to quality proportioning it is 10:0.2-0.5 by sodium chloride and DEXTROSE ANHYDROUS, is dissolved in appropriate ionized water, magnetic force
Stirring to solution is clarified, and is placed in culture dish under the conditions of -20 DEG C of freezer compartment of refrigerator and is freezed for 24 hours, the sample after freezing is put
In being lyophilized in freeze drier, grinding obtains composite powder presoma after freeze-drying；
(2) aluminium powder surface ball milling loads self assembled three-dimensional carbon nanomaterial presoma:
The ball aluminum powder that three-dimensional carbon nanomaterial precursor powder made from step (1) and 400 mesh are sieved is subjected to ball milling
Mixing obtains three-dimensional carbon nanomaterial presoma/aluminium composite powder；Ball milling parameter is 200 revs/min of revolving speed, time 6h.
(3) calcining reduction in situ synthesizes three-dimensional carbon nanomaterial/aluminium composite powder:
The powder that step (2) obtains is placed in tube furnace, is passed through argon gas as carrier gas, with 10 DEG C/min, 60min heating
To 600 DEG C；Then high-temperature calcination reduction is carried out using argon gas, hydrogen gas mixture as carrier gas, filtered, washing removes sodium chloride template
Three-dimensional carbon nanomaterial/aluminium composite powder is obtained afterwards, and gas flow is set as hydrogen/argon gas gaseous mixture, ratio 100/
200mL/min, temperature are 600 DEG C, recovery time 2h.
(4) cold pressing-sinter molding of three-dimensional carbon nanomaterial/aluminium composite material block:
Three-dimensional carbon nanomaterial made from step (3)/aluminium composite powder is subjected to 600MPa cold moudling, then in tubular type
It is sintered in furnace, sintering temperature is set in 630 DEG C, and sintering time 1h, protective atmosphere is argon gas, obtains three-dimensional carbon and receives
Rice material/aluminium composite material block；
(5) the extrusion deformation processing of three-dimensional carbon nanomaterial/aluminium composite material block:
Three-dimensional carbon nanomaterial/aluminium composite material block made from step (4) is put into box type heater and is heated, then
Hot extrusion deformation processing is carried out, As-extruded composite material block is obtained.When hot extrusion, box type heater set temperature is 550 DEG C,
Extrusion ratio is 16:1.
The present invention is further illustrated below with reference to embodiment, and the embodiments are used only to illustrate the invention for these, is not intended to limit this
Invention.
Embodiment 1
The smooth uniform particle sizes in aluminium powder surface that the present invention uses, there is the aluminium oxide of one layer of homogeneous by about 40 μm (400 mesh)
The microscopic appearance of film, aluminium powder is as shown in Figure 1；Take the spherical aluminium powder of 20g according to ratio of grinding media to material 10:1 carry out ball milling, revolving speed be 352 turns/
Divide, ball milling 4h, the aluminium powder after ball milling is with a thickness of 1~2 μm, and aluminium powder surface is more smooth, as shown in Figure 2 a.It is 1wt.% with concentration
Surfactant CTAB (cetyl trimethylammonium bromide) to original aluminium powder (Fig. 1) carry out surface activation process after, obtain
Spherical aluminium powder surface it is brighter and cleaner, pattern is as shown in Figure 2 b.
According to quality proportioning it is 20:0.5 by sodium chloride and DEXTROSE ANHYDROUS, is dissolved in 75mL deionized water, magnetic force stirs
It mixes to solution and clarifies；It is obtained after ball aluminum powder and ball milling after above-mentioned CTAB (cetyl trimethylammonium bromide) is activated
Flake aluminum, be added separately in the three-dimensional carbon nanomaterial precursor solution in magnetic agitation, obtain mixing suspension, and
It is placed in culture dish under the conditions of -20 DEG C of freezer compartment of refrigerator and freezes for 24 hours, the sample after freezing is put in freeze drier and is frozen
Dry, grinding obtains composite powder presoma after freeze-drying；It is as shown in Figure 3 that pattern is observed by scanning electron microscope.
Above-mentioned composite powder presoma is placed in tube furnace and is calcined, is passed through argon gas as carrier gas, with 10 DEG C/min,
60min is warming up to 600 DEG C, then carries out high-temperature calcination reduction using argon gas, hydrogen gas mixture as carrier gas, filters, washing removes
Three-dimensional carbon nanomaterial/aluminium composite powder is obtained after sodium chloride template；The pattern of aluminium powder surface coating layer and micro- in composite powder
P-block element p EDAX results are as shown in Figure 4.Composite powder obtains three-dimensional carbon nanometer after being corroded with dilute hydrochloric acid to aluminum substrate
Material, it is as shown in Figure 5 by transmission electron microscope observation pattern.
The composite powder that above-mentioned technique obtains is excessively high due to carbon content, it is difficult to and it is body formed to carry out subsequent composite block,
But the above-mentioned process conditions for preparing three-dimensional carbon nanomaterial in aluminium powder surface in situ still have to a certain degree the invention achievement
Directive significance.Therefore to 1 adjusting parameter of embodiment and improve, form following examples 2,3 and blank control group embodiment
4。
Embodiment 2
According to quality proportioning it is 10:0.225 by sodium chloride and DEXTROSE ANHYDROUS, is dissolved in 50mL deionized water, magnetic force
Stirring to solution is clarified, and is placed in culture dish under the conditions of -20 DEG C of freezer compartment of refrigerator and is freezed for 24 hours, the sample after freezing is put
In being lyophilized in freeze drier, grinding obtains composite powder presoma after freeze-drying；The spherical shape that precursor powder and 400 mesh are sieved
Aluminium powder carries out ball milling according to the mass ratio of 1:10, and ball milling parameter is 200 revs/min of revolving speed, time 6h；Pass through scanning electron microscope
Pattern is as shown in Figure 6 after observing ball milling.Three-dimensional carbon nanomaterial presoma/aluminium composite powder is obtained after ball milling, is passed through argon gas work
For carrier gas, 600 DEG C are warming up to 10 DEG C/min, 60min, then carries out high-temperature calcination using argon gas, hydrogen gas mixture as carrier gas
Reduction filters, washing obtains three-dimensional carbon nanomaterial/aluminium composite powder after removing sodium chloride template；Pass through high power scanning electron
Microscope is observed, and pattern is as shown in Figure 7.Composite powder is subjected to 600MPa cold moudling, 630 DEG C of argon gas protections are lower to burn
Knot in batch-type furnace after 550 DEG C of heating, carries out hot extrusion according to the extrusion ratio of 16:1, obtains composite material block；Its stretching is answered
Stress-strain curve is as shown in Fig. 8 curve 1.
Embodiment 3
According to quality proportioning it is 10:0.225 by sodium chloride and DEXTROSE ANHYDROUS, is dissolved in 50mL deionized water, magnetic force
Stirring to solution is clarified, and is placed in culture dish under the conditions of -20 DEG C of freezer compartment of refrigerator and is freezed for 24 hours, the sample after freezing is put
In being lyophilized in freeze drier, grinding obtains composite powder presoma after freeze-drying；The spherical shape that precursor powder and 400 mesh are sieved
Aluminium powder carries out ball milling according to the mass ratio of 2:10, and ball milling parameter is 200 revs/min of revolving speed, time 6h, obtains three-dimensional carbon after ball milling and receives
Rice material precursor/aluminium composite powder；Argon gas is then passed to as carrier gas, is warming up to 600 DEG C with 10 DEG C/min, 60min, then
High-temperature calcination reduction is carried out using argon gas, hydrogen gas mixture as carrier gas, is filtered, washing obtains three-dimensional carbon after removing sodium chloride template
Nano material/aluminium composite powder；Composite powder is subjected to 600MPa cold moudling, the lower sintering of 630 DEG C of argon gas protections, in batch-type furnace
In 550 DEG C heating after, according to 16:1 extrusion ratio carry out hot extrusion, obtain composite material block；Its tensile stress strain curve
As shown in Fig. 8 curve 2.Composite material fracture is analyzed with scanning electron microscope, pattern is as shown in Figure 9.Comparative composite is burnt
Tie the X-ray diffraction spectrum of state and As-extruded, as shown in Figure 10, composite material after thermal deformation there are the preferred orientation of crystal grain,
It is deformed texture.
Embodiment 4 (blank control test)
The ball aluminum powder of 400 mesh sieving is subjected to ball milling, ball milling parameter is 200 revs/min of revolving speed, time 6h, after ball milling
Aluminium powder carry out 600MPa cold moudling, the lower sintering of 630 DEG C of argon gas protection, in batch-type furnace after 550 DEG C of heating, according to 16:1's
Extrusion ratio carries out hot extrusion, obtains composite material block；Its tensile stress strain curve is as shown in Fig. 8 curve 0.
Claims (3)
1. a kind of method for preparing three-dimensional carbon nanomaterial in aluminium powder surface in situ using sodium chloride template, including following mistake
Journey:
(1) sodium chloride template primary reconstruction three-dimensional carbon nanomaterial presoma:
According to quality proportioning it is 10:0.2-0.5 by sodium chloride and DEXTROSE ANHYDROUS, is dissolved in appropriate ionized water, after freezing again
Freeze-drying, grinding obtains three-dimensional carbon nanomaterial precursor powder after freeze-drying；
(2) aluminium powder surface ball milling loads self assembled three-dimensional carbon nanomaterial presoma:
The ball aluminum powder that three-dimensional carbon nanomaterial precursor powder made from step (1) and 400 mesh are sieved is subjected to ball milling mixing,
Obtain three-dimensional carbon nanomaterial presoma/aluminium composite powder.
(3) calcining reduction in situ synthesizes three-dimensional carbon nanomaterial/aluminium composite powder:
Three-dimensional carbon nanomaterial presoma/aluminium composite powder that step (2) is obtained is placed in tube furnace, is passed through argon gas as load
Gas is warming up to 600 DEG C with 10 DEG C/min, 60min；Then high-temperature calcination reduction is carried out using argon gas, hydrogen gas mixture as carrier gas,
It filters, washing obtains three-dimensional carbon nanomaterial/aluminium composite powder after removing sodium chloride template；
(4) cold pressing-sinter molding of three-dimensional carbon nanomaterial/aluminium composite material block:
Three-dimensional carbon nanomaterial made from step (3)/aluminium composite powder is subjected to cold moudling, then sintering processes, obtain three
Tie up carbon nanomaterial/aluminium composite material block.
(5) the extrusion deformation processing of three-dimensional carbon nanomaterial/aluminium composite material block:
Three-dimensional carbon nanomaterial/aluminium composite material block made from step (4) is put into box type heater and is heated, is then carried out
Hot extrusion deformation processing, obtains As-extruded composite material block.
2. the method according to claim 1, wherein the process conditions of step (4) are as follows: carry out 600MPa and be cold-pressed into
Then type is sintered in tube furnace, sintering temperature is set in 630 DEG C, and sintering time 1h, protective atmosphere is argon
Gas.
3. the method according to claim 1, wherein box type heater set temperature is when step (5) hot extrusion
550 DEG C, extrusion ratio 16:1.
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| CN110921651A (en) * | 2019-11-18 | 2020-03-27 | 天津大学 | Preparation of three-dimensional carbon-based composite material by metal-assisted salt template method |
| CN113979439A (en) * | 2021-11-30 | 2022-01-28 | 陕西科技大学 | Si5C3Micro-nano material and preparation method thereof |
| CN114042928A (en) * | 2021-11-25 | 2022-02-15 | 西北有色金属研究院 | Preparation method of ruthenium-cobalt-nickel-iron-copper high-entropy alloy nanoparticles |
| CN114888298A (en) * | 2022-05-20 | 2022-08-12 | 巢湖学院 | Two-dimensional high-entropy alloy and preparation method and application thereof |
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