CN104745856B - Preparation method of wear-resisting carbon nano paper-metal composite material - Google Patents
Preparation method of wear-resisting carbon nano paper-metal composite material Download PDFInfo
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- CN104745856B CN104745856B CN201510200480.0A CN201510200480A CN104745856B CN 104745856 B CN104745856 B CN 104745856B CN 201510200480 A CN201510200480 A CN 201510200480A CN 104745856 B CN104745856 B CN 104745856B
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Abstract
The invention discloses a preparation method of a wear-resisting carbon nano paper-metal composite material. A method of powder metallurgy is adopted, and metal powder is placed on a CNP (Carbon Nano Paper) to prepare the wear-resisting carbon nano paper-metal composite material. The preparation method comprises the following steps of (1) pressing: paving the carbon nano paper on a mold, uniformly paving a layer of metal powder on any one face or two faces, and cold press molding under 200MPa-1000MPa; (2) sintering: intermittently heating and sintering the pressed materials under the condition of inert gases, firstly rising the temperature to be 300 DEG C-400 DEG C, preserving heat, then rising the temperature to be 500 DEG C-1200 DEG C, preserving heat, and naturally cooling; (3) re-pressing: re-pressing the sintered materials under 200MPa-1000MPa; (4) re-sintering: re-sintering the re-pressed materials at the temperature of 500-700 DEG C under the condition of inert gases, preserving heat and sintering for 4h, and preparing to obtain the wear-resisting carbon nano paper-metal composite material which cannot be clustered, and is light in mass, low in cost and favorable in performance.
Description
Technical field
Technical field is utilized the invention belongs to high-abrasive material, and in particular to a kind of wear-resisting carbon nanometer paper-metallic composite
Preparation method.
Background technology
With developing rapidly for modern science and technology, particularly space flight and aviation, vapour tool (internal combustion engine connecting rod, brake disc,
Bearing) etc. some brakes develop rapidly, people to wear-resisting, low-expansion coefficient electric-conductivity heat-conductivity high material requirement increasingly
It is high.Chinese patent CN102555351A is prepared for a kind of wear-resisting bimetal composite material high using liquid, liquid composite casting method, but
Metal and its alloy friction are big, and metal and its alloy are prepared and require height.To reduce the coefficient of friction of metal and alloy,
Chinese patent CN101898239A describes a kind of preparation method of ceramic particle reinforcement of composite wear-resistant material, reinforcement be by
WC ceramic particles are sintered in vacuum high-temperature environment and formed, but the process is present that tungsten carbide is expensive, ceramic particle only
It is adapted to the defects such as tungsten carbide；For this foreign patent US3933482A employs some cheap and content relative abundance doping
Body (chromium, boron, titanium) is doped to alloy-based prepares the composite with anti-wear performance；Wang Dehong etc. uses mechanical alloying
Technique prepares Cu-Cr alloy powders, and adds a certain amount of SiC reinforcing materials wherein, but its preparation technology complexity is not suitable for
Batch production.Someone uses powder metallurgy by graphite and copper synthetic composite material to reduce coefficient of friction, coefficient of expansion etc. afterwards,
Although this can reduce metal friction coefficient can make production lot, mechanical property of graphite etc. compared with current popular its again
His carbon material is not high, and the abrasiveness of its composite is nor very well.
In order to improve the physical property such as mechanics of reinforcing material, and then adopted as reinforcement using CNT (CNTs)
CNTs- metal-base composites is prepared with methods such as powder metallurgy, but with the increase of CNTs contents, CNTs can occur cluster and show
As, and cause the composite property to reduce, and the quality of CNTs- metal-base composites is relatively heavier.Exist to improve CNTs
Agglomeration traits in metal, prepare CNTs and increase using CNTs scattered in advance with metal salt solution combination drying sintering and reducing
Strong metal composite；Or using electrochemical co-deposition method prepared conductance, thermal conductivity, mechanical strength than simple metal (Cu,
Ni etc.) the high and coefficient of expansion CNTs enhancing metal-base composites smaller than metal.Although both approaches solve CNTs's
Cluster problem, can also improve the performances such as mechanics, calorifics, the electricity of metallic composite, but, because metallic composite is in people
Production and living in occupy an leading position and need to commercially produce, and this two methods is not suitable for a large amount of productions, therefore, below we
It is introduced into new carbon nanometer paper and CNTs reunions, unsuitable commodity production, physical property is solved with the technology of prior powder metallurgy
Bad the problems such as.
, used as a kind of new material, dispersiveness is superior, also possesses excellent mechanics, electric property for carbon nanometer paper (CNP), and
Can be used as a kind of substrate.CNP is the nanoporous knot being prepared into by carbon nanomaterial (such as CNT CNTs, carbon fiber CNFs)
The paper-like material of structure, light weight, with excellent conductive, thermal conduction characteristic, and into nanometer loose and porous structure, its carbon nanometer paper
Appearance and SEM figures are as shown in Figure 1 and Figure 2.CNTs is respectively by a richness by one or more concentric graphitic cylinders and two ends
Strangle alkene cap composition；Its mechanics, electricity, thermal property are strong.
The content of the invention
It is an object of the invention to provide a kind of wear-resisting carbon nanometer paper-gold that reunion, light weight, low manufacture cost will not occur
Belong to the preparation method of composite.
Technical scheme is as follows：
(1) suppress：Alcohol washes mould is used before compacting, to ensure mould not contaminated samples, is allowed to dry and is used just now.Will
Carbon nanometer paper and copper powder are put into the mould being cleaned and dried, and any one or both sides of carbon nanometer paper uniformly spread layer of metal
Powder, its thickness is 4-10mm, and compacting 2-20min carries out cold moudling under 200MPa-1000MPa；
CNP- metal sheetings of the invention, are directly to spread layer of metal powder in a mold, and tile one layer of CNP lining thereon
Bottom, substrate upper berth metal powder (or directly spreading layer of metal powder in a mold, tile one layer of CNP substrate thereon), metal powder is
Any one metal powder of Cu, Cr, Al or the two or more metal powders mixed with certain proportion, its average grain diameter is 50nm-5 μm,
The thickness of CNP- metal sheetings is 4mm-11mm；Be pressed using the tablet press machine of powder metallurgy, static pressure for a period of time, energy
Make the sample of shaping firm a lot.
Preferably, before compacting, its skewness in a mold may be caused in mould because metal powder is put in, to prevent
CNP is put on metal powder and run-off the straight, metal powder can be pressed into piece with small pressure before CNP is put, then CNP is placed in into it
On, and the metal powder on CNP also can be operated so.
(2) sinter：The material that will be suppressed uses discontinuous heat-agglomerating in an inert atmosphere, first allows temperature to rise to
300 DEG C of -400 DEG C of insulation 1-2h, then temperature is raised to 500 DEG C of -1200 DEG C of insulation 1-3h, then be naturally cooling to 20 DEG C with
Under；
CNP- metal sheetings of the invention sintering, is sintered by tubular annealing stove, at the same by the use of inert gas as
Surrounding environment, it is ensured that CNP and metal are not oxidized；Sintering temperature is heated using discontinuous, first allows temperature to rise to 300 DEG C -400
DEG C, allowing one temperature for a period of time, preferably 2h, to decompose the polymer in CNP or to exclude air therein, makes
Its composite is finer and close；Temperature is raised to 500 DEG C -1200 DEG C by insulation again after a period of time, makes metal-powder and carbon nanometer paper
Generation Plastic Flow, to make the two more preferable fusion, allows its insulation a period of time, preferably 1h, then carries out Temperature fall.
(3) multiple pressure：The material for sintering presses 5-10min again under 200MPa-1000MPa；
Multiple pressure after CNP- metal sheetings sintering of the invention, generally uses 200MPa-1000MPa and is suppressed, and is to make
The space after the polymer in CNP is decomposed or excludes air therein is sintered in 500 DEG C -1200 DEG C to try one's best reduction, allows sample
More even compact.
(4) resintering knot：The sample for pressing again of the invention is sintered again, and is carried out under atmosphere of inert gases, sintering temperature
Degree is sintered again without higher than what is sintered before using 500-700 DEG C, and heat preservation sintering 2-4h, it is ensured that sample after multiple pressure
Compactness, be made the wear-resisting carbon nanometer paper-metallic composite.
The carbon fiber of table 1 synthesizes carbon nanometer paper performance parameter
The method that the present invention uses powder metallurgy, metal-powder is placed on CNP can prepare wear-resisting carbon nanometer paper-gold
Category composite, the composite do not reunite, light weight, low cost and anti-wear performance is good.
Brief description of the drawings
The invention will be further described below in conjunction with the accompanying drawings：
Fig. 1 is that the SEM of the carbon nanometer paper synthesized with carbon fiber schemes；
Fig. 2 is that the SEM of the carbon nanometer paper synthesized with CNT schemes；
Fig. 3 is the process flow diagram one of preparation method of the present invention；
Fig. 4 is the process flow diagram two of preparation method of the present invention；
Wherein, in Fig. 3-4, a. metallic particles；B. carbon nanometer paper；C. there is a small amount of metallic particles in CNP after suppressing；D. metal
The sheet metal of particle synthesis；E. there is further amounts of metallic particles in CNP after sintering.
Specific embodiment
Below in conjunction with embodiment and accompanying drawing in the present invention, the technical scheme in the embodiment of the present invention is carried out it is clear,
It is fully described by, it is clear that described embodiment is only a part of embodiment of the invention, rather than whole embodiments.Base
Embodiment in the present invention, those of ordinary skill in the art obtained under the premise of creative work is not made it is all its
His embodiment, belongs to the scope of protection of the invention.
Embodiment 1
Selection average grain diameter is 1.172 μm of Cu powder, (is purchased from Kunming to receive too with the carbon nanometer paper that carbon nano-fiber is prepared into
Limited energy company) it is substrate, carbon nanometer paper is cut into the sequin of diameter 12mm, and it is dried standby with alcohol washes,
Using the mould with the excessively dried diameter 12mm of alcohol washes, Cu powder, carbon nanometer paper (CNP), Cu are put into mould respectively
Powder, the small column of 5.635mm high is compressed into using 610.8MPa, and it keeps static pressure 2min to have suppressed relief；Static pressure is good
Cu-CNP-Cu be put into tubular annealing stove and in N2Under the conditions of fire, temperature is first risen to 350 DEG C from 20 DEG C with 1.5h, 350
DEG C when be incubated 2h, then rise to 750 DEG C with 1h, be incubated 1h again at this moment, relief its Temperature fall be cooled to room temperature；Compacting is burnt
The sample tied is put into mould for tabletting press and carries out multiple pressure 5min, the multiple pressure pressure 610.8MPa of sample；Then and in N2Under atmosphere from
20 DEG C rise to 600 DEG C, and are incubated 4h.Compared with fine copper, wearability improves 5.08% for it.
Embodiment 2
Selection average grain diameter is 1.172 μm of Cu powder, and the carbon nanometer paper being prepared into CNT (is purchased from Kunming and received and too can
Source Co., Ltd) it is substrate, carbon nanometer paper is cut into the sequin of diameter 12mm, and it is dried standby with alcohol washes, adopt
With the mould with the excessively dried diameter 12mm of alcohol washes, Cu powder, carbon nanometer paper (CNP), Cu powder are put into mould respectively
Deng, 4 layers of paper have been recycled to, Cu- multi-layer Cs NP is suppressed the small column of 4.041mm high using 610.8MPa, it is protected to have suppressed relief
Hold static pressure 2min；The good Cu- multi-layer Cs NP of static pressure is put into tubular annealing stove and in N2Under the conditions of fire, first with 1.5h by temperature
Rise to 350 DEG C from 20 DEG C, 2h be incubated at 350 DEG C, then 800 DEG C are risen to 2h, be incubated 2h again at this moment, relief its drop naturally
Temperature is cooled to room temperature；The sample that compacting sintering is crossed is put into mould for tabletting press carries out multiple pressure 5min, the multiple pressure pressure of sample
610.8MPa；Then and in N2600 DEG C are risen to from 20 DEG C under atmosphere, and is incubated 4h.Compared with fine copper, wearability improves for it
20.14%.
Embodiment 3
The equal particle diameter of Cu powder peaces for selecting average grain diameter to be 1.172 μm is 1.5 μm of Cr powder, and its Cr powder accounts for gross mass
8wt.%, the carbon nanometer paper being prepared into carbon nano-fiber (being purchased from Kunming Na Tai limited energies company) as substrate, by carbon nanometer
Paper is cut into the sequin of diameter 12mm, and dried standby with alcohol washes, using with the excessively dried diameter of alcohol washes
The mould of 12mm, is put into Cu and Cr mixed powders, carbon nanometer paper (CNP), Cu and Cr mixed powders, using 750MPa in mould respectively
Cu+Cr/CNP/Cu+Cr is suppressed the small column of 4.870mm high, it keeps static pressure 2min to have suppressed relief；By the good Cu+ of static pressure
Cr/CNP/Cu+Cr is put into tubular annealing stove and in N2Under the conditions of fire, temperature is first risen to 350 DEG C from 20 DEG C with 1.5h,
2h is incubated at 350 DEG C, then 750 DEG C is risen to 1h, be incubated 1h again at this moment, relief its Temperature fall be cooled to room temperature；Will pressure
The sintered sample of system is put into mould for tabletting press and carries out multiple pressure 5min, the multiple pressure pressure 750MPa of sample；Then and in N2Under atmosphere
600 DEG C are risen to from 20 DEG C, and is incubated 4h.Compared with fine copper, wearability improves 55.56% for it, its compared with Cu+Cr samples,
Wearability improves 12.22%.
Embodiment 4
Selection average grain diameter is the Cu powder of 50nm, and the carbon nanometer paper being prepared into carbon nano-fiber (is purchased from Kunming and received and too can
Source Co., Ltd) it is substrate, carbon nanometer paper is cut into the sequin of diameter 12mm, and it is dried standby with alcohol washes, adopt
With the mould with the excessively dried diameter 12mm of alcohol washes, be put into mould respectively nano Cu powder, carbon nanometer paper (CNP),
Nano Cu powder, Cu-CNP-Cu is suppressed the small column of 10.20mm high using 750MPa, and it keeps static pressure 2min to have suppressed relief；
The good Cu-CNP-Cu of static pressure is put into tubular annealing stove and in N2Under the conditions of fire, temperature is first risen to 350 from 20 DEG C with 1.5h
DEG C, 2h is incubated at 350 DEG C, then 900 DEG C are risen to 1h, be incubated 1h again at this moment, relief its Temperature fall be cooled to room temperature；
The sample that compacting sintering is crossed is put into mould for tabletting press carries out multiple pressure 7min, the multiple pressure pressure 750MPa of sample；Then and in N2Atmosphere
600 DEG C are risen to from 20 DEG C under enclosing, and is incubated 4h.Compared with fine copper, wearability improves 11.78% for it.
Embodiment 5
Selection average grain diameter is the Cu powder of 50nm, and the carbon nanometer paper being prepared into carbon nano-fiber (is purchased from Kunming and received and too can
Source Co., Ltd) it is substrate, carbon nanometer paper is cut into the sequin of diameter 12mm, and it is dried standby with alcohol washes, adopt
With the mould with the excessively dried diameter 12mm of alcohol washes, nano Cu powder, carbon nanometer paper (CNP) are put into mould respectively,
Cu-CNP is pressed into the small column of 10.25mm high using 650MPa, it keeps static pressure 2min to have suppressed relief；Static pressure is good
Cu-CNP is put into tubular annealing stove and in N2Under the conditions of fire, temperature is first risen to 350 DEG C from 20 DEG C with 1.5h, at 350 DEG C
Insulation 2h, then rises to 850 DEG C with 1h, is incubated 1h again at this moment, relief its Temperature fall be cooled to room temperature；By compacting sintering mistake
Sample be put into mould for tabletting press and carry out multiple pressure 5min, the multiple pressure pressure 650MPa of sample；Then and in N2Risen from 20 DEG C under atmosphere
To 650 DEG C, and it is incubated 4h.Compared with fine copper, wearability improves 6.67% for it.
Embodiment 6
Selection average grain diameter is 1.4 μm of Al powder, and the carbon nanometer paper being prepared into carbon nano-fiber (is purchased from Kunming and received and too can
Source Co., Ltd) it is substrate, carbon nanometer paper is cut into the sequin of diameter 12mm, and it is dried standby with alcohol washes, adopt
With the mould with the excessively dried diameter 12mm of alcohol washes, one layer of Al powder is uniformly spread in carbon nanometer paper (CNP) levels respectively,
Al-CNP-Al is suppressed using 750MPa, it keeps static pressure 2min to have suppressed relief；The good Al-CNP-Al of static pressure is put
Enter tubular annealing stove and in N2Under the conditions of fire, temperature is first risen to 350 DEG C from 20 DEG C with 1.5h, be incubated 2h at 350 DEG C, then
Rise to 600 DEG C with 1h, be incubated 1h again at this moment, relief its Temperature fall be cooled to room temperature；The sample that compacting sintering is crossed is put
Entering mould for tabletting press carries out multiple pressure 6min, the multiple pressure pressure 750MPa of sample；Then and in N2500 DEG C are risen to from 20 DEG C under atmosphere,
And it is incubated 4h.Compared with fine aluminium, wearability improves 15.79% for it.
It can be that professional and technical personnel in the field realize or use that above-mentioned implementation method is intended to illustrate the present invention, to above-mentioned
Implementation method is modified and will be apparent for those skilled in the art, therefore the present invention is included but is not limited to
Above-mentioned implementation method, it is any to meet the claims or specification description, meet with principles disclosed herein and novelty,
The method of inventive features, technique, product, each fall within protection scope of the present invention.
Claims (6)
1. a kind of preparation method of wear-resisting carbon nanometer paper-metallic composite, it is characterised in that comprise the following steps：
(1) suppress：Carbon nanometer paper is spread in mould, and one layer of 4-6mm thickness is uniformly spread in any one or both sides of carbon nanometer paper
Metal powder, and under 200MPa-1000MPa suppress 2-20min carry out cold moudling；
(2) sinter：The material that will be suppressed uses discontinuous heat-agglomerating in an inert atmosphere, first allows temperature to rise to 300
DEG C of -400 DEG C insulation 1-2h, then temperature is raised to 500 DEG C of -1200 DEG C of insulation 1-3h, then carry out being naturally cooling to less than 20 DEG C；
(3) multiple pressure：The material for sintering presses 5-10min again under 200MPa-1000MPa；
(4) resintering knot：Material after multiple pressure is sintered for 500-700 DEG C again in an inert atmosphere, and heat preservation sintering 2-
4h, is made the wear-resisting carbon nanometer paper-metallic composite；
The metal powder is any one metal powder of Cu, Cr, Al or the two or more metal powders mixed with certain proportion.
2. the preparation method of wear-resisting carbon nanometer paper-metallic composite according to claim 1, it is characterised in that described
The average grain diameter of metal powder is 50nm-5 μm.
3. the preparation method of wear-resisting carbon nanometer paper-metallic composite according to claim 1, it is characterised in that put carbon
Metal powder is pressed into piece before nanometer paper, then carbon nanometer paper is placed on it.
4. the preparation method of wear-resisting carbon nanometer paper-metallic composite according to claim 1, it is characterised in that described
Suppress, press through journey again, be pressed using the tablet press machine of powder metallurgy.
5. the preparation method of wear-resisting carbon nanometer paper-metallic composite according to claim 1, it is characterised in that described
Sinter, be sintered in being carried out in atmosphere tube type annealing furnace again.
6. wear-resisting carbon nanometer paper-metallic composite that the method as described in claim 1-5 any one is prepared.
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| CN1827827A (en) * | 2006-03-24 | 2006-09-06 | 哈尔滨工业大学 | Carbon nanotube enhanced aluminium-based composite material and air hot pressing preparation method thereof |
| CN101956149B (en) * | 2010-10-08 | 2012-08-29 | 昆明理工大学 | Process for preparing carbon nano-tube-enhanced aluminum-based composite material |
| CN102180460A (en) * | 2011-03-17 | 2011-09-14 | 东华大学 | Preparation method of highly-oriented carbon nanotube paper |
| JP5717860B2 (en) * | 2011-09-14 | 2015-05-13 | 株式会社フジクラ | Structure for forming carbon nanofiber, carbon nanofiber structure, manufacturing method thereof, and carbon nanofiber electrode |
| CN102864324A (en) * | 2012-09-06 | 2013-01-09 | 东北大学 | Preparation method for carbon nanomaterial enhanced aluminum base composite material |
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