CN107138527B - The preparation method of CNTs/Ti biomimetic micro-nano laminated composite materials - Google Patents
The preparation method of CNTs/Ti biomimetic micro-nano laminated composite materials Download PDFInfo
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- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
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- B21B1/00—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations
- B21B1/38—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations for rolling sheets of limited length, e.g. folded sheets, superimposed sheets, pack rolling
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Abstract
The invention discloses the preparation methods of CNTs/Ti biomimetic micro-nano laminated composite materials, belong to titanium matrix composite technical field.The technical barriers such as the invention solves CNTs to be difficult to be uniformly distributed in Titanium base, CNTs and Titanium base interfacial reaction and titanium matrix composite intensity-plasticity (toughness) are inverted.The method of the present invention：Titanium foil is pre-processed with HF solution, the carbon nanotube of acidification is configured to CNTs suspensions, CNTs layers of nanoscale is deposited on titanium foil surface obtain CNTs/Ti monolayer materials by electrophoretic deposition, then stacking is laminated in several CNTs/Ti monolayer materials, most upper and lower layer is pure Ti, recycles discharge plasma sintering (SPS) that zerolling is combined to prepare CNTs/Ti biomimetic micro-nano laminated composite materials.Products C NTs of the present invention is uniformly dispersed, and titanium purer than matrix multilayer is compared, and intensity improves 20%~50%, and elongation at break significantly reduces.
Description
Technical field
The invention belongs to titanium matrix composite technical fields；More particularly to CNTs/Ti biomimetic micro-nano laminated composite materials
Preparation method.
Background technology
Titanium matrix composite has many advantages, such as high specific strength, high ratio modulus and excellent high-temperature behavior, flies in aerospace
There is huge application potential on row device and high-performance weaponry.All the time, the tradition based on metal-base composites is ground
Study carefully thinking, most of researcher always pursues reinforced phase and is uniformly distributed in titanium alloy substrate, and is dedicated to increasing by improving
Strong phase content improves the mechanical property of titanium matrix composite.Although the strength and stiffness of titanium matrix composite significantly improve,
It is that plasticity and toughness are remarkably decreased, i.e., inversion relationship is presented in intensity-toughness (plasticity) of traditional titanium matrix composite.Currently, titanium
Based composites significantly limit its extensive use in industrial circle due to plasticity and toughness deficiency.
CNTs often includes by powder metallurgic method, stirring casting method or vapour deposition process etc. with complex method with titanium.Wherein
The most ripe is powder metallurgy process, is first uniformly to mix CNTs with titanium particle, it is quiet then to carry out hot pressing or heat etc. again
CNTs/Ti composite materials are prepared in pressure, progress hot extrusion or hot rolling etc. later.However what the method obtained is CNTs in titanium-based
Equally distributed CNTs/Ti composite materials in body.And at present the CNTs/Ti composite materials prepared of technique be primarily present it is following
3 common problems：(1) CNTs is difficult to be dispersed substantially in Titanium base, and the agglomeration of CNTs does not solve at all, this is
CNTs/Ti composite materials can reach far away one of the main reason for its ideal performance.(2) the unavoidable height of traditional combination process
Warm high-pressure sinter or high temperature deformation process, in the process CNTs easily with Titanium base occur interfacial chemical reaction and generate brittleness
TiC phases, to destroy the perfect structure of CNTs, and TiC easily grows up.Although large-sized TiC particles also have one
Fixed invigoration effect, but it strengthens effect well below CNTs, and this, which is CNTs/Ti composite materials, can reach far away its ideal performance
Another one of the main reasons.(3) CNTs/Ti composite materials are while keeping high intensity, how to improve its plasticity with it is tough
Property is still a huge challenge.
In conclusion the CNTs/Ti of exploitation high-strength tenacity (intensity improves keeps enough plasticity and toughness simultaneously) is compound
The novel processing step of material is imperative.
Invention content
The preparation method of presently disclosed CNTs/Ti biomimetic micro-nanos lamination is rarely reported.
The invention solves CNTs to be difficult to equally distributed technical barrier and existing method in Titanium base to carry
The technical issues of enough plasticity and toughness is kept while high intensity；And it is compound to provide CNTs/Ti biomimetic micro-nano laminations
The preparation method of material.
In order to solve the above technical problems, the preparation method of CNTs/Ti biomimetic micro-nanos laminated composite materials is in the present invention
It carries out in the steps below：
Step 1: being pre-processed to titanium foil surface with HF solution, with the mixed acid of the concentrated sulfuric acid and concentrated nitric acid to carbon nanometer
Pipe carries out acidification；
Step 2: preparing mixed liquor with absolute ethyl alcohol and acetone, then Al (NO are added into mixed liquor3)3It is acidified with step 1
Carbon nanotube that treated, ultrasonic disperse obtain CNTs suspension；
Step 3: using the titanium foil of step 1 processing as cathode, using stainless steel substrates as anode, the CNTs of step 2 acquisition
Suspension is electrolyte, applies direct current between electrode, obtains nanoscale CNTs sedimentaries on titanium foil surface, that is, obtains CNTs/Ti
Monolayer material；
Step 4: stacking is laminated in CNTs/Ti monolayer materials, lowest level and top layer are pure Ti foils, are then discharged
Plasma agglomeration (SPS)；
Step 5: carrying out zerolling to the material that step 4 obtains, that is, it is multiple to prepare CNTs/Ti biomimetic micro-nano laminations
Condensation material.
It further limits, the titanium foil thickness described in step 1 is 10-100 μm.
It further limits, the volumetric concentration of HF solution described in step 1 is 10%~20%.
It further limits, carbon nanotube, which carries out acidification, in step 1 is completed by following step：Use volume ratio
For (1~3):Mixed acid pair 0.1~0.6g carbon nanotubes of 1 concentrated sulfuric acid and concentrated nitric acid carry out acidification 2-8h, then dilute
It releases to neutrality, then carries out centrifugal treating.
It further limits, the volume ratio of absolute ethyl alcohol and acetone is 1 in mixed liquor in step 2:(1~5), every liter of mixing
Al (the NO of 0.04~0.2g are added in liquid3)3With the CNTs of 0.5~3.0g, the ultrasonic disperse time is 2~10h.
It further limits, the two poles of the earth distance between plates is 20~80mm in step 3, and electrophoretic deposition voltage is 10~50V, deposition
Time be 5~80s, obtain CNTs/Ti monolayer materials in CNTs deposit thickness general controls in 50~200nm.
It further limits, discharge plasma sintering temperature is 300~700 DEG C in step 4, and pressure is 40~100MPa, is protected
The warm time is 5~30min.
It further limits, rolling temperature is 300-500 DEG C in step 5, and annealing time is 5-30min, rolling speed between passage
Degree is 0.1~2m/s, and first pass deformation 40%~70%, pass deformation is 5%~15%, and rolling total deformation is 70%
~96%.
Layered distribution is presented in CNTs in Titanium base in product of the present invention, and Titanium base thickness in monolayer is 200nm-10 μm.
Natural seashell by the calcium carbonate layer of submicron order with fine micro-nano lamination structure with nano level due to (being had
Machine matter layer is alternately arranged composition), it is 3000 times of pure calcium carbonate or more to make its tensile strength, toughness be 30 times of pure calcium carbonate with
On, ideal reinforcing and the toughening double action of micro-nano lamination structure are fully demonstrated, this is derived from its perfect structure effect.
The present invention makes full use of it using carbon nano-sized carbon (CNTs) as layer building CNTs/Ti biomimetic micro-nano laminated composite materials are strengthened
Excellent structure effect, to solve intensity-toughness (plasticity) inversion problem of titanium matrix composite.The present invention uses electrophoretic deposition
Carbon nanotube is evenly spread to titanium foil surface by method, then combines zerolling by low temperature fast spark plasma sintering (SPS)
Technology prepares carbon nanotube and good carbon nanotube enhancing titanium-based (CNTs/Ti) biomimetic micro-nano of Titanium base interface cohesion is folded
Layer composite material
The present invention dexterously solves carbon nanotube using electrophoretic deposition combination zerolling technology and disperses in Titanium base
The problem of lack of homogeneity.In electrophoresis solution, due to electrostatic interaction, negatively charged carbon nanotube is mutually exclusive, and therefore, carbon is received
Mitron has good dispersion in electrophoresis solution；Under DC electric field effect, positively charged carbon nanotube can be with uniform deposition
CNTs/Ti monolayer materials are obtained to titanium foil surface.Carbon nanotube can be further increased in titanium by then carrying out zerolling deformation
Evenly dispersed degree in matrix.In addition, electrophoretic deposition technique and rolling technique have equipment simple, easily operated, can make
The features such as standby technical grade large size plate.
The present invention using low temperature fast spark plasma sintering process combination zerolling technology can solve carbon nanotube and
Key issues of interface vigorous reaction of Titanium base.Plasma discharging Fast Sintering method is that one kind developed in recent years is novel
Fast Sintering technology, it utilize pulse high current, make the material being compacted generate micro discharge to inspire plasma, so
Electrified regulation is to sintering temperature again afterwards, and therefore, the temperature of discharge plasma sintering is low, and sintering time is short, avoids traditional vacuum hot
Carbon nanotube caused by temperature and long-time heat preservation and the serious interfacial reaction of Titanium base are lifted at a slow speed when pressure sintering.Then carry out
The rolling deformation of aximal deformation value improves material interface layer and combines, while controlled rolling deformation temperature, can be to avoid carbon nanotube
With Titanium base interfacial reaction.
The present invention builds nano reinforcement layer by introducing carbon nanotube, while by increasing rolling reduction, by CNTs/Ti
The constituent element thickness of composite material is reduced to micro-or nano size, finally prepares the CNTs/ that tissue is controllable, comprehensive mechanical property is excellent
Ti biomimetic micro-nano laminated composite materials.
The present invention regulates and controls by adjusting CNTs deposit thickness, raw material titanium foil thickness and rolling reduction simultaneously
The micro-nano layer structure parameter of CNTs/Ti composite materials, realize CNTs/Ti biomimetic micro-nano laminated composite materials intensity with
Plasticity (toughness) best match.The intensity titanium purer than matrix multilayer of CNTs/Ti biomimetic micro-nano laminated composite materials improves 20%
~50%, while its uniform plastic deformation ability significantly improves, elongation at break significantly reduces.The bionical micro-nanos of CNTs/Ti
The mechanical property of rice laminated composite materials achieves the desired results.
The present invention is applied to aerospace, high-performing car field.
Description of the drawings
Fig. 1 is assembling schematic diagram in discharge plasma sintering stove, 1 in Fig. 1 --- CNTs/Ti monolayer materials, 2 --- and pure Ti
Foil；
Fig. 2 is CNTs/Ti monolayer material microstructure SEM photographs prepared by electrophoretic deposition；
Fig. 3 is the Raman test curve of discharge plasma sintering (SPS) and conventional thermocompression sintering (HP)；
Fig. 4 is the microstructure SEM photograph of discharge plasma sintering (SPS) CNTs/Ti laminar composites afterwards；
Fig. 5 is CNTs/Ti biomimetic micro-nano laminated composite materials microstructure TEM photos after rolling deformation 90%.
Specific implementation mode
Specific implementation mode one：The preparation method of CNTs/Ti biomimetic micro-nanos laminated composite materials is in present embodiment
It carries out in the steps below：
Step 1: pre-treatment of raw material：It is 50 μm of business TA1 pure titanium foils to take thickness, uses volumetric concentration for 15%HF
Solution carries out pretreatment 10s to titanium foil surface and removes oxide film dissolving etc.；Carbon nanotube decentralized processing：Use volume ratio for 2 first:1
The mixed acid prepared of the concentrated sulfuric acid and concentrated nitric acid acidification 5h is carried out to 0.3g carbon nanotubes, be then diluted to neutrality, then
Carry out centrifugal treating；
Step 2: being 1 with volume ratio:2 absolute ethyl alcohol and acetone prepares mixed liquor, takes 500ml, the Al of 0.06g is added
(NO3)3With the carbon nanotube after 0.2g step 1 acidifications, ultrasonic disperse 8 hours obtains CNTS suspension；
Step 3: using the titanium foil of step 1 processing as cathode, using stainless steel substrates as anode, the suspension of step 2 acquisition
Liquid is electrolyte, and two pole plates are immersed in suspension simultaneously, apply direct current between electrode, distance is fixed as between two-plate
50mm, voltage 30V, time 10s obtain CNTs sedimentaries on titanium foil surface, that is, obtain CNTs/Ti monolayer materials, CNTs
Deposit thickness is about 50nm, as shown in Figure 2；
Step 4: stacking is laminated in CNTs/Ti monolayer materials, lowest level and top layer are pure Ti foils (as shown in Figure 1), so
Discharge plasma sintering (SPS) is carried out afterwards, and sintering temperature is 500 DEG C, pressure 70MPa, soaking time 10min；Such as Fig. 3 institutes
Show, compared with conventional thermocompression sintering process, the quick SPS sintering of low temperature can be to avoid strong interfacial reaction occurs for CNTs and Ti and gives birth to
At brittle TiC phases.The sintered microstructures of SPS are as shown in figure 4, show apparent layer structure feature.
Step 5: carrying out 480 DEG C of rollings to the material that step 4 obtains, annealing time is 15min, mill speed between passage
For 0.15m/s, first pass deformation 50%, every time deflection is 10%, and rolling total deformation is 90%, that is, is prepared
CNTs/Ti biomimetic micro-nano laminated composite materials, pattern do not occur as shown in figure 5, CNTs and Titanium base interface cohesion are good
Apparent chemical reaction.Its tensile property is as shown in table 1,
The pure titanium of 1 multilayer of table is compared with CNTs/Ti biomimetic micro-nano laminated composite materials tensile properties
As shown in Table 1, compared with the pure titanium of matrix multilayer, tensile strength improves about 100MPa, and elongation after fracture is still up to
27%, mechanical property achieves the desired results.
Claims (10)
- The preparation method of 1.CNTs/Ti biomimetic micro-nano laminated composite materials, it is characterised in that the preparation method is by following What step carried out：Step 1: being pre-processed to titanium foil surface with HF solution, acidification is carried out to carbon nanotube with mixed acid, it is described mixed Acid is closed to be formulated by the concentrated sulfuric acid and concentrated nitric acid；Step 2: preparing mixed liquor with absolute ethyl alcohol and acetone, then Al (NO are added into mixed liquor3)3With step 1 acidification Carbon nanotube afterwards, ultrasonic disperse obtain CNTs suspension；Step 3: using the titanium foil of step 1 processing as cathode, using stainless steel substrates as anode, the CNTs that step 2 obtains suspends Liquid is electrolyte, applies direct current between electrode, obtains nanoscale CNTs sedimentaries on titanium foil surface, that is, obtains CNTs/Ti single layers Material；Step 4: stacking is laminated in CNTs/Ti monolayer materials, lowest level and top layer are pure Ti foils, then carry out discharging etc. from Son sintering (SPS)；Step 5: carrying out zerolling to the material that step 4 obtains, that is, prepare CNTs/Ti biomimetic micro-nano lamination composite woods Material.
- 2. the preparation method of CNTs/Ti biomimetic micro-nanos laminated composite materials according to claim 1, it is characterised in that step Titanium foil thickness described in rapid one is 10-100 μm.
- 3. the preparation method of CNTs/Ti biomimetic micro-nanos laminated composite materials according to claim 1, it is characterised in that step The volumetric concentration of the rapid HF solution is 10%~20%.
- 4. the preparation method of CNTs/Ti biomimetic micro-nanos laminated composite materials according to claim 1, it is characterised in that step Carbon nanotube, which carries out acidification, in rapid one is completed by following step：It is (1~3) with volume ratio:1 concentrated sulfuric acid prepares mixed acid with concentrated nitric acid, then with mixed acid to 0.1g~0.6g carbon nanometers Pipe carries out 2~8h of acidification, is then diluted to neutrality, then carries out centrifugal treating；The volume ratio of absolute ethyl alcohol and acetone is 1 in mixed liquor in step 2:(1~5), every liter of mixed liquor addition 0.04g~ Al (the NO of 0.2g3)3With the CNTs after 0.5g~3.0g step 1 acidifications, the ultrasonic disperse time is 2~10 hours.
- 5. the preparation method of CNTs/Ti biomimetic micro-nanos laminated composite materials according to claim 1, it is characterised in that step The two poles of the earth distance between plates is 20~80mm in rapid three, and electrophoretic deposition voltage is 10~50V, and sedimentation time is 5s~80s.
- 6. the preparation method of CNTs/Ti biomimetic micro-nanos laminated composite materials according to claim 1, it is characterised in that step Distance is fixed as 50mm between two-plate in rapid three, and electrophoretic deposition voltage is 30V, sedimentation time 10s.
- 7. the preparation method of CNTs/Ti biomimetic micro-nanos laminated composite materials according to claim 1, it is characterised in that step Discharge plasma sintering temperature is 300~700 DEG C in rapid four, and pressure is 40~100MPa, and soaking time is 5~30min.
- 8. the preparation method of CNTs/Ti biomimetic micro-nanos laminated composite materials according to claim 1, it is characterised in that step Discharge plasma sintering temperature is 500 DEG C, pressure 70MPa, soaking time 10min in rapid four.
- 9. the preparation method of CNTs/Ti biomimetic micro-nanos laminated composite materials according to claim 1, it is characterised in that step Rolling temperature is 300~500 DEG C in rapid five, and annealing time is 5~30min between passage, and mill speed is 0.1~2m/s, first road Secondary deflection 40%~70%, remaining pass deformation are 5%~15%, and rolling total deformation is 70%~96%.
- 10. the preparation method of CNTs/Ti biomimetic micro-nanos laminated composite materials according to claim 1, it is characterised in that Rolling temperature is 480 DEG C in step 5, and annealing time is 15min, mill speed 0.15m/s, first pass deformation between passage 50%, remaining every time deflection is 10%, and rolling total deformation is 90%.
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| CN107470358A (en) * | 2017-10-11 | 2017-12-15 | 宝鸡市永盛泰钛业有限公司 | A kind of processing method of titanium-alloy thin-plate |
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| CN111251691A (en) * | 2018-11-30 | 2020-06-09 | 哈尔滨工业大学 | Preparation method of multi-scale structure titanium alloy material |
| CN111379002B (en) * | 2020-03-31 | 2021-03-05 | 西安稀有金属材料研究院有限公司 | Method for rapidly preparing high-strength and high-toughness layered titanium-based composite material |
| CN114622110B (en) * | 2022-03-17 | 2023-02-10 | 西北有色金属研究院 | Preparation method of titanium-nickel alloy-based composite material with wide temperature range and high damping response |
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