CN102220603A - NbTi nanowires and preparation method thereof - Google Patents
NbTi nanowires and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to NbTi nanowires and a preparation method thereof. The NbTi nanowires comprise the components of Nb, Ti and Ni, and have a diameter of below 100 nm and a length of 10 mu m-5 mm. The present invention also provides the preparation method of the NbTi nanowires,. The method comprises the following steps of: placing a graphite electrode used as the cathode and a NbTi/TiNi composite wire used as the anode in an electrolyte for electrolysis until the current density decreases to zero, and controlling the output potential of a power supply at 1-10V during electrolysis; and taking out the anode, cleaning and drying to obtain the NbTi nanowires. The NbTi nanowires provided by present invention are from micron grade to millimeter grade. The preparation method of the NbTi nanowires by electrolysis provided by the present invention has the characteristics of simple process, low cost, high product yield, and the like.
Description
Technical field
The present invention relates to a kind of NbTi nano wire and preparation method thereof, belong to field of nano material preparation.
Background technology
One-dimensional nano structure material is owing to have unique optical characteristics and quantum transmission effects, and it is having important use to be worth aspect molecular circuit and the quantum components and parts, and the one-dimensional nano structure material of therefore synthetic superior performance becomes the focus that the scholar pays close attention to.
The method of synthesizing one-dimensional nano wire is more at present, mainly contains following several: template synthesis method, vapour deposition process, pyrolysis method, sol-gel method etc.Though all can access nano wire by above-mentioned preparation method, but have that complicated process of preparation, cost are higher, contaminate environment, be difficult to nano wire such as is successfully separated at problem from template and organic solvent, and problem such as yield poorly and nanowire length is short is especially outstanding.01127650.9 number Chinese patent discloses a kind of method of chemical Vapor deposition process growth SiC nano wire, method by this patent disclosure can prepare the SiC nano wire, but the SiC nanowire growth promptly stops growing to certain-length, the SiC nanowire length of its preparation is the longest to reach 5 microns only, has limited the development and the application of SiC nano wire greatly.
There are the problems referred to above in the preparation that is not only the SiC nano wire, and also there is identical problem in the preparation of a lot of nano wires, and these problems have limited the development and the application of one-dimensional nano line greatly.
The NbTi superconductor has obtained broad research and application since early 1960s is found, all be widely used as Magnetic resonance imaging (MRI), nucleus magnetic resonance (NMR), Laboratory Instruments, particle accelerator, electric power, clearance, the separation of ore magnetic, magnetic suspension train, superconducting energy storage fields such as (SMES).If can access the NbTi line of Nano grade, will promote the development of NbTi superconductor greatly and in above-mentioned Application for Field, still, do not have as yet at present the NbTi nano wire with and preparation method thereof report.
Summary of the invention
For solving the problems of the technologies described above, the object of the present invention is to provide a kind of NbTi nano wire, its length can reach micron order even millimeter level.
The present invention also aims to provide the preparation method of above-mentioned NbTi nano wire, obtain the NbTi nano wire, have characteristics such as cost is low, energy consumption is low, technology is simple, output height by the NbTi/TiNi matrix material is carried out electrolysis.
For achieving the above object, the present invention at first provides a kind of NbTi nano wire, and wherein, the one-tenth of this NbTi nano wire is grouped into and comprises: Nb element, Ti element and Ni element; And the diameter of this NbTi nano wire is 100nm following (being preferably 40nm-100nm), and length is 10 microns-5 millimeters.
According to concrete technical scheme of the present invention, preferably, above-mentioned NbTi nano wire obtains by electrolytic preparation, for example potentiostatic electrolysis.More preferably, in electrolytic process, with NbTi/TiNi matrix material silk material as anode, and, the composition of this NbTi/TiNi matrix material silk material consists of: atomic percent is the Nb element (being preferably 20at%) of 18-22%, and atomic ratio is 0.3: 1-1.5: 1 Ti element and Ni element, Ti element, Ni element and Nb elements atomic percentage sum are 100%.
NbTi nano wire provided by the invention is to be main component with Nb element and Ti element, the nano material that contains a certain amount of Ni element simultaneously, preferably, the one-tenth of above-mentioned NbTi nano wire is grouped into and comprises: the Ni of the Nb of 60-80at.%, the Ti of 15-30at.%, 2-8at.%, the per-cent sum of three kinds of elements is 100%.More preferably, the one-tenth of this NbTi nano wire is grouped into and comprises: the Ni of the Nb of 68-76at.%, the Ti of 20-26at.%, 4-6at.%, the per-cent sum of three kinds of elements is 100%.
The present invention also provides the preparation method of above-mentioned NbTi nano wire, and it may further comprise the steps:
With Graphite Electrodes as negative electrode, with NbTi/TiNi matrix material silk material as anode, place electrolytic solution to carry out electrolysis, stop electrolysis (generally electrolysis time can be controlled at 10-12 hour) when current density drops to zero, the output potential of power supply during electrolysis is controlled to be 1-10V;
Anode is taken out, and cleaning, drying obtains the NbTi nano wire.
In above-mentioned preparation method provided by the invention, preferably, electrolytic solution is by concentration (mass percent) is (0.05-0.5) for 80-99.9wt% methyl alcohol according to volume ratio for the nitric acid of 50-70wt% and concentration (mass percent): 1 mixed obtains.More preferably, above-mentioned electrolytic solution is by being that the nitric acid of 65-68% and concentration are that 99.5% methyl alcohol is (0.05-0.5) according to volume ratio with concentration: 1 mixed obtains.
In electrolytic process, electrolytic temperature may be controlled to 10-80 ℃, is preferably room temperature, and this electrolysis is preferably carried out in airtight lighttight space.
In above-mentioned preparation method provided by the invention, preferably, the NbTi/TiNi matrix material silk material that is adopted is to prepare by the preparation method who may further comprise the steps:
(1) choose the niobium that purity is 99.0wt.%-99.9wt.% by the composite material compositions proportioning, purity is the titanium of 99.0wt.%-99.9wt.%, and purity is the nickel of 99.0wt.%-99.9wt.%;
(2) above-mentioned simple substance Ti, Ni and Nb are put into vacuum tightness and be higher than 10
-1Carry out melting in the smelting furnace of Pa or protection of inert gas and obtain the NbTi/TiNi matrix material, and casting obtains ingot casting;
(3) in vacuum oven, the homogenizing annealing that under 950 ℃ ingot casting was carried out 10 hours is handled;
(4) ingot casting after will annealing becomes bar-shaped cast ingot or pie ingot casting 850 ℃ of forge hots;
(5) club-shaped material or the pie material that forge hot is obtained repeats plastic working, obtains NbTi/TiNi matrix material silk material.
In above-mentioned preparation method provided by the invention, preferably, the composition of above-mentioned NbTi/TiNi matrix material silk material consists of: atomic percent is the Nb element (being preferably 20at%) of 18-22%, and atomic ratio is 0.3: 1-1.5: 1 Ti element and Ni element, Ti element, Ni element and Nb elements atomic percentage sum are 100%.
In above-mentioned preparation method provided by the invention, the plastic working of being adopted is for ingot casting being processed into a material, promptly carries out wire drawing processing, preferably, can be undertaken by following dual mode:
Ingot casting through hot-forging forming is repeated cold-drawn and recrystallization annealing, obtain NbTi/TiNi matrix material silk material; Perhaps,
Ingot casting through hot-forging forming is carried out hot drawing, obtain NbTi/TiNi matrix material silk material.
In order to control the diameter of the NbTi nano wire for preparing, and in electrolytic process, make the NbTi nano wire keep continuum of states as far as possible, preferably, the diameter of the NbTi/TiNi matrix material silk material that obtains by plastic working is 0.5-2mm, and more preferably, the diameter of silk material is 1mm.
Preparation method provided by the invention is by carrying out metal simple-substance niobium, titanium, nickel mixing melting and obtain the ultra-fine eutectic structure of as cast condition in-situ authigenic NbTi/TiNi, then, by the ingot casting after the melting being carried out plastic workings such as forge hot and wire drawing, can make in the resulting NbTi/TiNi matrix material silk material, the length overlength of NbTi phase (wire or fibrous), and be evenly distributed in the TiNi matrix along axis direction.The preparation method of NbTi nano wire provided by the invention is by control electrolytic potential (1-10V), NbTi is in passivation region mutually so that TiNi is in the region of activation mutually, carry out electrolysis then, TiNi in the NbTi/TiNi matrix material silk material is corroded mutually, and reservation NbTi phase, after electrolysis, can make the NbTi nano wire keep its pattern in NbTi/TiNi matrix material silk material, its length can reach micron order even millimeter level.
NbTi nano wire of the present invention is expected in fields such as optics, electricity performances important research and using value, for example can be with its component units as the nano-electron components and parts, or connect each nano-electron components and parts with the built-up circuit unit as lead.
Preparation method by electrolytic preparation NbTi nano wire provided by the invention has characteristics such as technology is simple, with low cost, productive rate height, the length dimension of the NbTi nano wire for preparing is in micron order even millimeter level, all longer than existing nano wire, as shown in Figures 2 and 3, wherein, Fig. 2 is macroscopical picture that electrolysis finishes back NbTi nano line cluster, and as can be seen from Figure 3 NbTi nanowire length overlength has reached 2.17 millimeters.Adopt the preparation method of nano wire provided by the invention can also avoid being difficult in the traditional preparation process technology with nano wire and template (carbon nanotube, multiaperture pellumina, polycarbonate membrane, biomolecules etc.) or the isolating drawback of organic solvent (ethylene glycol, N, dinethylformamide etc.).The preparation method of above-mentioned NbTi nano wire provided by the invention is the preparation method of the high-quality NbTi nano wire of a kind of acquisition of economy.
Description of drawings
Fig. 1 is the synoptic diagram of electrolyzer of the present invention;
Fig. 2 is the photo of NbTi nano wire;
Fig. 3 is the stereoscan photograph of NbTi nano wire;
The stereoscan photograph of the NbTi nano wire that Fig. 4 provides for embodiment 1;
The energy spectrum analysis collection of illustrative plates of the NbTi nano wire that Fig. 5 provides for embodiment 1;
The stereoscan photograph of the NbTi nano wire that Fig. 6 provides for embodiment 2;
The energy spectrum analysis collection of illustrative plates of the NbTi nano wire that Fig. 7 provides for embodiment 2;
The stereoscan photograph of the NbTi nano wire that Fig. 8 provides for embodiment 3;
The energy spectrum analysis collection of illustrative plates of the NbTi nano wire that Fig. 9 provides for embodiment 3.
Embodiment
Below by specific embodiment NbTi nano wire of the present invention and preparation method thereof is further detailed, but but can not be interpreted as the qualification that practical range of the present invention is done.
According to specific embodiments of the present invention, the preparation method of NbTi nano wire provided by the invention can may further comprise the steps:
1, preparation NbTi/TiNi matrix material silk material
(1) choose the niobium that purity is 99.0wt.%-99.9wt.% by the composition proportion of NbTi/TiNi matrix material silk material, purity is the titanium of 99.0wt.%-99.9wt.%, and purity is the nickel of 99.0wt.%-99.9wt.%;
(2) above-mentioned composite material compositions is put into smelting furnace, melting obtains the NbTi/TiNi memory alloy composite material under the argon shield of-0.05MPa, and it is cast into ingot casting;
(3) (final vacuum is 6.7 * 10 at vacuum oven
-4Pa) in, the homogenizing annealing that under 950 ℃ ingot casting was carried out 10 hours is handled;
(4) ingot casting after will annealing becomes bar-shaped cast ingot 850 ℃ of forge hots;
(5) bar-shaped cast ingot that forge hot is obtained repeats plastic working, up to obtaining the NbTi/TiNi matrix material silk material that diameter is 0.5-2mm; This plastic working comprises following dual mode:
The bar-shaped cast ingot that obtains through forge hot is repeated cold-drawn and recrystallization annealing, obtain NbTi/TiNi matrix material silk material; Perhaps,
The bar-shaped cast ingot that obtains through forge hot is carried out hot drawing, obtain NbTi/TiNi matrix material silk material.
2, NbTi/TiNi matrix material silk material is carried out electrolytic preparation NbTi nano wire
(1) be that the nitric acid of 65-68% is that 99.5% methyl alcohol is (0.05-0.5) according to volume ratio with concentration with concentration: 1 ratio is mixed, and obtains electrolytic solution;
(2) with Graphite Electrodes as negative electrode, the NbTi/TiNi matrix material silk material that with the diameter is 0.5-2mm is as anode, wherein, the length of silk material is exceeded can put into electrolyzer, before electrolysis, at first that the surface finish of NbTi/TiNi matrix material silk material is clean, and with acetone through the row ultrasonic cleaning; The synoptic diagram of electrolyzer of the present invention as shown in Figure 1;
(3) control D.C. regulated power supply output potential is 1-10V, carries out electrolysis, stops electrolysis when current density drops to zero;
(4) remaining anode is taken out, after acetone ultrasonic cleaning and infrared lamp oven dry, obtain the NbTi nano wire.
Present embodiment provides a kind of NbTi nano wire, and its preparation method may further comprise the steps:
1, preparation NbTi/TiNi matrix material silk material
(1) press Nb content 20at.%, Ti and 21: 19 proportioning of Ni atomic ratio are chosen the niobium that purity is 99.9wt.%, and purity is the titanium of 99.9wt.%, and purity is the nickel of 99.9wt.%, and wherein, the atomic percent sum of Nb, Ti and Ni is 100%;
(2) above-mentioned three kinds of metal components are put into vacuum melting furnace, under the argon shield of-0.05MPa, be smelted into ingot casting;
(3) in vacuum oven, the homogenizing annealing that under 950 ℃ ingot casting was carried out 10 hours is handled;
(4) under 850 ℃, the ingot casting forge hot after the annealing is become club-shaped material (bar-shaped cast ingot);
(5) under 600 ℃, it is Nb that the club-shaped material that forge hot is obtained carries out the composition that hot drawing obtains diameter 1mm
20Ti
42Ni
38Memory alloy composite material silk material.
2, NbTi/TiNi matrix material silk material is carried out electrolytic preparation NbTi nano wire
(1) at normal temperatures and pressures, be that 55% nitric acid and concentration are that 85% methyl alcohol volume ratio is 1: 5 configuration 600ml electrolytic solution with concentration, change in the electrolyzer behind the uniform mixing;
(2) from the Nb of diameter 1mm
20Ti
42Ni
38Choose 20cm on the memory alloy composite material silk material, after polishing and the ultrasonic cleaning, make electrolytic anode, as electrolysis cathode, electrolytic anode and electrolysis cathode are inserted in the electrolyzer with Graphite Electrodes;
(3) be electrolysis power with the constant-voltage DC source, output voltage is controlled to be 6V, and electrolysis to current density stops when dropping to zero, and electrolysis time is approximately 12 hours, and in the electrolytic process, electrolysis temperature is about 20 ℃;
(4) electrolytic anode is taken out, after acetone ultrasonic cleaning and infrared lamp oven dry, promptly obtain the NbTi nano wire.
The stereoscan photograph of the NbTi nano wire of present embodiment preparation can see that by Fig. 4 the diameter of the NbTi nano wire that obtains after the electrolysis is about 40nm as shown in Figure 4, and length is more than 2 μ m.Fig. 5 is the EDAX results of the NbTi nano wire of present embodiment preparation, and energy spectrometer analysis shows that the composition of the NbTi nano wire of present embodiment preparation consists of: the Ni of the Nb of 68.77at.%, the Ti of 25.87at.%, 5.36at.%.
Embodiment 2
Present embodiment provides a kind of NbTi nano wire, and its preparation method may further comprise the steps:
1, preparation NbTi/TiNi matrix material silk material
(1) press Nb content 20at.%, Ti and 21: 19 proportioning of Ni atomic ratio are chosen the niobium that purity is 99.9wt.%, and purity is the titanium of 99.9wt.%, and purity is the nickel of 99.9wt.%, and wherein, the atomic percent sum of Nb, Ti and Ni is 100%;
(2) above-mentioned three kinds of metal components are put into vacuum melting furnace, under the argon shield of-0.05MPa, be smelted into ingot casting;
(3) in vacuum oven, the homogenizing annealing that under 950 ℃ ingot casting was carried out 10 hours is handled;
(4) under 850 ℃, the ingot casting forge hot after the annealing is become club-shaped material (bar-shaped cast ingot);
(5) under 600 ℃, it is Nb that the club-shaped material that forge hot is obtained carries out the composition that hot drawing obtains diameter 1.5mm
20Ti
42Ni
38Memory alloy composite material silk material.
2, NbTi/TiNi matrix material silk material is carried out electrolytic preparation NbTi nano wire
(1) under the normal temperature and pressure, with concentration be 60% nitric acid and concentration be 95% methyl alcohol according to volume ratio configuration in 1: 5 600ml electrolytic solution, change electrolyzer behind the uniform mixing over to;
(2) from the Nb of diameter 1.5mm
20Ti
42Ni
38Choose 20cm on the memory alloy composite material silk material, after polishing and the ultrasonic cleaning, make electrolytic anode, as electrolysis cathode, electrolytic anode and electrolysis cathode are inserted in the electrolyzer with Graphite Electrodes;
(3) be electrolysis power with the constant-voltage DC source, output voltage is controlled to be 5V, and electrolysis to current density stops when dropping to zero, and electrolysis time is approximately 10 hours, and in the electrolytic process, electrolysis temperature is about 23 ℃;
(4) electrolytic anode is taken out, after acetone ultrasonic cleaning and infrared lamp oven dry, promptly obtain the NbTi nano wire.
The stereoscan photograph of the NbTi nano wire of present embodiment preparation can see that by Fig. 6 the diameter that obtains the NbTi nano wire after the electrolysis is that length is more than 500nm about 86.8nm as shown in Figure 6.Fig. 7 is the EDAX results of the NbTi nano wire of present embodiment preparation, and energy spectrometer analysis shows that the composition of the NbTi nano wire of present embodiment preparation consists of: the Ni of the Nb of 71.00at.%, the Ti of 22.68at.%, 6.32at.%.
Embodiment 3
Present embodiment provides a kind of NbTi nano wire, and its preparation method may further comprise the steps:
1, preparation NbTi/TiNi matrix material silk material
(1) press Nb content 20at.%, Ti and 21: 19 proportioning of Ni atomic ratio are chosen the niobium that purity is 99.9wt.%, and purity is the titanium of 99.9wt.%, and purity is the nickel of 99.9wt.%, and wherein, the atomic percent sum of Nb, Ti and Ni is 100%;
(2) above-mentioned three kinds of metal components are put into vacuum melting furnace, under the argon shield of-0.05MPa, be smelted into ingot casting;
(3) in vacuum oven, the homogenizing annealing that under 950 ℃ ingot casting was carried out 10 hours is handled;
(4) under 850 ℃, the ingot casting forge hot after the annealing is become club-shaped material (bar-shaped cast ingot);
(5) under 600 ℃, it is Nb that the club-shaped material that forge hot is obtained carries out the composition that hot drawing obtains diameter 0.5mm
20Ti
42Ni
38Memory alloy composite material silk material.
2, NbTi/TiNi matrix material silk material is carried out electrolytic preparation NbTi nano wire
(1) under the normal temperature and pressure, is 68% nitric acid and methyl alcohol configuration in 1: the 5 by volume 600ml electrolytic solution that is 99.5% with concentration, changes electrolyzer behind the uniform mixing over to concentration;
(2) from the Nb of diameter 0.5mm
20Ti
42Ni
38Choose 20cm on the memory alloy composite material silk material, after polishing and the ultrasonic cleaning, make electrolytic anode, as electrolysis cathode electrolytic anode and electrolysis cathode are inserted in the electrolyzer with Graphite Electrodes;
(3) be electrolysis power with the constant-voltage DC source, output voltage is controlled to be 7V, and electrolysis to current density stops when dropping to zero, and electrolysis time is approximately 12 hours, and in the electrolytic process, electrolysis temperature is about 20 ℃;
(4) electrolytic anode is taken out, after acetone ultrasonic cleaning and infrared lamp oven dry, promptly obtain the NbTi nano wire.
The stereoscan photograph of the NbTiNbTi nano wire of present embodiment preparation can see that by Fig. 8 the diameter that obtains the NbTi nano wire after the electrolysis is that length is more than 500nm about 59.8nm as shown in Figure 8.Fig. 9 is the EDAX results of the NbTi nano wire of present embodiment preparation, and energy spectrometer analysis shows that the composition of the NbTi nano wire of present embodiment preparation consists of: the Ni of the Nb of 75.34at.%, the Ti of 20.58at.%, 4.07at.%.
Above embodiment only is used to illustrate technical scheme of the present invention and is unrestricted, although the present invention is had been described in detail with reference to preferred embodiment, those of ordinary skill in the art is to be understood that, can make amendment or be equal to replacement technical scheme of the present invention, and not break away from the spirit and scope of technical solution of the present invention.
Claims (10)
1. a NbTi nano wire is characterized in that, the one-tenth of this NbTi nano wire is grouped into and comprises: Nb, Ti and Ni; And the diameter of this NbTi nano wire is below the 100nm, and length is 10 microns-5 millimeters.
2. NbTi nano wire as claimed in claim 1 is characterized in that, this NbTi nano wire obtains by electrolytic preparation.
3. NbTi nano wire as claimed in claim 2, it is characterized in that, in described electrolysis, with NbTi/TiNi matrix material silk material as anode, and, the one-tenth of described NbTi/TiNi matrix material silk material is grouped into and comprises: atomic percent is the Nb of 18-22%, and atomic ratio is 0.3: 1-1.5: 1 Ti and Ni, the atomic percent sum of Ti, Ni and Nb is 100%.
4. NbTi nano wire as claimed in claim 1 is characterized in that, the one-tenth of this NbTi nano wire is grouped into and comprises: the Ni of the Nb of 60-80at.%, the Ti of 15-30at.%, 2-8at.%, the per-cent sum of three kinds of elements is 100%.
5. as the preparation method of each described NbTi nano wire of claim 1-4, it may further comprise the steps:
As negative electrode, as anode, place electrolytic solution to carry out electrolysis with NbTi/TiNi matrix material silk material with Graphite Electrodes, stop electrolysis when current density drops to zero, the output potential of power supply during electrolysis is controlled to be 1-10V;
Anode is taken out, and cleaning, drying obtains the NbTi nano wire.
6. preparation method as claimed in claim 5, wherein, described electrolytic solution is by being that the nitric acid of 50-70wt% and concentration are that 80-99.9wt% methyl alcohol is (0.05-0.5) according to volume ratio with concentration: 1 mixed obtains.
7. preparation method as claimed in claim 5 is characterized in that, described NbTi/TiNi matrix material silk material prepares by following steps:
(1) choose the niobium that purity is 99.0wt.%-99.9wt.% by the composite material compositions proportioning, purity is the titanium of 99.0wt.%-99.9wt.%, and purity is the nickel of 99.0wt.%-99.9wt.%;
(2) above-mentioned simple substance Ti, Ni and Nb are put into vacuum tightness and be higher than 10
-1Carry out melting in the smelting furnace of Pa or protection of inert gas and obtain the NbTi/TiNi matrix material, and casting obtains ingot casting;
(3) in vacuum oven, the homogenizing annealing that under 950 ℃ ingot casting was carried out 10 hours is handled;
(4) ingot casting after will annealing becomes bar-shaped cast ingot or pie ingot casting 850 ℃ of forge hots;
(5) club-shaped material or the pie material that forge hot is obtained repeats plastic working, obtains NbTi/TiNi matrix material silk material.
8. as claim 5 or 7 described preparation methods, wherein, the composition of described NbTi/TiNi matrix material silk material consists of: atomic percent is the Nb of 18-22%, and atomic ratio is 0.3: 1-1.5: 1 Ti and Ni, the atomic percent sum of Ti, Ni and Nb is 100%.
9. preparation method as claimed in claim 7, wherein, described plastic working is:
Ingot casting through hot-forging forming is repeated cold-drawn and recrystallization annealing, obtain NbTi/TiNi matrix material silk material; Perhaps,
Ingot casting through hot-forging forming is carried out hot drawing, obtain NbTi/TiNi matrix material silk material.
10. preparation method as claimed in claim 9, wherein, the diameter of described NbTi/TiNi matrix material silk material is 0.5-2mm.
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| CN110216281A (en) * | 2019-07-23 | 2019-09-10 | 安徽工业大学 | A kind of NiTi nano wire and preparation method thereof |
| CN110216281B (en) * | 2019-07-23 | 2022-01-14 | 安徽工业大学 | NiTi nanowire and preparation method thereof |
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