CN105442035A - Method for controllably preparing single crystal tin nanowires/micron wires from surface of tin-aluminum alloy - Google Patents
Method for controllably preparing single crystal tin nanowires/micron wires from surface of tin-aluminum alloy Download PDFInfo
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- CN105442035A CN105442035A CN201510789340.1A CN201510789340A CN105442035A CN 105442035 A CN105442035 A CN 105442035A CN 201510789340 A CN201510789340 A CN 201510789340A CN 105442035 A CN105442035 A CN 105442035A
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B1/00—Single-crystal growth directly from the solid state
- C30B1/02—Single-crystal growth directly from the solid state by thermal treatment, e.g. strain annealing
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/02—Elements
Abstract
The invention discloses a method for controllably preparing single crystal tin nanowires/micron wires from the surface of tin-aluminum alloy, belonging to the field of preparation of metal nanometerials. According to the method, the diameter and length size controllable preparation of the single crystal tin nanowires/micron wires can be realized; the tin-aluminum alloy is taken as a raw material and is subjected to smelting, high-temperature storage and the like so as to prepare the single crystal tin nanowires/micron wires with controllable diameters and lengths; by adjusting the microcosmic structural size of the alloy, the preparation of the tin nanowires/micron wires with different diameters can be realized, and the diameter range is 10nm-20mu m; by adjusting the high-temperature storage conditions, the preparation of the tin nanowires/micron wires with different lengths can be realized, and the length range is 100nm-2mm; conventional chemical methods for preparing the nanowires are broken through, complex technical processes including the preparation, dissolving and the like of templates are omitted, the preparation process is simple, and a novel method is provided for the controllable preparation of the single crystal tin nanowires/micron wires.
Description
Technical field
The present invention relates to metal nano material preparing technical field, be specifically related to a kind of method from Sn-Al alloy surface controlled synthesis monocrystalline stannum nanowire/micro wire, the controlled synthesis of stannum nanowire/micro wire length and diameter etc. can be realized.
Background technology
Nano wire is monodimension nanometer material, because it has peculiar physicals (electricity, magnetics, optics and mechanics), have potential application in fields such as microelectronics and photoelectric device, sensor, solar cells, therefore the controlled synthesis of nano wire just causes the very big concern of investigator.Metallic tin nano wire has a wide range of applications in fields such as chemical sensor, lithium ion battery, photodiodes.Especially, the electron transport property of monocrystalline stannum nanowire is more excellent, can increase substantially its performance, and can show superconducting characteristic.Therefore, the controlled synthesis realizing monocrystalline stannum nanowire is of great significance its application tool.
At present, preparing the most frequently used method of metallic tin nano wire is template.Electrochemical deposition, collosol and gel, chemical vapour deposition etc. is adopted to pass through template synthesis stannum nanowire.Template can regulate and control the pattern of stannum nanowire well, and can obtain the array of the consistent stannum nanowire of orientation.But template complex process, aftertreatment is more loaded down with trivial details, and the stannum nanowire prepared is generally polycrystalline stannum nanowire.LuoB adopts the template improved successfully to prepare monocrystalline stannum nanowire (Nanoscale, 2010 of [100] orientation; 2:1661), but preparation process is very complicated.In addition, adopt microwave, ultrasonic assistant reduction method, laser radiation method and hydrothermal method etc. can synthetic metals nano wire, but these methods are all difficult to realize the diameter of nano wire and the controlled synthesis of length, and complicated process of preparation, also to repeatedly wash to prevent ion residues.
Tin content is the tin monocrystal nanowire/micro wire grown under stress condition, and its growth has preferred orientation.Lee's wealth and the tin content of Liu Zhiquan report more than 80% be low index direction growth (Acta.Mater.2013 along [100], [001], [101] and [103] etc.; 61:589).Research is thought, the growth of tin content is the crystal growth pattern under a kind of special conditions, and tin or tinbase coating can both autonomous growth tin content with some tin alloy surfaces.The autonomous growth of tin content can be given as electronic devices and components bring integrity problem, if this special crystal growth pattern can be utilized to realize the controllable growth of tin content, this will be a kind of method simply, effectively preparing monocrystalline stannum nanowire/micro wire.
Summary of the invention
The object of the present invention is to provide a kind of method from Sn-Al alloy surface controlled synthesis monocrystalline stannum nanowire/micro wire, solve the problem such as complex process, impurities left existed in existing chemical technology method.
Technical scheme of the present invention is:
From a method for Sn-Al alloy surface controlled synthesis monocrystalline stannum nanowire/micro wire, the method take Sn-Al alloy as starting material, by smelt and high temperature such as to deposit at the process, prepares the monocrystalline stannum nanowire/micro wire of length and controlled diameter on its surface; The method specifically comprises the steps:
(1) using Al content be the Sn-Al alloy of 5 ~ 99wt.% as starting material, obtain Sn-Al alloy ingot casting through quick cooling after smelting;
(2) the Sn-Al alloy ingot casting obtained is cut into the Sn-Al alloy sample of desired thickness, then grinding, polishing are to obtain clean Sn-Al alloy specimen surface;
(3) deposit under the Sn-Al alloy sample obtained being placed in hot conditions, namely its surface grows described monocrystalline stannum nanowire/micro wire.
In above-mentioned steps (1), in gained Sn-Al alloy ingot casting, the size of tin phase constitution determines the size of stannum nanowire/micro wire diameter, and the diameter range of the monocrystalline finally obtained stannum nanowire/micro wire is 10nm ~ 20 μm.In gained Sn-Al alloy ingot casting, the size of tin phase constitution is determined by the preparation technology of Sn-Al alloy ingot casting, comprises Sn-Al alloy composition, alloy smelting Method and process parameter.Adopt electric arc furnace or induction furnace melting method during melting Sn-Al alloy, ambient environmental conditions is vacuum, shielding gas or atmospheric condition, and speed of cooling is greater than 5 DEG C/min, and the microtexture size of the alloy that different smelting processes and condition prepare is different.
In above-mentioned steps (2), described Sn-Al alloy sample is block or sheet, and its thickness is greater than 0.2mm; Or Sn-Al alloy sample is whole Sn-Al alloy ingot casting.
In above-mentioned steps (3), the storage temperature of described Sn-Al alloy sample is constant temperature or thermal cycling mode, and during constant temperature, temperature range is 30 ~ 200 DEG C, and temperature is higher, and the thermal mismatch stress of alloy inside is larger, and the speed of growth of stannum nanowire/micro wire is faster; During thermal cycling mode, by the storage temperature of Sn-Al alloy sample according to " heat up-cooling-intensification " process reciprocation cycle, temperature cycle range is-40 ~ 200 DEG C, by the length and the quantity that regulate all numbers of thermal cycling can control stannum nanowire/micro wire, all numbers of thermal cycling are more, the stand density of stannum nanowire/micro wire is larger (namely in unit surface, growth population is more), length shorter (a circulating cycle number refers to that storage temperature is warmed up to 200 DEG C from-40 DEG C, then is cooled to the process of-40 DEG C).
The length range of prepared stannum nanowire/micro wire is 100nm ~ 2mm, and stand density is 10 ~ 500/mm
2, the speed of growth is 0.1 ~ 1.0nm/s.
In above-mentioned steps (3), described Sn-Al alloy sample storage environment condition is vacuum, gas shield or atmospheric condition.Shelf-time of described Sn-Al alloy sample is 0.5 little of 200 days, stannum nanowire/the micro wire of different lengths can be prepared by the shelf-time adjusting sample, shelf-time is longer, and length is longer, and the length range of the stannum nanowire/micro wire prepared is 100nm ~ 2mm.
Utilize the method for growth of tin crystal whisker at Sn-Al alloy surface controlled synthesis monocrystalline stannum nanowire/micro wire in the present invention, solve the complex process existed in existing method.Compared with the template extensively adopted at present, the present invention has the following advantages:
1, the present invention breaches the traditional chemical routes preparing stannum nanowire/micro wire, utilizes Sn-Al alloy for starting material, by smelting, can realize the preparation of a large amount of monocrystalline stannum nanowire/micro wire at short notice, and technique is simple, easy handling;
2, the present invention realizes the control of monocrystalline stannum nanowire/micro wire diameter by the microtexture of the alloy regulating melting, and diameter range is 10nm ~ 20 μm, and controllability is strong; By the control regulating the condition of high temperature storage to realize stannum nanowire/micro wire length, its length range is 100nm ~ 2mm.
Accompanying drawing explanation
Fig. 1 is the tin micro wire of Sn80Al alloy surface growth in embodiment 1.
Fig. 2 is a tin micro wire of Sn80Al alloy surface growth in embodiment 1, diameter about 1 μm.
Fig. 3 is the tin micro wire of Sn50Al alloy surface growth in embodiment 2.
Fig. 4 is that the length of Sn80Al alloy surface growth in embodiment 3 is greater than the tin micro wire of 1mm.
Fig. 5 is a tin micro wire and the transmission electron diffraction (TED) spectrum thereof of Sn80Al alloy surface growth in embodiment 3; Wherein: (a) monocrystalline stannum nanowire; B () transmission electron diffraction (TED) is composed.
Embodiment:
Below in conjunction with drawings and Examples, the present invention is described in further detail.
The present invention is the method from Sn-Al alloy surface controlled synthesis monocrystalline stannum nanowire/micro wire, utilizes Sn-Al alloy for starting material, by the process such as smelting, high temperature is deposited, prepares the controlled monocrystalline stannum nanowire/micro wire such as length and diameter at specimen surface.Concrete steps are as follows:
(1) Sn-Al alloy choosing certain ingredients, as starting materials, obtains Sn-Al alloy ingot casting by smelting, fast cooling;
(2) the Sn-Al alloy ingot casting obtained is cut into certain thickness sample, then enter grinding, polishing to obtain clean surface;
(3) deposit for some time under the sample obtained being placed in hot conditions, a large amount of monocrystalline stannum nanowire/micro wires will be prepared in its surface.
In the present invention, in Sn-Al alloy, the massfraction of Al can between 5 ~ 99% (being all massfraction in following examples), and the microtexture size that different alloying constituents smelts the alloy obtained is different.
In the present invention; the method such as electric arc furnace, induction furnace can be adopted during molten alloy; ambient environmental conditions can be vacuum, shielding gas or atmospheric condition, and speed of cooling is greater than 5 DEG C/min, and the microtexture size of the alloy that different smelting processes and condition obtain is different.
In the present invention, can by regulating the thick and tiny controlled synthesis realizing stannum nanowire/micro wire diameter of microtexture of Sn-Al alloy, diameter range is 10nm ~ 20 μm.
In the present invention, Sn-Al alloy sample can be block and sheet, but thickness can not be too thin, be thicker than 0.2mm, and this sample can also be whole alloy cast ingot.
In the present invention, the temperature that the alloy high-temp for the preparation of stannum nanowire/micro wire is deposited is 30 ~ 200 DEG C, and temperature is higher, and the thermal mismatch stress of alloy inside is larger, and the speed of growth of stannum nanowire/micro wire is faster; Storage environment condition can be vacuum, gas shield or atmospheric condition.
In the present invention, can be regulated the length of stannum nanowire/micro wire by Control Assay in the time that high temperature is deposited, the time of depositing is 0.5 little of 200 days, and the length range of nano wire/micro wire is 100nm ~ 2mm.
In the present invention, the storage condition of sample can also be thermal cycle conditions, and temperature cycle range can between-40 ~ 200 DEG C, all numbers of thermal cycling are more, the quantity of stannum nanowire/micro wire is more, and length is shorter, can by length and the quantity regulating all numbers of thermal cycling to control whisker.
Embodiment 1
(1) smelt Sn80Al alloy in atmosphere, then adopt water-cooled to cool fast, alloy structure is more tiny;
(2) adopt Linear cut by the Sn80Al alloy of smelting cut become the sample that thickness is 1.5mm, then through grinding, polishing, cleaning to obtain smooth, clean surface;
(3) sample obtained is incubated 24 hours in the loft drier of 60 DEG C, sample surfaces can obtain a large amount of monocrystalline tin micro wire, and as shown in Figure 1, stand density is 40/mm
2.Fig. 2 is a wherein micro wire, and diameter is about 1 μm.
Embodiment 2
(1) smelt Sn50Al alloy in atmosphere, then cool fast, alloy structure is thicker;
(2) adopt Linear cut by the Sn50Al alloy of smelting cut become the sample that thickness is 1mm, then through grinding, polishing, cleaning to obtain smooth, clean surface;
(3) sample obtained is incubated 72 hours in the loft drier of 60 DEG C, sample surfaces and side grow a large amount of monocrystalline tin micro wire, and stand density is 40/mm
2..Wherein the micro wire of lateral growth as shown in Figure 3, and its diameter is 2 ~ 5 μm.
Embodiment 3
(1) smelt Sn80Al alloy in atmosphere, then adopt water-cooled to cool fast;
(2) adopt Linear cut by the Sn80Al alloy of smelting cut become the sample that thickness is 2mm, then through grinding, polishing, cleaning to obtain smooth, clean surface;
(3) sample obtained is incubated 6 hours in the loft drier of 150 DEG C, sample surfaces can obtain a large amount of monocrystalline tin micro wire, and as shown in Figure 4, gained micro wire length is greater than 1mm.Fig. 5 is this sample surfaces tin micro wire and transmission electron microscope electron diffraction pattern thereof, shows that this micro wire is monocrystalline.
The above results shows, present invention, avoiding preparation technology complicated in conventional chemical methods, and can realize the controlled synthesis of monocrystalline stannum nanowire/micro wire, providing convenience for preparing monocrystalline stannum nanowire/micro wire device.
The embodiment more than provided is only explain the mode illustrated, should not think to limit scope of the present invention, and any method being equal to replacement according to technical scheme of the present invention and inventive concept thereof or changing, all should be encompassed within protection scope of the present invention.
Claims (10)
1. the method from Sn-Al alloy surface controlled synthesis monocrystalline stannum nanowire/micro wire, it is characterized in that: the method take Sn-Al alloy as starting material, by the process of smelting and high temperature is deposited, prepare the monocrystalline stannum nanowire/micro wire of length and controlled diameter on its surface.
2., according to the method from Sn-Al alloy surface controlled synthesis monocrystalline stannum nanowire/micro wire according to claim 1, it is characterized in that: the method specifically comprises the steps:
(1) using Al content be the Sn-Al alloy of 5 ~ 99wt.% as starting material, obtain Sn-Al alloy ingot casting through quick cooling after smelting;
(2) the Sn-Al alloy ingot casting obtained is cut into the Sn-Al alloy sample of desired thickness, then grinding, polishing are to obtain the Sn-Al alloy sample of clean surface;
(3) deposit under the Sn-Al alloy sample obtained being placed in hot conditions, namely its surface grows described monocrystalline stannum nanowire/micro wire.
3. according to the method from Sn-Al alloy surface controlled synthesis monocrystalline stannum nanowire/micro wire according to claim 2, it is characterized in that: in step (1), in gained Sn-Al alloy ingot casting, the size of tin phase constitution determines the size of stannum nanowire/micro wire diameter, and the diameter range of the monocrystalline finally obtained stannum nanowire/micro wire is 10nm ~ 20 μm.
4. according to the method from Sn-Al alloy surface controlled synthesis monocrystalline stannum nanowire/micro wire according to claim 3, it is characterized in that: in gained Sn-Al alloy ingot casting, the size of tin phase constitution is determined by the preparation technology of Sn-Al alloy ingot casting, comprises Sn-Al alloy composition, alloy smelting Method and process parameter.
5. according to the method from Sn-Al alloy surface controlled synthesis monocrystalline stannum nanowire/micro wire according to claim 4; it is characterized in that: during melting Sn-Al alloy, adopt electric arc furnace or induction furnace melting method; ambient environmental conditions is vacuum, shielding gas or atmospheric condition, and speed of cooling is greater than 5 DEG C/min.
6. according to the method from Sn-Al alloy surface controlled synthesis monocrystalline stannum nanowire/micro wire according to claim 2, it is characterized in that: in step (2), described Sn-Al alloy sample is block or sheet, and its thickness is greater than 0.2mm; Or Sn-Al alloy sample is whole Sn-Al alloy ingot casting.
7. according to the method from Sn-Al alloy surface controlled synthesis monocrystalline stannum nanowire/micro wire according to claim 2, it is characterized in that: the storage temperature of described Sn-Al alloy sample is constant temperature or thermal cycling mode, during constant temperature, temperature range is 30 ~ 200 DEG C, temperature is higher, and the speed of growth of stannum nanowire/micro wire is faster; During thermal cycling mode, by the storage temperature of Sn-Al alloy sample according to " heat up-cooling-intensification " process reciprocation cycle, temperature cycle range is-40 ~ 200 DEG C, by the length and the quantity that regulate all numbers of thermal cycling can control stannum nanowire/micro wire, all numbers of thermal cycling are more, the stand density of stannum nanowire/micro wire is larger, and length is shorter.
8., according to the method from Sn-Al alloy surface controlled synthesis monocrystalline stannum nanowire/micro wire according to claim 7, it is characterized in that: the length range of prepared stannum nanowire/micro wire is 100nm ~ 2mm, and stand density is 10 ~ 500/mm
2, the speed of growth is 0.1 ~ 1.0nm/s.
9., according to the method from Sn-Al alloy surface controlled synthesis monocrystalline stannum nanowire/micro wire according to claim 2, it is characterized in that: in step (3), described Sn-Al alloy sample storage environment condition is vacuum, gas shield or atmospheric condition.
10. according to the method from Sn-Al alloy surface controlled synthesis monocrystalline stannum nanowire/micro wire described in claim 2 or 9, it is characterized in that: in step (3), shelf-time of described Sn-Al alloy sample is 0.5 little of 200 days, stannum nanowire/the micro wire of different lengths can be prepared by the shelf-time adjusting sample, shelf-time is longer, length is longer, and the length range of the stannum nanowire/micro wire prepared is 100nm ~ 2mm.
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CN106517316A (en) * | 2016-10-31 | 2017-03-22 | 华南理工大学 | Method for preparing polymorphic micro-nano tin dioxide by electro-thermal coupling field loading |
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