CN204981128U - A load mould for assisting preparation optic fibre growth zinc oxide nano wire - Google Patents
A load mould for assisting preparation optic fibre growth zinc oxide nano wire Download PDFInfo
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- CN204981128U CN204981128U CN201520461098.0U CN201520461098U CN204981128U CN 204981128 U CN204981128 U CN 204981128U CN 201520461098 U CN201520461098 U CN 201520461098U CN 204981128 U CN204981128 U CN 204981128U
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Abstract
The utility model discloses a load mould for assisting preparation optic fibre growth zinc oxide nano wire, wherein, the both ends of loading the mould are provided with the first recess that is used for holding optic fibre tip respectively, correspond on the first recess to be provided with and be used for fixing the cushion on loading the mould with optic fibre, the cushion is fixed in in the first recess for dismantling, the middle part of loading the mould is provided with the second recess that is used for reserving the space for optic fibre growth zinc oxide nano wire, and the second recess sets up between two first recesses, and the degree of depth of second recess is greater than the degree of depth of first recess. This loading mould can make optic fibre in the first step and plant safe removal the effectively, during second step growth zinc oxide nano wire, can keep a suitable posture to can prevent that the white sediment from dropping on on the optic fibre.
Description
Technical field
The utility model relates to technical field of nanometer material preparation, particularly relates to a kind of loading mould for auxiliary preparation YAG Fiber Growth zinc oxide nanowire.
Background technology
Along with the development of science and technology, Fibre Optical Sensor demonstrates its advantage from strength to strength, but optical fiber itself does not have responding ability to biochemical gas, if the combination of the nano material with zinc oxide nanowire etc., optical fiber just can respond the concentration etc. of biochemical gas, in order to make zinc oxide nanowire effectively be combined with optical fiber, zinc oxide nanowire grows and just becomes of crucial importance on optical fiber.Zinc oxide nanowire be manufactured with a variety of method, and two one-step hydrothermals are comparatively simple, and the instrument and equipment of needs is not expensive yet, is beneficial to popularization, and are adapted at method that optical fiber makes.But most of similar technique is all be that substrate successfully prepares zinc oxide nanowire with silicon, and rare mentioning utilizes two one-step hydrothermals growth of zinc oxide nano line on optical fiber.Because growth of zinc oxide nano line exists two problems on optical fiber, optical fiber is wire, and after peeling coat off, comparatively fragile.This and other substrates, as silicon chip, mainly there is bigger difference in plane bulk, silicon chip be no matter the first step the growth of zinc oxide nano line of kind and second step can very easily move with tweezers and in growing container, keep suitable posture.Optical fiber is then different, due to the feature of its fragility and wire, in the first step that plant can not safety moving effectively, in the process of second step growth of zinc oxide nano line, a large amount of white precipitates can be produced, and these precipitations can drop on optical fiber, the zinc oxide nanowire prepared is made not to be very even.Therefore, prior art need development.
Utility model content
In view of above-mentioned the deficiencies in the prior art, the purpose of this utility model is to provide a kind of loading mould for auxiliary preparation YAG Fiber Growth zinc oxide nanowire, is intended to solve in prior art adopt two one-step hydrothermals growth of zinc oxide nano line Problems existing on optical fiber.
The technical solution of the utility model is as follows:
For a loading mould for auxiliary preparation YAG Fiber Growth zinc oxide nanowire, wherein, the two ends of described loading mould are respectively arranged with the first groove for optical fibre end; The corresponding cushion be provided with for optical fiber being fixed on loading mould on first groove, described cushion is for being removably fixed in the first groove; The middle part of described loading mould is provided with for the second groove for YAG Fiber Growth zinc oxide nanowire slot milling, and the second groove is arranged between two first grooves, and the degree of depth of the second groove is greater than the degree of depth of the first groove.
Further, described first groove comprises first slot suitable with optical fiber width being separately positioned on the first groove two ends, and is arranged on the second slot between slot, two ends first, and the second slot communicates with first slot at two ends, and the degree of depth is identical; Cushion is removably fixed in the second slot.
Further, described loading mould adopts polytetrafluoroethylene (PTFE) to make, and described cushion adopts dimethyl silicone polymer to make.
Beneficial effect: adopt the loading mould for auxiliary preparation YAG Fiber Growth zinc oxide nanowire provided by the utility model, optical fiber can in the first step, and plant can safety moving effectively, during second step growth of zinc oxide nano line, the posture that one suitable can be kept, and can prevent white precipitate from dropping on optical fiber, make optical fiber be applicable to two one-step hydrothermal growth of zinc oxide nano lines, and the zinc oxide nanowire growth of optical fiber surface evenly.And, adopt loading mould two one-step hydrothermals to prepare YAG Fiber Growth zinc oxide nanowire, easy and simple to handle.
Accompanying drawing explanation
Fig. 1 is the Facad structure schematic diagram that the utility model loads mould (not with cushion).
Fig. 2 is the Facad structure schematic diagram after the utility model loading mould (not with cushion) loads optical fiber.
Fig. 3 is the Facad structure schematic diagram after the utility model loading mould (band cushion) loads optical fiber.
Fig. 4 loads the Facad structure schematic diagram that container put into by mould in growth course in the utility model embodiment.
Fig. 5 loads the side structure schematic diagram that container put into by mould in growth course in the utility model embodiment.
Detailed description of the invention
The utility model provides a kind of YAG Fiber Growth zinc oxide nanowire and preparation method thereof and loading mould, for making the purpose of this utility model, technical scheme and effect clearly, clearly, further describes below to the utility model.Should be appreciated that specific embodiment described herein only in order to explain the utility model, and be not used in restriction the utility model.
Because optical fiber has the feature of fragility and wire, therefore in prior art, major part prepares zinc oxide nanowire on optical fiber is not use two one-step hydrothermals, and a kind of loading mould for auxiliary preparation YAG Fiber Growth zinc oxide nanowire provided by the utility model, just can solve the problem that two one-step hydrothermals are not suitable for growth of zinc oxide nano line on optical fiber.This loading mould optical fiber can be made in the first step plant can safety moving effectively, during second step growth of zinc oxide nano line, the posture that is suitable can be kept, and can prevent white precipitate from dropping on optical fiber.
Particularly, shown in composition graphs 1 ~ Fig. 3, the two ends of described loading mould are respectively arranged with the first groove 100 for optical fibre 400 end; The corresponding cushion 300 be provided with for optical fiber 400 being fixed on loading mould on first groove 100, described cushion 300 is for being removably fixed in the first groove 100; The middle part of described loading mould is provided with for the second groove 200 for optical fiber 400 growth of zinc oxide nano line slot milling, second groove 200 is arranged between two first grooves 100, the degree of depth of the second groove 200 is greater than the degree of depth of the first groove 100, and optical fiber 400 is soared aloft in the second groove 200.
Further, described first groove 100 is divided into three parts, be separately positioned on first slot 101 suitable with optical fiber 400 width at the first groove 100 two ends, and the second slot 102 be arranged between slot, two ends first 101, second slot 102 communicates with first slot 101 at two ends, and the degree of depth is identical.First slot 101 at two ends is suitable with the width of optical fiber 400, after the first groove 100 put into by optical fiber 400, undertaken spacing by the first slot 101, then in the second slot 102, cushion 300 is settled, because the first slot 101 is identical with the degree of depth of the second slot 102, just by the end winding support of optical fiber 400 between mould and cushion 300, and not easily can cause damage to optical fiber 400.Preferably, described loading mould adopts polytetrafluoroethylene (PTFE) to make, and described cushion 300 adopts PDMS (dimethyl silicone polymer) to make.Polytetrafluoroethylene (PTFE) acid-fast alkali-proof, do not react with growth solution, anti-aging, do not adhere to, high temperature resistant, operating temperature can reach 250 DEG C, and owing to there being these advantages, polytetrafluoroethylene (PTFE) is suitable as growth of zinc oxide nano traditional thread binding year mould on optical fiber 400 very much.And this material of PDMS is corrosion-resistant equally, do not react with growth solution, operating temperature can reach 200 DEG C, and character is soft, can not damage optical fiber 400 as pressure pad.Get Teflon mould, then the PDMS (dimethyl silicone polymer) of reusable liquid fills with in first groove 100 on the both sides of Teflon mould, through vacuumizing, remove the bubble of the inside, heat again, become soft solid, then take out, just obtain the PDMS cushion that may be used for fixing and pressed fiber 400, shape and first groove 100 of this PDMS cushion are suitable.
Optical fiber 400 is loaded into process on Teflon mould as shown in Figures 1 to 3, first mould is kept flat, again optical fiber 400 1 one is put into mould in order, then PDMS (dimethyl silicone polymer) cushion made in advance is pressed in first groove 100 at two ends.After completing these three steps, optical fiber 400 just steadily has been fixed on mould.
The size of loading mould can design as required, the place having any to note is exactly, the position of optical fiber 400 growth of zinc oxide nano line will be placed in the second groove 200, optical fiber 400 is soared aloft, mold bottom can not be touched, so the degree of depth of depth ratio both sides first groove 100 of general second groove 200 at least want dark about 2mm, so just can effectively carry out the first step kind and keep suitable growth posture when carrying out second step.
A kind of preparation method of YAG Fiber Growth zinc oxide nanowire is also provided in the utility model, optical fiber is fixed on the above-mentioned loading mould having zinc oxide nanowire for auxiliary preparation growth by described preparation method, then adopts two one-step hydrothermals growth of zinc oxide nano line on optical fiber.Adopt above-mentioned loading mould fixed fiber, optical fiber convenient mobile and operation in each step that is clean, that grow can be made, can ensure that again optical fiber is not fractureed safely in above process, and can ensure that optical fiber ensures suitable posture obliquely in the process of developing zinc oxide, thus avoid the precipitation of the bulky grain in solution to fall optical fiber surface, hinder the growth of zinc oxide nanowire.
Particularly, the preparation method of described YAG Fiber Growth zinc oxide nanowire, can comprise the following steps:
The first step: load and clean optical fiber.
1) by optical fiber stripping coat, be loaded on described loading mould, be put in container; Add deionized water, ultrasonic cleaning, then pour out deionized water; Change absolute ethyl alcohol, ultrasonic cleaning, then pour out absolute ethyl alcohol; Change acetone, ultrasonic cleaning; By the mobile mould that loads, optical fiber is put in thermostatic drying chamber again, dry.
Second step: on optical fiber kind.
1) zinc oxide seed liquid is prepared:
The zinc acetate ethanolic solution of configuration 0.01M-0.1M, the NaOH ethanolic solution of configuration 0.03M-0.3M, then by two kinds of solution mixing; Put the solution mixed into temperature constant magnetic stirring water-bath to stir, obtain white opacity solution, leave standstill some hours, at the bottom of waiting for that large particulate matter is deposited to bottle, obtain settled solution; Irradiate settled solution with laser again, observe whether there is obvious light path by solution, if having, namely show that the seed liquor configured is colloid, and namely zinc oxide seed solution is successfully prepared containing zinc oxide crystal seed particle in solution.
Seed solution is after preparation, can not use immediately, because in solution except the zinc oxide seed of required size (tens nanometers), also have many fat persons' particle, these particle volume sizes can reach micron level, the even rank of tens microns, so seed solution is at this time muddy, if do not discharge these large-size particles from, just smooth zinc oxide seed layer can not be obtained, also the irregular of zinc oxide growth can be made, uneven.Therefore, the method by leaving standstill after preparing seed solution, makes the large-size particle in solution sink to container bottom, obtains the zinc oxide seed liquid of clarification with this.
Further, before mixing two kinds of solution, two kinds of solution are respectively charged in beaker, dissolve to fully make it, two kinds of solution are hocketed magnetic agitation and sonic oscillation, obtain uniform zinc acetate ethanol solution and NaOH ethanol solution, then both are mixed by the volume ratio of 100:30-100:52.
2) on optical fiber, Seed Layer is spread:
Loading mould will be inconjunction with through ultrasonic cleaning and dried optical fiber and slowly be immersed in zinc oxide seed liquid, then pull-up, and put the thermostatic drying chamber that temperature has been adjusted to 100 DEG C-150 DEG C into, annealing 30min-50min, repeat above-mentioned steps for several times.One deck zinc oxide seed layer is obtained like this on optical fiber.
3rd step: growth of zinc oxide nano line.
1) configure the HMTA (methenamine) of 10mM-100mM and the zinc nitrate of 10mM-100mM, be mixed to get mixed aqueous solution according to the volume ratio of 1:1, stir 30min, to ensure to mix.Loading mould is inconjunction with optical fiber and puts mixed aqueous solution into, at this moment will note the posture of the loading mould loading optical fiber, mold tilt will be loaded and place, and make be mounted with optical fiber one to face down, shown in composition graphs 4 and Fig. 5, this clearly shows optical fiber and places obliquely.Adopt this modes of emplacement, loading mould lattice can be made to keep off the sediment produced in growth course, make it can not drop on growth optical fiber surface hindering zinc oxide nanowire.After placement, then capping, puts thermostatic drying chamber into, drying box temperature is adjusted to 70-95 DEG C, keeps 0.5h-20h, then from thermostatic drying chamber, take out the solution bottle that sample fiber is housed, twist-off closure, taken out by related for mould optical fiber with tweezers, zinc oxide nanowire has grown on optical fiber.
Further, the mixed process of methenamine solution and zinc nitrate solution is specially to put two different beakers into by methenamine and zinc nitrate, add deionized water respectively again, use magnetic stirrer respectively, make it fully dissolve, and then both are mixed, finally prick upper elastic, stir 30min, to ensure that methenamine solution and zinc nitrate solution mix.
2) load the loading mould of optical fiber respectively with deionized water and absolute ethyl alcohol ultrasonic cleaning, then the loading mould loading optical fiber is put in thermostatic drying chamber, 80 DEG C-95 DEG C annealing 1.5-2 hour.
After these steps above, zinc oxide nanowire grows and completes on optical fiber.Adopt the YAG Fiber Growth zinc oxide nanowire that said method prepares, the zinc oxide nanowire of optical fiber surface is comparatively even.Therefore, also provide a kind of YAG Fiber Growth zinc oxide nanowire in the utility model, described YAG Fiber Growth zinc oxide nanowire adopts said method to be prepared from.The utility model makes optical fiber be combined with material, create a subject transboundary, the important substrate that made material many, also make optical fiber can biochemical future development in the past, at present, zinc oxide nanowire main or with conductive materials such as silicon chips for substrate, mainly make use of the electrical property of zinc oxide nanowire, even if utilize zinc oxide nanowire to the sensing of biochemical gas, be also be mapped with electricity correlative, as resistance, voltage, electric current etc.And optical fiber take light as medium, after grown one deck zinc oxide nanowire, can to biochemical gas sensing, what be mapped is exactly the amount with optical correlation, as phase place, wavelength, energy etc.Than electricity advantageously, as precision is higher, anti-interference is higher for the amount of optical correlation, and the scope of application is stronger, as being exactly preferably prove in oil field, also has the transmission bandwidth that electricity is incomparable.
Below by way of specific embodiment, the utility model is described further.
The loading mould adopted in the present embodiment is a rectangle platy structure, and long is 80.00mm, and width is 40.00mm, and thickness is 15.00mm; First slot of the first groove and the degree of depth of the second slot are 8.00mm, and often end is provided with four the first slots, and its width is 1.50mm, is spaced apart 6.00mm between every two the first slots; The width of the second slot is 30.00mm, and length is 15.00mm; The length of the second groove is 40.00mm, and width is 30.00mm, and the degree of depth is 10.00mm.
The first step: load and clean optical fiber.
1) by optical fiber stripping coat, be loaded on described loading mould, be put in beaker, then add deionized water, ultrasonic cleaning 10 minutes, then pour out deionized water, change absolute ethyl alcohol, ultrasonic cleaning 10 minutes, pour out absolute ethyl alcohol again, change acetone, ultrasonic cleaning 10 minutes.By the mobile mould that loads, optical fiber is put in thermostatic drying chamber again, be adjusted to 80 DEG C, dry half clock.Second step: on optical fiber kind.
1) zinc oxide seed liquid is prepared:
Take the zinc acetate ethanolic solution of 0.0954g zinc acetate preparation 52ml, 0.01M with assay balance, the NaOH taking 0.1200g with assay balance makes 100ml, the NaOH ethanolic solution of 0.03M.Two kinds of solution are respectively charged in beaker, beaker mouth is sealed with preservative film, rubber band on bundle, stir with magnetic stirrer respectively again, dissolve to fully make it, after stirring for 5 min, stop stirring, put solution into supersonic cleaning machine, ultrasonic 5min, impel bulky grain medicine to be broken into granule, and then magnetic agitation 5min, hocketed by magnetic agitation and sonic oscillation, obtain uniform zinc acetate ethanol solution and NaOH ethanol solution, then both are mixed in the ratio of 100:52.Then the solution mixed being put into temperature constant magnetic stirring water-bath keeps 60 DEG C to stir 2 hours.Final acquisition white opacity solution, leave standstill some hours, at the bottom of waiting for that large particulate matter is deposited to bottle, obtain settled solution, then irradiate settled solution with laser, observe and whether have obvious light path to pass through solution, if have, namely show that the seed liquor configured is colloid, and namely zinc oxide seed solution is successfully prepared containing zinc oxide crystal seed particle in solution.
2) on optical fiber, Seed Layer is spread:
To be inconjunction with loading mould through ultrasonic cleaning and dried optical fiber and slowly be immersed in zinc oxide seed liquid, then pull-up, put the thermostatic drying chamber that temperature has been adjusted to 150 DEG C into, annealing 30min, repeats above-mentioned steps five times.One deck zinc oxide seed layer is obtained like this on optical fiber.3rd step: growth of zinc oxide nano line.
1) HMTA (methenamine) of 0.2804g is taken with assay balance, the zinc nitrate of 0.5950g, put two different beakers into, add 100ml deionized water respectively again, use magnetic stirrer respectively, make it fully dissolve, then both are mixed, obtain 10mMHMTA and the 10mM zinc nitrate mixed aqueous solution of 200ml, stir 30min, to ensure to mix.Loading mould is inconjunction with the aqueous solution that mixing put into by optical fiber, mold tilt will be loaded place, and make be mounted with optical fiber one to face down, make loading mould energy lattice keep off the sediment produced in growth course, make it can not drop on growth optical fiber surface hindering zinc oxide nanowire.After placement, then capping, puts thermostatic drying chamber into, drying box temperature is adjusted to 95 DEG C, keeps 80min, then from thermostatic drying chamber, take out the solution bottle that sample fiber is housed, twist-off closure, taken out by related for mould optical fiber with tweezers, zinc oxide nanowire has grown on optical fiber.
2) use deionized water and absolute ethyl alcohol ultrasonic cleaning sample 10min respectively, then sample is put in thermostatic drying chamber, anneal 1.5 hours for 80 DEG C.
After these steps above, zinc oxide nanowire grows and completes on optical fiber.
Should be understood that; application of the present utility model is not limited to above-mentioned citing; for those of ordinary skills, can be improved according to the above description or convert, all these improve and convert the protection domain that all should belong to the utility model claims.
Claims (3)
1. for a loading mould for auxiliary preparation YAG Fiber Growth zinc oxide nanowire, it is characterized in that, the two ends of described loading mould are respectively arranged with the first groove for optical fibre end; The corresponding cushion be provided with for optical fiber being fixed on loading mould on first groove, described cushion is for being removably fixed in the first groove; The middle part of described loading mould is provided with for the second groove for YAG Fiber Growth zinc oxide nanowire slot milling, and the second groove is arranged between two first grooves, and the degree of depth of the second groove is greater than the degree of depth of the first groove.
2. loading mould according to claim 1, it is characterized in that, described first groove comprises first slot suitable with optical fiber width being separately positioned on the first groove two ends, and the second slot be arranged between slot, two ends first, second slot communicates with first slot at two ends, and the degree of depth is identical; Cushion is removably fixed in the second slot.
3. loading mould according to claim 1 and 2, is characterized in that, described loading mould adopts polytetrafluoroethylene (PTFE) to make, and described cushion adopts dimethyl silicone polymer to make.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104944365A (en) * | 2015-06-30 | 2015-09-30 | 深圳大学 | Optical fiber growth zinc oxide nano wire as well as preparation method and containing mold thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104944365A (en) * | 2015-06-30 | 2015-09-30 | 深圳大学 | Optical fiber growth zinc oxide nano wire as well as preparation method and containing mold thereof |
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