CN109847684B - Equipment for preparing metal oxide micro-nano array - Google Patents
Equipment for preparing metal oxide micro-nano array Download PDFInfo
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- CN109847684B CN109847684B CN201910329434.9A CN201910329434A CN109847684B CN 109847684 B CN109847684 B CN 109847684B CN 201910329434 A CN201910329434 A CN 201910329434A CN 109847684 B CN109847684 B CN 109847684B
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Abstract
The invention provides equipment for preparing a metal oxide micro-nano array. The equipment for preparing the metal oxide micro-nano array comprises a reactor, a heating device, a sample adding device, a transmission device and a two-dimensional substrate. The invention also provides a method for preparing the metal oxide micro-nano array by using the equipment. The invention can greatly improve the growth efficiency of the metal oxide micro-nano array on the two-dimensional substrate, save production procedures, improve the consistency of products and further reduce the production cost of the products.
Description
Technical Field
The invention relates to the technical field of materials, in particular to equipment for preparing a metal oxide micro-nano array.
Background
The metal oxide has wide application in the related fields of environmental protection, energy regeneration and storage and the like due to the excellent oxidation-reduction property, and the oxidation-reduction property of the metal oxide can be effectively enhanced by manufacturing the metal oxide into a micro-nano array with ordered microcosmic appearance. The metal oxide micro-nano array can grow on various two-dimensional substrates such as carbon foam, nickel foam, copper foam, aluminum foil paper and the like through low-temperature hydrothermal reaction.
Currently, in the prior art, as shown in fig. 1, an apparatus 100 for preparing a metal oxide micro-nano array generally includes a reactor 101, a heating stage 102, a substrate 103, and a reaction solution 104 disposed in the reactor 101. The preparation method mainly adopts a batch method to carry out low-temperature hydrothermal synthesis of the metal oxide micro-nano array, and the main process is that precursors (usually salts such as nitrate, sulfate, acetate, chlorate and the like) of each element are dissolved in solvents such as water and the like according to the element molar ratio required by the synthesized oxide, then a substrate 103 is immersed in a prepared reaction solution 104, hydrothermal reaction is excited by heating, finally the metal oxide micro-nano array growing on the surface of the substrate 103 is obtained, after the reaction, the substrate 103 is taken out, then the reaction solution 101 and the substrate 103 in the reactor 101 are replaced, and the next batch of preparation is carried out.
However, before each batch of reaction, fresh reaction solution and substrate need to be replaced, the steps are complex, and when the large-scale production needs to be carried out, a feasible method only enlarges the size of the reactor or increases the number of the reactors in parallel, which is not advantageous in terms of production efficiency or production cost, and the metal oxide micro-nano arrays grown in different batches are difficult to achieve high consistency.
Disclosure of Invention
The invention provides equipment for preparing a metal oxide micro-nano array, which can effectively solve the problems.
The invention is realized by the following steps:
an apparatus for preparing a metal oxide micro-nano array, comprising:
a reactor, wherein a reaction solution is contained in the reactor;
the heating device is arranged below or on the side of the reactor;
the sample adding device is arranged above the reactor;
the transmission device comprises an initial rolling shaft, a tail end rolling shaft and at least one first rolling shaft, the initial rolling shaft is arranged at the starting point of the transmission device, the tail end rolling shaft is arranged at the terminal point of the transmission device, the initial rolling shaft and the tail end rolling shaft are arranged outside the reactor, and the at least one first rolling shaft is arranged inside the reactor; and
the two-dimensional substrate is wound on the surface of the initial roller, the two-dimensional substrate is provided with a first end and a second end which are opposite to each other, the first end of the two-dimensional substrate is wound and fixed on the surface of the initial roller, the second end of the two-dimensional substrate is fixed on the surface of the tail end roller, and the two-dimensional substrate is sequentially connected with the initial roller, the at least one first roller and the tail end roller.
As a further improvement, the transmission device comprises a second roller and a third roller, and the second roller and the third roller are fixedly arranged at the upper end of the side wall of the reactor.
As a further improvement, the two-dimensional substrate is connected to the initial roller, the second roller, the at least one first roller, the third roller, and the end roller in sequence.
As a further improvement, the number of the first rollers is an odd number.
As a further improvement, the first rollers are spaced in two upper and lower rows in the reactor, and the number of the first rollers in the upper row is one less than that of the first rollers in the lower row.
As a further improvement, the upper row of first rollers and the lower row of first rollers are arranged in a staggered manner.
As a further improvement, the two-dimensional substrate forms a V-shape or a pattern formed by connecting a plurality of V-shapes in the reactor.
As a further improvement, the equipment for preparing the metal oxide micro-nano array comprises a concentration meter, and the concentration meter is arranged in the reactor.
As a further improvement, the sample adding device is an automatic sample adding device, the equipment for preparing the metal oxide micro-nano array comprises a controller, and the automatic sample adding device and the concentration meter are respectively connected with the controller.
The invention has the beneficial effects that: firstly, the metal oxide micro-nano array is prepared by adopting a rolling method, so that a substrate can be continuously immersed into a reaction solution on one hand, and the substrate with a product growing on the surface can be pulled out at the same speed on the other hand, and the substrate does not need to be replaced regularly; secondly, continuously injecting solute required by the reaction into the reaction solution to maintain the concentration of the reaction solution in a constant range without replacing fresh reaction solution regularly; thirdly, the growth rate of the metal oxide micro-nano array is in direct proportion to the concentration of the reaction solution, and the solute in the reaction solution is continuously supplemented, so that the growth rate of the micro-nano array can be maintained at a high level, the time required by production can be greatly shortened, and the production efficiency can be improved; fourthly, in the process of preparing the metal oxide micro-nano array, the substrate and the fresh reaction solution do not need to be replaced regularly, the production process can be saved, the consistency of products is improved, the production cost of the products is further reduced, and meanwhile, the metal oxide micro-nano array can grow continuously in a large scale.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are required to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
Fig. 1 is a schematic structural diagram of an apparatus for preparing a metal oxide micro-nano array in the prior art.
Fig. 2 is a schematic structural diagram of an apparatus for preparing a metal oxide micro-nano array according to a first embodiment of the present invention.
FIG. 3 is a schematic view of the arrangement of the first rollers in the reactor according to the first embodiment of the present invention.
FIG. 4 is a schematic diagram illustrating a connection relationship among a concentration meter, a sample adding device and a controller according to a first embodiment of the present invention.
Fig. 5 is a schematic structural diagram of an apparatus for preparing a metal oxide micro-nano array according to a second embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the embodiments of the present invention will be described clearly and completely with reference to the accompanying drawings of the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all embodiments of the present invention. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention. Thus, the following detailed description of the embodiments of the present invention, presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
In the description of the present invention, the terms "first" and "second" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implying any number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.
Referring to fig. 1, a first embodiment of the present invention provides an apparatus 200 for preparing a metal oxide micro-nano array. The apparatus 200 for preparing a metal oxide micro-nano array includes:
a reactor 201, wherein a reaction solution 2011 is contained in the reactor 201;
a heating device 202, wherein the heating device 202 is arranged below or on the side of the reactor 201;
the sample adding device 203 is arranged above the reactor 201;
a driving device 204, wherein the driving device 204 includes an initial roller 2041, a terminal roller 2042 and at least one first roller 2043, the initial roller 2041 is disposed at a beginning of the driving device 204, the terminal roller 2042 is disposed at an end of the driving device 204, the initial roller 2041 and the terminal roller 2042 are disposed outside the reactor 201, and the at least one first roller 2043 is disposed inside the reactor 201; and
a two-dimensional substrate 205, the two-dimensional substrate 205 is wound on the surface of the initial roller 2041, the two-dimensional substrate 205 has two opposite ends, which are respectively defined as a first end and a second end, the first end of the two-dimensional substrate 205 is fixedly wound on the surface of the initial roller 2041, the second end of the two-dimensional substrate is fixed on the surface of the terminal roller 2041, and the two-dimensional substrate is sequentially connected to the initial roller 2041, the at least one first roller 2043 and the terminal roller 2042.
Specifically, the reaction solution 2011 within the reactor 201 includes a solvent, and metal oxide precursors and other additives dissolved in the solvent. The solvent may be water or an organic solvent, etc. The metal element in the metal oxide may be magnesium (Mg), calcium (Ca) or some series of transition metal elements, such as titanium (Ti), vanadium (V), manganese (Mn), iron (Fe), cobalt (Co), nickel (Ni), copper (Cu), zinc (Zn), etc. The metal oxide precursor is typically a salt, such as a nitrate, sulfate, acetate, chlorate, or the like. The additive is a necessary auxiliary material for promoting the growth of the metal oxide micro-nano array; the additive can be acid, such as hydrochloric acid, sulfuric acid or nitric acid, or a material which generates alkaline substances after hydrolysis, such as ammonia, urea, hexamethylene tetramine and the like. The concentration of the metal oxide precursor is 0.2-1 mol/L. The concentration of the additive is also 0.2 mol/L-1 mol/L. In one example, 0.25 mole of zinc salt and 0.25 mole of hexamethylene tetramine are added to 1 liter of deionized water.
The heating device 202 may be disposed below the reactor 201. Alternatively, the heating device 202 is disposed on a side of the reactor 201. When the heating device 202 is disposed at the side of the reactor 201, the heating device 202 may be disposed around the sidewall of the reactor 201, so that the reaction solution 2011 in the reactor 201 may be uniformly heated. Alternatively, the heating device 202 may be disposed below and at the side of the reactor 201.
In the driving device 204, the initial roller 2041, the end roller 2042, and the at least one first roller 2043 are connected by the two-dimensional substrate 205, and the at least one first roller 2043 is located between the initial roller 2041 and the end roller 2042. A two-dimensional substrate on which no metal oxide micro-nano array grows is wound on the surface of the initial roller 2041. The end roller 2042 is used for collecting the two-dimensional substrate on the surface of which the metal oxide micro-nano array grows. The number and the arrangement of the first rollers 2043 are not limited, preferably, the number of the first rollers 2043 is odd, when the number of the first rollers 2043 is greater than 1, the first rollers 2043 form two upper rows and two lower rows spaced apart in the reactor 201, and the number of the first rollers in the lower row is one more than that of the first rollers in the upper row. More preferably, referring to fig. 3, the upper row of first rollers and the lower row of first rollers are arranged in a staggered manner.
The two-dimensional substrate 205 sequentially fits around the initial roller 2041, the at least one first roller 2043, and the end roller 2042 to connect the initial roller 2041, the at least one first roller 2043, and the end roller 2042. The two-dimensional substrate 205 forms a "V" or a pattern of connected "V" shapes within the reactor 201. The material of the two-dimensional substrate 205 is not limited, and specifically, the material may be carbon foam, nickel foam, copper foam, aluminum foil paper, or the like. The length and width of the two-dimensional substrate 205 are not limited, and a two-dimensional substrate 205 with a suitable length and width can be selected according to actual requirements, and a roller with a suitable size can be selected according to the width of the two-dimensional substrate 205.
Further, the apparatus 200 for preparing a metal oxide micro-nano array may include a concentration meter 206. The concentration meter 206 is provided in the reaction solution 2011 in the reactor 201, and the concentration meter 206 detects the concentration of the reaction solution 2011, and can determine the amount of the substance to be added to the reaction solution 2011 based on data detected by the concentration meter 206. Further, when the sample adding device 203 is an automatic sample adding device, the apparatus 200 for preparing a metal oxide micro-nano array may further include a controller 207. Referring to fig. 4, the controller 207 is connected to the concentration meter 206 and the sample adding device 203, respectively. The concentration meter 206 transmits the detected concentration signal to the controller 207. The controller 207 instructs the sample adding device 203 to increase or decrease the sample adding amount according to the received concentration signal. Therefore, the concentration of the reaction solution can be controlled more accurately, the concentration of the reaction solution is kept consistent all the time, and the prepared metal oxide micro-nano array has high consistency.
Further, the apparatus 200 for preparing a metal oxide micro-nano array may further include a stirring device (not shown), and the stirring device may include a stirring paddle, and the stirring paddle is disposed in the reaction solution 2011 of the reactor 201. The stirring device is used for stirring the reaction solution 2011, so that the reaction substances are uniformly distributed and uniformly contacted with the two-dimensional substrate 205, and the prepared metal oxide micro-nano array has high consistency.
The first embodiment of the present invention further includes a method for preparing a metal oxide micro-nano array using the apparatus for preparing a metal oxide micro-nano array 200, which includes the steps of:
step one, starting the heating device 202 to heat the reaction solution 2011 in the reactor 201;
secondly, starting the transmission device 204 to move the two-dimensional substrate 205;
adding a reaction substance into the reaction solution through the sample adding device 203 according to the change of the concentration of the reaction solution;
and step four, collecting the two-dimensional substrate with the metal oxide micro-nano array growing on the surface by a tail end roller of the transmission device 204.
The first to fourth steps will be described in detail below.
In step one, the heating device 202 is started to heat the reaction solution 2011 in the reactor 201.
The reaction solution 2011 is heated by the heating device 202 to reach a desired reaction temperature, such as 70-90 ℃ for zinc oxide, and then the temperature is kept constant, and then the next operation is performed.
And step two, starting the transmission device 204 to move the two-dimensional substrate 205.
Starting each roller of the transmission device 204, so that the initial roller, the at least one first roller and the tail end roller rotate at a constant speed, the two-dimensional substrate 205 moves along with the rotation of each roller, and the two-dimensional substrate 205 passes through each roller and the reaction solution at a constant speed. The reaction substance in the reaction solution undergoes a hydrothermal reaction, and a metal oxide micro-nano array is generated on the surface of the two-dimensional substrate 205. The reaction time is controlled by the rotating speed of each roller, the slower the rotating speed of each roller is, the longer the time for the two-dimensional substrate to be soaked in the reaction solution is, and the longer the reaction time is, the more the metal oxide micro-nano array grows on the surface of the two-dimensional substrate. If the two-dimensional substrate 205 is driven in the reaction solution over a distance of 1 meter and the reaction time is 1 hour, the roller speed should be 1 meter/hour.
And a third step of adding a reaction substance into the reaction solution by the sample addition device 203 according to a change in the concentration of the reaction solution.
In the reaction process, according to the concentration change of the reaction solution, the reaction solute is continuously added into the reaction solution through the sample adding device so as to maintain the concentration of the reaction solution in a constant range. It is to be noted that the reaction solution may be directly added to the reaction solution; the concentration of the reaction solution may be maintained by dissolving a reaction solute in a solvent to prepare a high concentration reaction solution, and then continuously adding the high concentration reaction solution into the reaction solution, and the concentration of the high concentration reaction solution may be 12.5 mol/l to 25 mol/l.
And step four, collecting the two-dimensional substrate with the metal oxide micro-nano array growing on the surface by a tail end roller of the transmission device 204.
The end roller 2042 continuously pulls the two-dimensional substrate 205 from the reaction solution, which is continuously wound around the surface of the end roller 2042 as the end roller 2042 rotates.
The invention adopts a roll-to-roll method, the substrate is continuously immersed into the reaction solution and is pulled out at the same speed, meanwhile, the reaction solute is continuously added into the solution which is reacting to maintain the concentration of the reaction solution, and the substrate keeps the efficient growth of the micro-nano array on the substrate when passing through the reaction solution at a constant speed.
Referring to fig. 5, a second embodiment of the present invention provides a manufacturing apparatus 300 for a metal oxide micro-nano array. The apparatus 300 for preparing the metal oxide micro-nano array comprises
A reactor 301, wherein a reaction solution 3011 is contained in the reactor 301;
a heating device 302, wherein the heating device 302 is arranged below or on the side of the reactor 301;
the sample adding device 303, the sample adding device 303 is arranged above the reactor 301;
a driving device 304, the driving device 304 includes an initial roller 3041, a terminal roller 3042, at least one first roller 3043, a second roller 3044 and a third roller 3045, the initial roller 3041 is disposed at a beginning of the driving device 304, the terminal roller 3042 is disposed at an end of the driving device 304, the initial roller 3041 and the terminal roller 3042 are disposed outside the reactor 201, the at least one first roller 3043 is disposed inside the reactor 301, and the second roller 3044 and the third roller 3045 are fixedly disposed at an upper end of a sidewall of the reactor 301; and
a two-dimensional substrate 305, the two-dimensional substrate 305 is wound on the surface of the initial roller 3041, the two-dimensional substrate 305 has two opposite ends respectively defined as a first end and a second end, the first end of the two-dimensional substrate 305 is fixedly wound on the surface of the initial roller 3041, the second end of the two-dimensional substrate is fixed on the surface of the end roller 3041, and the two-dimensional substrate is sequentially connected to the initial roller 2041, the second roller 2044, the at least one first roller 2043, the third roller 2045, and the end roller 2042.
A reactor 301, a heating device 302, a sample-loading device 303, a transmission device 304 and a two-dimensional substrate 305.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (7)
1. An apparatus for preparing a metal oxide micro-nano array, comprising:
a reactor, wherein a reaction solution is contained in the reactor;
the heating device is arranged below or on the side of the reactor;
the sample adding device is arranged above the reactor;
the transmission device comprises an initial rolling shaft, a tail end rolling shaft and at least one first rolling shaft, the initial rolling shaft is arranged at the starting point of the transmission device, the tail end rolling shaft is arranged at the terminal point of the transmission device, the initial rolling shaft and the tail end rolling shaft are arranged outside the reactor, and the at least one first rolling shaft is arranged inside the reactor; and
the two-dimensional substrate is wound on the surface of the initial roller and provided with a first end and a second end which are opposite, the first end of the two-dimensional substrate is wound and fixed on the surface of the initial roller, the second end of the two-dimensional substrate is fixed on the surface of the tail end roller, and the two-dimensional substrate is sequentially connected with the initial roller, the at least one first roller and the tail end roller;
the transmission device comprises a second roller and a third roller, and the second roller and the third roller are fixedly arranged at the upper end of the side wall of the reactor;
the number of the first rollers is odd.
2. The apparatus of claim 1, wherein the two-dimensional substrate is sequentially connected to the initial roller, the second roller, the at least one first roller, the third roller, and the end roller.
3. The apparatus for preparing a metal oxide micro-nano array according to claim 1, wherein the first rollers are spaced in two rows in the reactor, and the number of the first rollers in the upper row is one less than that of the first rollers in the lower row.
4. The apparatus for preparing a metal oxide micro-nano array according to claim 3, wherein the upper row of first rollers and the lower row of first rollers are arranged in a staggered manner.
5. The apparatus for preparing a metal oxide micro-nano array according to claim 1, wherein the two-dimensional substrate forms a "V" shape or a pattern formed by connecting a plurality of "V" shapes in a reactor.
6. The apparatus for preparing a metal oxide micro-nano array according to claim 1, wherein the apparatus for preparing a metal oxide micro-nano array comprises a concentration meter, and the concentration meter is disposed in the reactor.
7. The apparatus for preparing a metal oxide micro-nano array according to claim 6, wherein the sample adding device is an automatic sample adding device, the apparatus for preparing a metal oxide micro-nano array comprises a controller, and the automatic sample adding device and the concentration meter are respectively connected to the controller.
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| WO2018226652A1 (en) * | 2017-06-05 | 2018-12-13 | Worcester Polytechnic Institute | Superhydrophobic coatings |
| CN109207958A (en) * | 2018-10-16 | 2019-01-15 | 中国地质大学（北京） | A kind of preparation method of the phosphating sludge nano-chip arrays structure perpendicular to substrate grown |
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| KR101420680B1 (en) * | 2008-09-22 | 2014-07-17 | 삼성전자주식회사 | Apparatus and method for surface treatment of carbon fiber using resistive heating |
| JP5959510B2 (en) * | 2011-06-02 | 2016-08-02 | Ｊｘ金属株式会社 | Copper foil for producing graphene and method for producing graphene |
| US9702054B2 (en) * | 2014-11-10 | 2017-07-11 | Seoul Semiconductor Co., Ltd. | Solution deposition method for forming metal oxide or metal hydroxide layer |
| CN207352983U (en) * | 2017-10-09 | 2018-05-11 | 深圳市国华光电研究院 | A kind of equipment of assemble nanometer bead |
| CN108557868A (en) * | 2018-02-09 | 2018-09-21 | 神华（北京）光伏科技研发有限公司 | Nano-structure array and preparation method thereof and device |
| CN108977846B (en) * | 2018-06-21 | 2020-02-28 | 太原理工大学 | Preparation method of iron oxide nanobelt array film |
| CN210133883U (en) * | 2019-04-23 | 2020-03-10 | 福建龙新三维阵列科技有限公司 | Equipment for preparing metal oxide micro-nano array |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104176702A (en) * | 2014-09-05 | 2014-12-03 | 苏州中科纳福材料科技有限公司 | Device for large-area quick manufacture of nanometer material orderly-assembled functional film |
| WO2018226652A1 (en) * | 2017-06-05 | 2018-12-13 | Worcester Polytechnic Institute | Superhydrophobic coatings |
| CN109207958A (en) * | 2018-10-16 | 2019-01-15 | 中国地质大学（北京） | A kind of preparation method of the phosphating sludge nano-chip arrays structure perpendicular to substrate grown |
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