CN109926597B - Method for preparing tin nanosheet by oil bath heating - Google Patents
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Abstract
Disclosed herein is a method for preparing tin nanoplatelets by oil bath heating, which belongs to the field of electronic circuits and catalytic materials. The method comprises the steps of firstly preparing the tin nanowire with uniform and controllable size by an electrodeposition method, then placing the tin nanowire in polydimethylsiloxane or liquid paraffin solvent, heating in an oil bath, and fully cleaning to obtain the tin nanosheet. The preparation method of the tin nanosheet is novel in concept, and the prepared nanosheet is stable in tissue performance, high in electric conductivity and thermal conductivity and capable of being used as a raw material for preparing a nano solder or a tin dioxide catalyst. Tin nanotopography can also be an important component of nanoscale interconnects in circuit technology because of its low cost, low melting point, good solderability and mechanical properties.
Description
Technical Field
The invention relates to the technical field of electronic circuits and catalytic materials, in particular to a method for preparing a tin nanosheet through oil bath heating.
Background
The nanometer technology is a new comprehensive scientific technology, and as people carry out deep research on macroscopic objects and microscopic basic particles, the chemical compositions of the macroscopic objects and the microscopic basic particles are the same, but the properties of the macroscopic objects and the microscopic basic particles are greatly different, and the substances in the nanometer transition state and the substances in the macroscopic state have very large differences in the aspects of electronic properties, surface properties and the like, a new subject-nanometer scientific technology is immediately made. Specific nanostructures such as nanowires, nanorods, nanoplatelets, nanocomposites, etc., are well known. These materials have been successfully synthesized and characterized by self-assembly and directed assembly. However, the broader use of nanomaterials in the field of industrial manufacturing is far from mature. The nano-sheet, the nano-wire and the nano-ball have great application value in the fields of electronic circuits and catalytic materials. In nanoelectronics, nanoelectromechanical systems (NEMS) and nanophotonics, forming a robust interconnect with good mechanical, thermal and electrical properties is one of the key requirements. Among the methods for forming a robust interconnection for functional devices, soldering should be one of the most widely used methods, and numerous studies have shown that nanoscale soldering of nano solder particles has very high operability, and interconnection of materials at a nanoscale can be achieved from the perspective of experimental design; in the field of catalytic materials, catalysts in industrial production have the advantages of large surface area, good stability, high activity and the like, and nano materials just meet the characteristics. Compared with the conventional catalyst, the catalyst prepared by the nano material has higher catalytic efficiency and selectivity, better effect and easy realization of large-scale application, so the development of the nano material catalyst is very necessary.
Tin is used as a traditional metal material, mainly for producing tin compounds and chemicals. Inorganic compounds of tin are mainly used as catalysts, stabilizers, additives and emulsifiers in the ceramic industry. Tin dioxide can also be used as a catalyst for preventing air pollution, for example, the toxic carbon monoxide gas often contained in automobile exhaust gas, which can be largely converted into carbon dioxide at 300 ℃ under the catalysis of tin dioxide. The metal alloy of tin can be used as the main component of the traditional brazing material, and the nano-form material of the tin also has the advantages of low cost, low melting point, good welding capability and mechanical property and excellent wettability with a metal matrix. In the field of nano welding, the tin nanowire, the tin nanosheet and the alloy thereof have wide application prospects.
Disclosure of Invention
The invention aims to provide a method for preparing a tin nanosheet by oil bath heating, which comprises the steps of directionally growing a tin nanowire on a substrate with a prepared through hole by using a direct current electroplating means, and converting the nanowire into the tin nanosheet by the oil bath heating method.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a method for preparing a tin nano-sheet by oil bath heating always comprises the steps of firstly preparing a tin nano-wire in a porous template by adopting direct current electrodeposition, and then placing the obtained tin nano-wire in polydimethylsiloxane or liquid paraffin solvent for oil bath heating to uniformly disperse the nano-wire in the solvent; and then fully cleaning to obtain the tin nano-sheet.
When the tin nanowire is prepared, firstly, a silver seed layer is prepared at the bottom of the porous template, then the silver seed layer is used as a cathode, pure tin is used as an anode, the silver seed layer at the bottom of the template is gradually filled upwards by adopting a direct current deposition method, and finally the tin nanowire grows. The length of the tin nanowires is regulated by controlling the current and/or deposition time.
The preparation of the tin nanowire specifically comprises the following steps:
(1) preparing a silver seed layer on one surface of the porous template (the bottom surface of the template) by a magnetron sputtering method; in the magnetron sputtering process, the power is 40-80 KW, and the sputtering time is 10-30 min; the thickness of the prepared silver seed layer is 300-1000 nm;
(2) preparing electroplating solution of a tin methane sulfonate system, wherein the components of the electroplating solution comprise methane sulfonic acid, tin methane sulfonate, gelatin, polyethylene glycol, ascorbic acid and deionized water;
(3) d, direct current electrodeposition: the current density is 5-50 mA/cm2The deposition time is 3-20 min;
(4) and after the electrodeposition is finished, taking down the template, fully cleaning the template by using acetone, and sequentially placing the template in nitric acid and sodium hydroxide solution to remove the seed layer and the template to obtain the sodium hydroxide solution containing the tin nanowires.
(5) And (5) placing the sodium hydroxide solution containing the tin nano-wire prepared in the step (4) in a centrifuge for repeated centrifugation, shaking and cleaning to obtain a clean tin nano-wire, and storing the clean tin nano-wire in alcohol for later use.
The oil bath heating process comprises the following steps: slowly dripping alcohol containing tin nanowires into a beaker filled with polydimethylsiloxane or liquid paraffin solvent; then placing the mixture in a vacuum drying oven, heating and drying at 60-70 ℃, and after the alcohol is completely evaporated, repeatedly stirring and ultrasonically vibrating to uniformly disperse the nanowires in the solvent; and (3) placing the beaker with the dispersed nanowires in an oil bath pot, heating to 250-300 ℃ under the stirring condition, preserving the heat for 4-12 hours, and taking out to obtain the mixed liquid of the nanowires and the solvent.
And (3) repeatedly centrifuging and ultrasonically vibrating and cleaning the mixed liquid of the nanowire and the solvent obtained after heating by using cyclohexane or acetone to obtain a clean tin nanosheet, and storing for later use.
Compared with the prior art, the invention has the beneficial effects that:
1. the tin nanosheet is prepared by an oil bath heating method, wherein in the preparation process, a tin nanowire is filled from the bottom of an anodic aluminum oxide template by an electrodeposition method, and then the nanowire is converted into the tin nanosheet by the oil bath heating method; tin nanowires with different lengths can be prepared by controlling the current density and time of electrodeposition, and then the scale of the nanosheets is controlled in subsequent heating.
2. The method has the advantages of wide raw material source, simple process, low cost, high process repeatability, no generation of any toxic and harmful gas and low environmental pollution.
3. The direct current electrodeposition and oil bath heating process adopted by the invention is compatible with the existing microelectronic packaging and catalytic material preparation technology, has wide application prospect in preparing nano interconnection materials and catalytic materials, and the achievement of the invention is easy to realize industrialization.
4. The tin nanosheet prepared by heating the nanowire in the oil bath can be used as a raw material of tin dioxide and other tin-based catalysts in the field of catalytic materials and used for preparing nano material catalysts. In the field of low-melting-point nano solder, the tin nanosheet can be further used as a reinforcing phase and a filling phase of the solder paste, so that the tin nanosheet has great significance for wider application of tin-based materials in the industrial field.
Drawings
FIG. 1 is a schematic view of the process of example 1 for preparing tin nanoplatelets by heating in a tin nanowire oil bath.
FIG. 2 is a schematic view of a tin nanowire obtained by fully cleaning after electrodeposition according to the present invention; wherein: (a) a microscopic topography map of a plurality of tin nanowires, and (b) a high-power topography map of a single tin nanowire.
FIG. 3 shows a tin nanosheet of the present invention after the tin nanowire has been heated in an oil bath and then thoroughly washed with acetone. Wherein: (a) is a micro-topography map of a plurality of tin nanoplates; (b) is a high-power tin nanosheet morphology map; (c) is a topographic map of the appearance of a portion of the tin nanospheres.
Figure 4 is an EDS elemental identification and composition profile of tin nanoplatelets.
Detailed Description
The invention is described in detail below with reference to the accompanying drawings and examples.
The invention is a method for preparing tin nano-sheets by oil bath heating, firstly preparing tin nano-wires by a direct current deposition method, gradually filling the tin nano-wires by a silver seed layer at the bottom of a template under the action of a direct current power supply, and finally growing the tin nano-wires; then the nano wire is converted into a tin nano sheet by an oil bath heating method; the method specifically comprises the following steps:
(1) preparing a silver seed layer: preparing a silver seed layer on one side (bottom surface) of a bi-pass anodic aluminum oxide template by a magnetron sputtering method, fixing the template on a silicon wafer, and sputtering for 10-30 min at a sputtering rate of 40-80 KW, wherein the thickness of the prepared silver seed layer is about 300-1000 nm.
(2) Preparing the electroplating solution of a methane sulfonic acid tin system, wherein the main components of the electroplating solution comprise methane sulfonic acid, methane sulfonic acid tin, gelatin, polyethylene glycol, ascorbic acid, deionized water, a flatting agent and the like.
(3) Fixing the AAO template on a copper sheet for electrodeposition, wherein the current density is 5-50 mA/cm2And preparing the tin nanowire within 3-20 min.
(4) And after the electrodeposition is finished, taking down the template, fully cleaning the template by using acetone, and sequentially placing the template in nitric acid and sodium hydroxide solution to remove the seed layer and the template to obtain the sodium hydroxide solution containing the tin nanowires.
(5) And (5) placing the tin nano wire prepared in the step (4) in a centrifuge for repeated centrifugal vibration cleaning to obtain a clean tin nano wire, and storing the clean tin nano wire in alcohol for later use.
(6) The alcohol solution containing tin nanowires was slowly added dropwise to polydimethylsiloxane or liquid paraffin. And then placing the mixture in a vacuum drying oven for heating and drying, and after the alcohol is completely evaporated, repeatedly stirring and ultrasonically vibrating to uniformly distribute the nanowires in the solvent. And (3) placing the beaker with the dispersed nanowires in an oil bath pot, heating to 250-300 ℃ under a stirring state, and taking out after heat preservation for 4-12 hours.
Example 1:
FIG. 1 is a schematic view showing a process of preparing tin nanosheets by heating tin nanowires through an oil bath. The process comprises the following steps:
(1) a nano-porous polycarbonate film or an anodic aluminum oxide film (AAO) is used as a template, a silver seed layer is prepared on one side of a double-pass anodic aluminum oxide template through a magnetron sputtering method, the sputtering power is 40-80 KW, the magnetron sputtering time is 15min, and the thickness of a sputtering layer is about 850 nm. And placing the template subjected to magnetron sputtering in vacuum for storage, and reducing the oxidation of the silver film in the air.
(2) Preparing a methane sulfonic acid tin system electroplating solution: weighing 3g of gelatin by using a tray balance, adding 120ml of deionized water, covering a preservative film, placing the preservative film in a magnetic stirrer, and keeping the temperature at 60-70 ℃ until the gelatin is completely dissolved into light yellow liquid for later use; adding 70ml of deionized water into a beaker, measuring 60ml of methanesulfonic acid with the purity of 99.5% by using a measuring cylinder, slowly dropping the methanesulfonic acid into the water under the stirring state, and uniformly stirring for later use; adding 20ml of deionized water into a beaker, weighing 0.06g of ascorbic acid, adding the ascorbic acid into the beaker, dripping 4.5ml of 38 wt.% formaldehyde solution and 0.5ml of cinnamaldehyde under the stirring state, adding 30ml of polyethylene glycol and 15ml of prepared gelatin solution after uniformly mixing, and uniformly stirring for later use; slowly dropping the prepared cinnamaldehyde solution into the methanesulfonic acid solution, then adding 27ml tin methanesulfonate, finally adding deionized water to fix the volume to 450ml, and performing an electrodeposition experiment after uniformly stirring.
(3) Fixing the template on the copper sheet by taking copper as a bottom plate at the bottom end of the through hole, taking a conductive silver seed layer as a cathode and pure tin as an anode, filling a tin nanowire from the bottom of the silver seed layer upwards by adopting a direct current deposition method, and adopting 50mA/cm during electrodeposition2The deposition time was 8 min.
(4) After the electrodeposition is completed, the template is taken off and washed with acetone for many times. Then the anode alumina template is cleaned and placed in nitric acid of 6mol/L to dissolve the silver seed layer. And after the silver seed layer is completely dissolved, repeatedly cleaning the anodic aluminum oxide template by using deionized water. Placing the template with the silver film dissolved in a prepared 6mol/L sodium hydroxide solution to dissolve the template, and adding benzotriazole with a certain mass fraction to protect the tin nanowire from being corroded when preparing the sodium hydroxide solution; when the polycarbonate template is adopted to prepare the tin nanowire, the template is taken down and cleaned after electrodeposition, and the tin nanowire is placed in nitric acid to dissolve away the silver seed layer. After repeated washing of the template with deionized water, the polycarbonate template was dissolved with methylene chloride, releasing the tin nanowires. The sodium hydroxide solution containing the tin nanowire is placed in a centrifuge, repeated centrifugal cleaning and solution replacement are carried out under the condition of 10000-rotation centrifugal rotating speed, and the figure 2 is a figure of the macroscopic appearance and single appearance of the nanowire.
(5) Putting the cleaned tin nanowires into alcohol to prepare turbid liquid, taking a beaker, adding polydimethylsiloxane or liquid paraffin into the beaker, slowly dropwise adding the turbid liquid on the surface layer of the polydimethylsiloxane or liquid paraffin oil, then putting the beaker into a vacuum drying oven, and drying at 60-70 ℃ for 30min and taking out the beaker. The beaker is repeatedly placed in a magnetic stirrer and an ultrasonic cleaner for stirring and oscillation, so that the nanowires are uniformly distributed in the polydimethylsiloxane or the liquid paraffin before being heated, and the agglomeration of the nanowires is reduced as much as possible.
(6) Placing the polydimethylsiloxane or the liquid paraffin with the uniformly distributed nanowires in a magnetic stirring oil bath heating pot, heating to 280 ℃, keeping the temperature for 8 hours under the stirring state, greatly reducing the liquid in a beaker during the heating process, and adding a proper amount of polydimethylsiloxane or liquid paraffin.
(7) After heating, the beaker is taken out, cyclohexane or acetone is adopted for repeated centrifugal cleaning, the tin nanosheet shown in fig. 3 is prepared, the nanosheets are uniform in shape and large in specific surface area, part of the nanosheets can be gradually transformed into nanosphere shapes, and fig. 4 shows EDS identification and component distribution of the tin nanosheets prepared in the embodiment.
Claims (5)
1. A method for preparing tin nano-sheets by oil bath heating is characterized in that: firstly, preparing a tin nanowire in a porous template by adopting direct current electrodeposition, and then placing the obtained tin nanowire in polydimethylsiloxane or liquid paraffin solvent for oil bath heating to uniformly disperse the nanowire in the solvent; then fully cleaning to obtain the tin nano-sheets;
when preparing the tin nanowire, firstly preparing a silver seed layer at the bottom of the porous template, then gradually filling the silver seed layer at the bottom of the template upwards by adopting a direct current deposition method by taking the silver seed layer as a cathode and pure tin as an anode, and finally growing the tin nanowire;
the oil bath heating process comprises the following steps: slowly dripping alcohol containing tin nanowires into a beaker filled with polydimethylsiloxane or liquid paraffin solvent; then placing the mixture in a vacuum drying oven for heating and drying, and after the alcohol is completely evaporated, repeatedly stirring and ultrasonically vibrating to uniformly disperse the nanowires in the solvent; and (3) placing the beaker with the dispersed nanowires in an oil bath pot, heating to 250-300 ℃ under the stirring condition, preserving the heat for 4-12 hours, and taking out to obtain the mixed liquid of the nanowires and the solvent.
2. The method for preparing tin nanoplatelets by oil bath heating according to claim 1, wherein: the length of the tin nanowires is regulated by controlling the current and/or deposition time.
3. The method for preparing tin nanoplatelets by oil bath heating according to claim 1, wherein: the preparation of the tin nanowire comprises the following steps:
(1) preparing a silver seed layer at the bottom of the porous template by a magnetron sputtering method;
(2) preparing electroplating solution of a tin methane sulfonate system, wherein the components of the electroplating solution comprise methane sulfonic acid, tin methane sulfonate, gelatin, polyethylene glycol, ascorbic acid and deionized water;
(3) d, direct current electrodeposition: the current density is 5-50 mA/cm2The deposition time is 3-20 min;
(4) after the electrodeposition is finished, taking down the template, fully cleaning the template by using acetone, and sequentially placing the template in nitric acid and sodium hydroxide solution to remove the seed layer and the template to obtain sodium hydroxide solution containing the tin nanowires;
(5) and (5) placing the sodium hydroxide solution containing the tin nano-wire prepared in the step (4) in a centrifuge for repeated centrifugation, shaking and cleaning to obtain a clean tin nano-wire, and storing the clean tin nano-wire in alcohol for later use.
4. The method for preparing tin nanoplatelets by oil bath heating according to claim 1, wherein: in the oil bath heating process, the temperature for heating and drying by using the vacuum drying oven is 60-70 ℃.
5. The method for preparing tin nanoplatelets by oil bath heating according to claim 1, wherein: and (3) repeatedly centrifuging and ultrasonically vibrating and cleaning the mixed liquid of the nanowire and the solvent obtained after heating by using cyclohexane or acetone to obtain a clean tin nanosheet, and storing for later use.
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