CN111268731A - Preparation process of α -molybdenum oxide nanowire with high linearity and high yield - Google Patents

Preparation process of α -molybdenum oxide nanowire with high linearity and high yield Download PDF

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CN111268731A
CN111268731A CN202010182300.1A CN202010182300A CN111268731A CN 111268731 A CN111268731 A CN 111268731A CN 202010182300 A CN202010182300 A CN 202010182300A CN 111268731 A CN111268731 A CN 111268731A
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molybdenum oxide
yield
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linearity
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蒋连福
董文英
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Nanjing Beige Electronic Technology Co ltd
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Abstract

The invention discloses a preparation process of α -molybdenum oxide nanowires with high linearity and high yield, belonging to the field of nonferrous metal processing2O2In a solvent, stirring thoroughly, passing through H2O2Oxidizing high-purity molybdenum powder to prepare orange precursor solution, and then heating for 48 hours at 180 ℃ to obtain milky MoO3Finally, the nano-wire dispersion liquid is subjected to high-speed centrifugation, washing and drying to obtain a high-purity α -molybdenum oxide nano-wire sample, and meanwhile, MoO is accelerated by introducing a substrate plate3The crystal growth speed of the precursor solution provides a growth method of the α -molybdenum oxide nano-wire with the nanometer grade and linear shape.

Description

Preparation process of α -molybdenum oxide nanowire with high linearity and high yield
The invention is a divisional application, and the original application information is as follows, namely a preparation process of α -molybdenum oxide nanowires for industrial production, with the application number of 2019104703418 and the application date of 2019.05.31.
Technical Field
The invention belongs to the field of nonferrous metal processing, and particularly relates to a high-linearity high-yield α -molybdenum oxide nanowire preparation process.
Background
In recent years, many research subjects control the morphology of molybdenum oxide to excavate the potential application of increasing the performance of nano molybdenum oxide, and α -molybdenum oxide nanowire is a semiconductor material, and the wire-shaped morphology with large specific surface area can be widely applied to the fields of electrode materials of rechargeable batteries, electrode materials of super capacitors, thermoelectric materials, electrochromism and the like.
To date, molybdenum-based feedstocks have found widespread use in the petrochemical industry as a means of selectively oxidizing and cracking hydrocarbons. The shape of the nano material is a key parameter for determining the application of the nano material, and the one-dimensional nano material with large specific surface area is an ideal material for researching electricity.
The existing preparation method of the molybdenum oxide nanowire mainly comprises two preparation processes of top-down preparation and bottom-up preparation; the method is mainly used for preparing zero-dimensional nano materials, and the prepared one-dimensional nano materials have low purity, nanometer fineness and one-dimensional structural integrity and cannot meet the use requirements of the existing molybdenum oxide nanowires; preparing precursor solutions by a bottom-up process, and then spontaneously assembling the precursor solutions into nanoscale substances with certain shapes under certain chemical or physical regulation; but the crystallization yield of the molybdenum oxide nanowire is extremely low due to crystallization processes, parameters and the like. In addition, in the existing preparation processes of molybdenum oxide nanowires, researchers pay more attention to the crystallization process of molybdenum oxide, for example, the optimal reaction conditions of the molybdenum oxide self-coiling mechanism are provided by changing the hydrothermal temperature and the water bath time, optimizing the concentration of a precursor, introducing a protective gas and the like, and the crystallization yield of the molybdenum oxide nanowires is improved. Because of the research results, most of the research results are in small-batch production in a laboratory, and the yield of the crystallization means is greatly different from the small-batch production when the applicant actually uses the crystallization means to carry out large-batch production.
Disclosure of Invention
The invention aims to provide a preparation process of α -molybdenum oxide nanowires with high linearity and high yield, and provide a growth method of α -molybdenum oxide nanowires with high cost performance and high yield, which can be industrially produced and are in a nanometer and linear shape.
The technical scheme is that the preparation process of the α -molybdenum oxide nanowire with high linearity and high yield comprises the following steps:
s1, slowly adding 4 parts of high-purity molybdenum powder into 30-40 parts of H for 4-8 times2O2And 58-68 parts of purified water, and filling O in the mixed liquid2Fully stirring the mixture for 3 to 5 hours at constant temperature in a sealed reaction kettle serving as protective atmosphere to form orange precursor solution;
s2, adjusting the concentration of the orange precursor solution to 0.4-0.5 mol/L, raising the temperature of the reaction kettle to ensure that the precursor solution is at 100-200 ℃, heating for 10-100 h, and obtaining milky MoO after the reaction is finished3A nanowire dispersion;
and S3, carrying out high-speed centrifugation, washing and drying to obtain a pure α -molybdenum oxide nanowire sample.
In further embodiments, the H2O2Is an oxidation source and has the mass fraction of 30 to 100 percent.
In further implementation, in the step S1, the molybdenum powder is mixed with H2O2The molar concentration ratio of (1): (15-20).
In the further implementation process, the reaction kettle shell in the steps S1 and S2 is made of high-temperature and high-pressure resistant sealed stainless steel, and a layer of sealed polytetrafluoroethylene material is embedded in the inner layer to form a protective layer.
In further implementation, the reaction temperature in the step S2 is 180 ℃, and the heating time is 48 h.
In a further implementation, the step of S2 may further be: diluting the orange solution to a water solution with the mass concentration of 0.05g/ml, adding the diluted orange solution into a transparent glass container, then thoroughly cleaning and drying the surface of the substrate plate, stably placing the substrate plate on the liquid surface of the diluted solution, sealing the glass container, finally placing the sealed glass container into an oven, and heating for 4-20 hours at the temperature of 40-80 ℃.
In a further embodiment, the substrate plate has an area of 1X 1cm2Hollow simple substance silicon is used as a main body, and the average density of the whole body is 1 g/ml; and a copper coating with the thickness of 450-600 nm is coated on the surface of the simple substance silicon.
In a further implementation process, in the step S3, the high-speed centrifugation process specifically includes:
the method comprises the following steps: to milk white MoO3Adding ethylenediamine accounting for 0.1 percent of the total dispersion liquid mass into the nanowire dispersion liquid, and then introducing the nanowire dispersion liquid into a centrifugal tube of centrifugal separation equipment through an overflow pipe;
step two: opening the stirring device to provide centrifugal force, and rotating and centrifuging the centrifugal tube at the rotating speed of 2000-2500 r/min;
step three: centrifuging for 15-30 min, and separating out heavy-phase solid residues through a slag discharge pipeline in a centrifuge tube, wherein solid matters separated in the step are molybdenum oxide nanowires with complete crystal shapes;
step four: continuously carrying out centrifugal separation on the light phase liquid, and rotating and centrifuging at the rotating speed of 3000-4500 r/min;
step five: centrifuging for 45-60 min, and separating the heavy-phase solid residue through a residue discharge valve in a centrifuge tube, wherein the solid matter separated in the step is molybdenum oxide nanowires.
In a further implementation process, in the step S3, the washing process specifically includes:
the method comprises the following steps: transferring the separated solid molybdenum oxide nanowires into a washing container, spraying absolute ethyl alcohol washing liquid onto the coagulated solid molybdenum oxide nanowires at a high speed from a spray head, and completely scattering the blocky solid molybdenum oxide nanowires into particles by matching with a stirring device;
step two: continuously stirring for 10-15 min to form uniformly distributed heterogeneous dispersion liquid by the molybdenum oxide nanowires and the absolute ethanol washing liquid, and then filtering the dispersion liquid to obtain a molybdenum oxide nanowire filter cake through separation;
step three: repeating the first step and the second step for 1-2 times; replacing the absolute ethyl alcohol washing liquid with distilled water, and continuously repeating the first step and the second step for 2-3 times;
step four: drying the molybdenum oxide nanowire filter cake; natural air drying or drying in an oven to ensure that the drying temperature is lower than 40 ℃;
in a further implementation process, in the step S1, a temperature measuring step is further included, in which a temperature measuring device is disposed in the reaction vessel for measuring the temperature of the reaction system; after adding the molybdenum powder once, sampling once, and detecting the absorbance of the orange solution by using a spectrophotometric agent.
The invention has the beneficial effects that the invention relates to a preparation process of α -molybdenum oxide nanowires with high linearity and high yield, which is implemented by H2O2Oxidizing high-purity molybdenum powder to prepare orange precursor solution, and then heating for 48 hours at 180 ℃ to obtain milky MoO3Finally, the nano-wire dispersion liquid is centrifuged at high speed, washed and dried to obtain α -molybdenum oxide nano-wire sample with high purity, or a substrate plate is introduced to accelerate MoO3The growth speed of the precursor solution in the crystal in the vertical direction on the surface of the substrate plate provides a growth method of the α -molybdenum oxide nano-wire with the nanometer grade and linear property.
Drawings
Figure 1 is X-ray diffraction (XRD) data for α -molybdenum oxide nanowire samples obtained in example 2.
FIG. 2 is a Scanning Electron Microscope (SEM) photograph of a sample of α -molybdenum oxide nanowires obtained in example 2.
FIG. 3 is SEM-Mapping elemental distribution data for the α -molybdenum oxide nanowire sample obtained in example 2.
Fig. 4 is a Transmission Electron Microscope (TEM) photograph of α -molybdenum oxide nanowire samples obtained in example 2.
FIG. 5 shows examples 1 to 2 and other concentrations of H2O2The absorbance of the orange precursor solution obtained by the experiment is related to H2O2The change curve of the concentration.
FIG. 6 is a bar graph showing the absorbance of the precursor solutions obtained in examples 1 to 4.
FIG. 7 is a bar graph of the yield and one-dimensional structure integrity of the molybdenum oxide nanowires obtained in example 2 and examples 5-7.
Detailed Description
In the following description, numerous specific details are set forth in order to provide a more thorough understanding of the present invention. It will be apparent, however, to one skilled in the art, that the present invention may be practiced without one or more of these specific details. In other instances, well-known features have not been described in order to avoid obscuring the invention.
In order to solve the problems in the prior art, after the applicant intensively studies the preparation process of the existing molybdenum oxide nanowire, the following findings are obtained: 1. the existing preparation method of the molybdenum oxide nanowire mainly comprises two preparation processes of top-down preparation and bottom-up preparation; the method is mainly used for preparing zero-dimensional nano materials, and the prepared one-dimensional nano materials have low purity, nanometer fineness and one-dimensional structural integrity and cannot meet the use requirements of the existing molybdenum oxide nanowires; preparing precursor solutions by a bottom-up process, and then spontaneously assembling the precursor solutions into nanoscale substances with certain shapes under certain chemical or physical regulation; but the crystallization yield of the molybdenum oxide nanowire is extremely low due to crystallization processes, parameters and the like. 2. In the existing preparation process of molybdenum oxide nanowires, researchers pay more attention to the crystallization process of molybdenum oxide, for example, the optimal reaction conditions of a molybdenum oxide self-coiling mechanism are provided by means of changing the hydrothermal temperature and the water bath time, optimizing the concentration of a precursor, introducing protective gas and the like, and the crystallization yield of the molybdenum oxide nanowires is improved. 3. Because of the research results, most of the research results are in small-batch production in a laboratory, and the yield of the crystallization means is greatly different from the small-batch production when the applicant actually uses the crystallization means to carry out large-batch production.
Through analysis and comparison, the applicant gradually confirms that the crystallization force among molybdenum oxide molecules is reduced due to the interference reasons such as the purity of the precursor solution, the introduction of residual oxidant and secondary impurities, and the finished product loss is caused in the cleaning and drying processes, so that the crystallization yield of the molybdenum oxide nanowire is extremely low. The purity of the precursor solution used in small batches in a laboratory is higher, and if a laboratory purification means is adopted for amplification, the economic cost of the precursor solution is inevitably greatly improved, so that the research of finding an oxidant which has little or no influence on molybdenum oxide crystals for preparing the precursor solution becomes the key of the research.
Example 1
A preparation process of α -molybdenum oxide nanowires with high linearity and high yield comprises the following steps:
step S1, slowly adding 4 parts of high-purity molybdenum powder into 30 parts of H for 8 times2O2And 68 parts of purified water, in a mixed liquid filled with O2Opening a condensation circulating device in a sealed reaction kettle as a protective atmosphere, keeping the temperature of the reaction kettle at 25 ℃, and fully stirring for 3 hours to form an orange precursor solution;
step S2, adjusting the concentration of the orange precursor solution to 0.5mol/L, raising the temperature of the reaction kettle to ensure that the precursor solution is in a 180 ℃ condition and is in a supersaturated state, heating for 48 hours, and obtaining milky MoO after the reaction is finished3A nanowire dispersion;
and S3, after high-speed centrifugation, washing and drying to obtain a pure α -molybdenum oxide nanowire sample.
Wherein, the reaction kettle shell in the steps S1 and S2 is made of high temperature and high pressure resistant closed stainless steel, and the inner layer is embedded with a layer of closed polytetrafluoroethylene material to make a protective layer. In the step S1, a temperature measuring step is further included, in which a temperature measuring device is provided in the reaction vessel for measuring the temperature of the reaction system; after adding the molybdenum powder once, sampling once, and detecting the absorbance of the orange solution by using a spectrophotometric agent.
The high-speed centrifugation process specifically comprises the following steps:
step S301: mixing the milky white MoO3Nanowire and method of manufacturing the sameThe dispersion liquid is led into a centrifuge tube of centrifugal separation equipment through an overflow pipe;
step S302: opening the stirring device, providing centrifugal force, and rotating and centrifuging the centrifuge tube at the rotating speed of 2500 r/min;
step S303: centrifuging for 30min, and separating out heavy phase solid residue through a residue discharge pipeline in a centrifuge tube, wherein solid matters separated in the step are molybdenum oxide nanowires with complete crystal shapes;
wherein, the washing and drying process specifically comprises the following steps:
step S304: transferring the separated solid molybdenum oxide nanowires into a washing container, spraying absolute ethyl alcohol washing liquid onto the coagulated solid molybdenum oxide nanowires at a high speed from a spray head, and completely scattering the blocky solid molybdenum oxide nanowires into particles by matching with a stirring device;
step S305: continuously stirring for 15min to form uniformly distributed heterogeneous dispersion liquid by the molybdenum oxide nanowire and the absolute ethyl alcohol washing liquid, and then filtering the dispersion liquid to obtain a molybdenum oxide nanowire filter cake through separation;
step S306: replacing the absolute ethyl alcohol washing liquid with distilled water, and continuously repeating the first step and the second step;
step S307: drying the molybdenum oxide nanowire filter cake; putting the mixture into an oven for drying, and ensuring the drying temperature to be 40 ℃;
example 2
The present embodiment is different from embodiment 1 in that step S1: 4 parts of high-purity molybdenum powder are slowly added into 40 parts of H by 8 times2O2And 58 parts of purified water. The rest of the procedure was the same as in example 1.
Example 3
The present embodiment is different from embodiment 1 in that step S1: the temperature of the reaction kettle was 75 ℃. The rest of the procedure was the same as in example 1.
Example 4
The present embodiment is different from embodiment 1 in that step S1: in the reaction kettle, no O is generated2As the protective atmosphere, the reaction kettle is in an open environment. The rest of the procedure was the same as in example 1.
Example 5
The present embodiment is different from embodiment 2 in that in step S301: will turn to milky white MoO3Ethylenediamine with the amount of 0.1% of the total dispersion was added to the nanowire dispersion, and then introduced into a centrifugal tube of a centrifugal separation apparatus through an overflow pipe. The remaining steps were the same as in example 2.
Example 6
The present embodiment is different from embodiment 2 in that in step S3:
step S301: to milk white MoO3Adding ethylenediamine accounting for 0.1 percent of the total dispersion liquid mass into the nanowire dispersion liquid, and then introducing the nanowire dispersion liquid into a centrifugal tube of centrifugal separation equipment through an overflow pipe;
step S302: opening the stirring device to provide centrifugal force, and rotating and centrifuging the centrifuge tube at the rotating speed of 4500 r/min;
step S303: centrifuging for 60min, and separating out the heavy phase solid residue through a residue discharge pipeline in a centrifuge tube, wherein the solid substance separated out in the step is the molybdenum oxide nanowire with complete crystal shape.
The remaining steps were the same as in example 2.
Example 7
The present embodiment is different from embodiment 6 in that in step S304: the absolute ethanol detergent was changed to isopropanol. The remaining procedure was the same as in example 6.
Example 8
The present embodiment is different from embodiment 2 in that in step S2: diluting/purifying the orange precursor solution to a water solution with the concentration of 0.5mol/L, then thoroughly cleaning and drying the surfaces of a plurality of substrate plates, stably placing the substrate plates on the liquid level of the diluted solution, finally adjusting the temperature of the reaction kettle, and heating for 24 hours at 40 ℃. Wherein the substrate plate has an area of 1 × 1cm2Hollow simple substance silicon is used as a main body, and the average density of the whole body is 1 g/ml; a600 nm copper plating layer is plated on the surface of the simple substance silicon. The remaining steps were the same as in example 2.
The experimental results of the above examples 1 to 7 are shown in FIGS. 1 to 7; basic data such as XRD data, SEM photograph and TEM photograph data of the molybdenum oxide nanowires prepared in example 2 and example 8 are compared, and experimental data thereof are as follows:
Figure 424771DEST_PATH_IMAGE001
in summary, the embodiments described above can be combined with the accompanying drawings to obtain:
1) due to H2O2The reaction with molybdenum powder is an excess reaction with H2O2The mass concentration of the precursor solution is increased, the absorbance and the concentration of the precursor solution are gradually increased, and when the precursor solution finally reaches H2O2When the mass concentration of (2) is 40%, the absorbance and concentration of the precursor solution are gradually stabilized, and when the mass concentration is 40% H2O2The solution is already capable of providing sufficient oxidizing concentration to allow the molybdenum powder to react completely; meanwhile, the molybdenum powder is dissolved in H2O2When in use, a large amount of heat is released, and H is added step by step at a temperature of 25 DEG C2O2Synthesis of precursor solution, not only reducing H2O2The decomposition can also accelerate the reaction speed of the molybdenum powder; selecting O2As a protective atmosphere, H can be reduced2O2Decomposition of (2); and is selected from H2O2As an oxygen source, the method has almost no influence on the crystallization process of the one-dimensional nanostructure of the molybdenum oxide, and the raw material utilization rate is improved to the maximum extent and the economic cost is saved by the process. And the shell of the reaction kettle is made of high-temperature and high-pressure resistant closed stainless steel, and the inner layer is embedded with a layer of closed polytetrafluoroethylene material to make a protective layer, so that the influence of iron ions on the crystallization of the molybdenum oxide one-dimensional nanostructure is reduced.
2) By turning to milky white MoO3Ethylenediamine with the mass of 0.1 percent of the total dispersion liquid is added into the nanowire dispersion liquid to provide a weak alkaline condition, so that MoO (MoO) can be reduced to the maximum extent3Solubility in organic solvents and water reduces damage to the finished crystals during cleaning. Meanwhile, the separation efficiency and the crystal yield can be greatly improved by increasing the centrifugal power, but the one-dimensional structure of the molybdenum oxide nanowire can be damaged by excessive shearing force. It should be noted that: the washing effect of the isopropanol and the absolute ethyl alcohol is almost not muchThe cost of isopropanol is far less than that of absolute ethanol.
3) Compared with the embodiment 2 and the embodiment 8, the introduction of the substrate plate can not only greatly improve the crystal growth speed of the molybdenum oxide wire structure, but also improve the fineness of the nanowire, and simultaneously, the diameter of the molybdenum oxide nanowire is reduced, so that the increase of the wire length is limited to a certain extent, and the application performance of the molybdenum oxide nanowire in specific occasions, such as the detection sensitivity in electrochromic, can be improved due to the more refined structure.
It should be noted that the various features described in the above embodiments may be combined in any suitable manner without departing from the scope of the invention. The invention is not described in detail in order to avoid unnecessary repetition.

Claims (7)

1. A preparation process of α -molybdenum oxide nanowires with high linearity and high yield is characterized by comprising the following steps:
step S1, slowly adding 4 parts of high-purity molybdenum powder into 30-40 parts of H for 4-8 times2O2And 56-66 parts of purified water, sampling once after molybdenum powder is added once, and detecting the absorbance of the orange solution by using a spectrophotometric agent; after being filled with O2Keeping the temperature of 25 ℃ constant in a sealed reaction kettle as a protective atmosphere, and fully stirring for 3-5 h to form an orange precursor solution;
step S2, diluting the orange solution to a water solution with the mass concentration of 0.05g/ml, adding the orange solution into a transparent glass container, then thoroughly cleaning and drying the surface of the substrate plate, stably placing the substrate plate on the liquid surface of the diluted solution, sealing the glass container, finally placing the sealed glass container into an oven, and heating for 4-20 hours at the temperature of 40-80 ℃;
s3, after high-speed centrifugation, washing and drying to obtain a pure α -molybdenum oxide nanowire sample;
in step S3, the high-speed centrifugation process specifically includes:
the method comprises the following steps: to milk white MoO3Adding ethylenediamine accounting for 0.1% of the total dispersion liquid mass into the nanowire dispersion liquid, and then introducing into a centrifugal tube of centrifugal separation equipment through an overflow pipe;
step two: opening the stirring device to provide centrifugal force, and rotating and centrifuging the centrifugal tube at the rotating speed of 2000-2500 r/min;
step three: centrifuging for 15-30 min, and separating out heavy-phase solid residues through a slag discharge pipeline in a centrifuge tube, wherein solid matters separated in the step are molybdenum oxide nanowires with complete crystal shapes;
step four: continuously carrying out centrifugal separation on the light phase liquid, and rotating and centrifuging at the rotating speed of 3000-4500 r/min;
step five: centrifuging for 45-60 min, and separating the heavy-phase solid residue through a residue discharge valve in a centrifuge tube, wherein the solid matter separated in the step is molybdenum oxide nanowires;
in step S3, the washing process specifically includes:
the method comprises the following steps: transferring the separated solid molybdenum oxide nanowires into a washing container, spraying absolute ethyl alcohol washing liquid onto the coagulated solid molybdenum oxide nanowires at a high speed from a spray head, and completely scattering the blocky solid molybdenum oxide nanowires into particles by matching with a stirring device;
step two: continuously stirring for 10-15 min to form uniformly distributed heterogeneous dispersion liquid by the molybdenum oxide nanowires and the absolute ethanol washing liquid, and then filtering the dispersion liquid to obtain a molybdenum oxide nanowire filter cake through separation;
step three: repeating the first step and the second step for 1-2 times; replacing the absolute ethyl alcohol washing liquid with distilled water, and continuously repeating the first step and the second step for 2-3 times;
step four: drying the molybdenum oxide nanowire filter cake; natural air drying or drying in a drying oven is adopted, and the drying temperature is ensured to be lower than 40 ℃.
2. The high-linearity high-yield α -molybdenum oxide nanowire preparation process of claim 1, wherein the H is2O2Is an oxidation source.
3. According to the rightThe process for preparing α -molybdenum oxide nanowires with high linearity and high yield according to claim 1, wherein in the step S1, the molybdenum powder and H are mixed2O2The molar concentration ratio of (1): (25-30).
4. The preparation process of high-linearity high-yield α -molybdenum oxide nanowires of claim 1, wherein the reactor shell in steps S1 and S2 is made of high-temperature and high-pressure resistant sealed stainless steel, and the inner layer is embedded with a layer of sealed polytetrafluoroethylene material to form a protective layer.
5. The high-linearity high-yield α -molybdenum oxide nanowire preparation process of claim 1, wherein the reaction temperature in the S2 step is 40 ℃ and the heating time is 20 h.
6. The high-linearity high-yield α -molybdenum oxide nanowire preparation process of claim 1, wherein the step S1 further comprises a temperature measurement step of providing a temperature measurement device inside the reaction vessel for measuring the temperature of the reaction system.
7. The process for preparing high-linearity high-yield α -molybdenum oxide nanowires of claim 1, wherein the substrate plate has an area of 1 x 1cm2Hollow simple substance silicon is used as a main body, and the average density of the whole body is 1 g/ml; and a copper coating with the thickness of 450-600 nm is coated on the surface of the simple substance silicon.
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