CN105948128B - A kind of method that tungsten oxide nanometer rod length is adjusted by oxygen - Google Patents
A kind of method that tungsten oxide nanometer rod length is adjusted by oxygen Download PDFInfo
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Abstract
A kind of method that tungsten oxide nanometer rod length is adjusted by oxygen, belongs to tungsten based nano-material technical field.This method is using tungsten metal salt as tungsten source, CNT is carrier, and ethylene glycol is dispersant, and hydrochloric acid is added in the reaction system, wolframic acid is directly separated out in carbon nano tube surface and cover its surface, and the bar-shaped compound of wolframic acid/CNT is formed along its superficial growth.The compound is placed in into high temperature reaction zone afterwards to be heat-treated, it is passed through oxidizing atmosphere, CNT is set to burn, the speed of CNT burning degree and generation carbon dioxide is controlled by controlling gas flow and oxygen content, so that the breaking degree and surface shrinkage degree of tungsten oxide nanometer rod are controlled, reach the purpose sheared to tungsten oxide nanometer rod length.
Description
Technical field
The present invention relates to a kind of preparation method of tungsten based nano-material technical field, is specifically that a kind of adjusted by oxygen aoxidizes
The method of tungsten nanorod length.
Background technology
Tungsten oxide with nanostructured because showing special physical effect with higher specific surface area so that
It has wide application value in fields such as electrochromism, photochromic, sensing and catalysis.The performance of tungsten carbide is mainly and oxygen
It is closely related to change tungsten raw material, for tungsten oxide during carbonizing reduction, the tungsten carbide crystal grain of generation is abnormal because mutually assembling easily formation
Thick particle.Therefore, if preparing the nanostructured tungsten oxide of high-specific surface area, it will further improve its physical chemistry
Performance, expand its application value, particularly its value in the preparation and application field of nanometer tungsten carbide.
Nanostructured（Such as nanometer rods, nanometer sheet, nanosphere, nanotube etc.）The synthesis of tungsten oxide mainly has solid-bed break-up
The methods of method, liquid phase deposition, vapour deposition process.At present, the common method for preparing tungsten oxide is to use liquid phase method.But in liquid phase
During preparing wolframic acid, wolframic acid particle is in automatic coalescence because of thermodynamic instability；In addition, the free moisture on particle surface
Son forms hydrogen bond with free hydroxyl, then forms hydrogen chain with the hydrone on adjacent particle surface, produces bridge linking effect.Thus, this
Kind wolframic acid is fired, further dehydration, and hydrogen bond is converted into the high bridging oxygen key of intensity, forms hard aggregation, and granularity significantly increases,
It has impact on the performance of its performance.Usual solution is to improve its stability and viscosity using surfactant is added, so
And due to the addition of surfactant so that contain more surfactant and adsorbate in final prepared tungsten oxide,
Its chemical property is caused to decline.Template is that pattern, the size of control and decorative material are gone using template as main body, and then improves material
Expect a kind of preparation method of property.Using the space confinement effect of template and structure-directing effect, nanometer can be effectively prevented
The generation of grain secondary agglomeration phenomenon, can effectively be modulated to the size of synthesis particle, pattern, structure and arrangement etc..Therefore,
If can be in wolframic acid forming process, there is provided template or interleaving agent, wolframic acid particle is mutually isolated, prevent or suppress hydrone with
The hydrogen bond that hydroxyl is formed on its surface, and the chemical bond force formed between particle, to improving hard aggregation and preparing nanostructured
Tungsten oxide tool is of great significance.
Currently, using liquid phase method combination template, nanostructured tungsten oxide is successfully prepared.Pham Van Tong etc.
《Sensors and Actuators B》（Sensor and actuator B）183rd phase page 372-380 in 2013 has delivered topic
For《Diameter controlled synthesis of tungsten oxide nanorod bundles for
highly sensitive NO2gas sensors 》(it is used for high quick NO2The tungsten oxide nanometer cluster of gas sensor it is straight
Footpath control synthesis) text.Commented in text：The diameter of tungsten oxide nanometer cluster is regulated and controled using hydro-thermal method, and with polymer
Its pattern is controlled as surfactant.Due to the limitation in the preparation method, i.e. hydro-thermal method reaction is all close
Carried out in the high-temperature high-pressure reaction kettle of envelope, during the course of the reaction, the external world can not intervene the growth of tungsten oxide particles.In addition, oxidation
Tungsten particle is often along the superficial growth of template so that the patterns of the tungsten oxide nanofibers the prepared heredity shape of template
Looks.Using the bigger template of major diameter, then the tungsten oxide draw ratio prepared is also larger.It is bigger according to this major diameter
Aoxidize tungsten fiber be used as the raw material for preparing tungsten carbide, during its carbonizing reduction, because aoxidize tungsten fiber between mutually wind,
The tungsten carbide particle for making to obtain is easy to grow up, and greatly have impact on the structure and performance of tungsten carbide.If the tungsten oxide used is former
Material is the nano oxidized tungsten particle of high-specific surface area, then is easier to prepare that structure is more loose, dispersed preferable tungsten carbide powder
End.Therefore, if being controlled to the length of the tungsten oxide nanofibers of preparation, it will further expand its application value, it is special
It is not that it is particularly important in terms of the preparation and application field of nanometer tungsten carbide.
The content of the invention
It is an object of the invention to provide a kind of method that tungsten oxide nanometer rod length is adjusted by oxygen, with a diameter of 2-
200 nm, the number of plies are that the surface-functionalized CNT of 1-30 layers is carrier, and tungsten metal salt is tungsten source, in CNT second two
Hydrochloric acid is added dropwise in alcohol suspension and tungsten metal salt system, using strong acid weak acid principle, makes wolframic acid particle directly in CNT
Surface separates out and along its superficial growth, is on the one hand to utilize CNT so as to form the bar-shaped compound of wolframic acid/CNT
Tube bank is isolated and supported to wolframic acid particle, wolframic acid particle is separated out on its surface and covers its surface, and enters along its surface
Row growth, so as to generate club shaped structure；On the other hand it is to utilize ethylene glycol dispersing Nano carbon tubes and increase system viscosity, controls tungsten
The growth rate of granulates, reduce intergranular secondary agglomeration.Afterwards, the compound is placed in high temperature reaction zone, is passed through difference
The oxygen and nitrogen of ratio, are heat-treated, and obtain tungsten oxide nanometer rod.In heat treatment process, we are by controlling gas
Flow（30-500 mL/min）And oxygen content（0-100%）To control the speed of CNT burning generation carbon dioxide, enter
And tungsten oxide nanometer rod breaking degree is adjusted, so as to quickly be sheared to tungsten oxide nanometer rod and form different length（20-
800 nm）Tungsten oxide nanometer rod.
The present invention is achieved by the following technical solutions, and the inventive method is related to one kind and received by oxygen regulation tungsten oxide
The method of rice rod length, is mainly included the following steps that：
(1) CNT is pre-processed：By a diameter of 2-200 nm of 1-50 mg, the number of plies is the carbon nanometer of 1-30 layers
Pipe is soaked in strong acid（One kind or wherein several mixing in hydrochloric acid, nitric acid, sulfuric acid）In, under 100-140 DEG C of constant temperature stirs
Backflow, filter, dry, then be placed in 10-500 mL ethylene glycol, ultrasonic wave disperses 8-24 h, obtains finely dispersed carbon nanometer
Pipe glycolic suspension.
(2) configuration of tungsten metal salt solution：Tungsten metal salt is dissolved completely in solvent（In deionized water, ethylene glycol or two
The mixed liquor of person）In, obtain the tungsten metal salt solution that concentration is 0.01-0.5 mol/L.
(3) the CNT glycolic suspension of step (1) is added in the tungsten metal salt solution of step (2), in machine
Tool power stirs（Constant temperature blender with magnetic force or ultrasonic oscillator）Under effect, it is mixed uniformly, wherein tungsten metal salt and carbon are received
The mol ratio of mitron is 1:1-40:1, then be added dropwise thereto（The methods of using microsyringe, dropper or hydrochloric acid being atomized）1-
20 mL concentration are 5-12 mol/L hydrochloric acid, and the pH value of solution is adjusted into 1-5；Flowed back under the conditions of 80-140 DEG C of constant temperature oil bath
5-48 h, then be filtered by vacuum, washed, dry, wherein drying temperature is 100-150 DEG C, and drying time is 3-24 h, is obtained
To the bar-shaped compound of wolframic acid/CNT.
(4) compound that step (3) obtains is laid in corundum reaction boat, pipe is together placed in together with corundum reaction boat
In horizontal crystal reaction tube in formula resistance furnace, when being calcined to sample, different proportion is passed through into horizontal crystal reaction tube
Oxygen and nitrogen, its flow is 30-500 mL/min, and wherein oxygen content is 0-100%, heat treatment temperature 400-800
DEG C, heat treatment time is 0.5-12 h.Normal temperature is cooled to, is taken out, produces the tungsten oxide nanometer rod that length is 20-800 nm.
Strong acid described in step (1) is hydrochloric acid, nitric acid, one kind in sulfuric acid or wherein several mixing.Purpose is profit
Carbon nano tube surface is subjected to hydroxylating with strong acid and sheared, to provide substantial amounts of forming core in its surface graft wolframic acid
Point.
Tungsten metal salt described in step (2) is any one in sodium tungstate, tungsten hexachloride, ammonium metatungstate etc..
In step (3), microsyringe, dropper can be used or hydrochloric acid is introduced the methods of hydrochloric acid is atomized, hydrochloric acid it is dense
It is 1-20 mL to spend for 5-12 mol/L, dosage, and the purpose for introducing hydrochloric acid is that the principle of weak acid is prepared using strong acid, that is, utilizes salt
Acid prepares wolframic acid.
In step (4), the flow of oxygen and nitrogen is 30-500 mL/min, and wherein oxygen content is 0-100%.
The present invention respectively as carrier and is divided using tungsten metal salt and hydrochloric acid as reaction solution, CNT and ethylene glycol
Powder is added in reaction solution, and wolframic acid directly separates out in carbon nano tube surface and covers its surface, while along its surface
Grow and form the bar-shaped compound of wolframic acid/CNT.Wolframic acid particle can be adjusted by adjusting the ratio of ethylene glycol and water
The speed of precipitation, because ethylene glycol adds the viscosity of solution, reduce intergranular secondary agglomeration phenomenon, it is new so as to avoid
The wolframic acid particle of formation occurs secondary agglomeration and excessively grown up, and reaction solution can also be heated into 80 DEG C before hydrochloric acid is added dropwise
Reach the effect that wolframic acid uniformly separates out above.And wolframic acid can be controlled in carbon by adjusting the ratio of tungsten metal salt and CNT
The coverage of nanotube surface, form club shaped structure wolframic acid/carbon mano-tube composite.In high temperature reaction zone, nitrogen and oxygen mix
Conjunction gas flow is 30-500 mL/min, and wherein oxygen content is 0-100 %, ensure wolframic acid dehydration while, CNT with
Combustion reaction occurs for oxygen.By control mixed gas flow and wherein the content of oxygen come control CNT burning generation two
The speed of carbonoxide, so that the breaking degree of wolframic acid nanometer rods and surface shrinkage degree are controlled, reach and tungsten oxide is received
The purpose that rice rod length is sheared.
The present invention has the advantages that：The present invention using CNT as template, first with liquid phase method prepare wolframic acid/
Carbon nanotube rod, afterwards, wolframic acid/carbon nanotube rod is placed in the high temperature reaction zone of tube furnace, in wolframic acid presoma
During being dehydrated and being converted into tungsten oxide, oxidizing atmosphere is passed through, makes CNT occur to burn and generate carbon dioxide gas
Body, with the disappearance of CNT, wolframic acid nanometer rods are fractureed, and surface is restrained along CNT so as to intervene tungsten oxide
Growth.Particular by the flow of control oxidizing atmosphere（30-500 mL/min）And the wherein content of oxidizing gas（Oxygen
Gas content is 0-100%）To control the shrinkage degree of CNT burning degree and tungsten oxide surface, and generate carbon dioxide
Speed, so as to obtain tungsten oxide nanometer rod of the length in 20-800 nm.The raw material of the present invention is easy to get, and preparation technology is simple, technique
Control is succinct, and can be as needed, the mixed gas flow and the content of wherein oxygen being passed through is controlled, so as to be grown
Spend the tungsten oxide nanometer rod for 20-800 nm.
Brief description of the drawings
Fig. 1 is the transmission electron microscope photo of the bar-shaped compound of wolframic acid/CNT.
Fig. 2 is the transmission electron microscope photo of tungsten oxide nanometer rod in embodiment 3.
Fig. 3 is the transmission electron microscope photo of tungsten oxide nanometer rod in embodiment 4.
Embodiment
The present embodiment be premised on inventive technique scheme under implemented, give detailed embodiment and process,
But protection scope of the present invention is not limited to following embodiments.
Embodiment 1.
By a diameter of 30-200 nm of 12 mg, the number of plies is soaked in nitric acid for the CNT of 20-30 layers, in 100 DEG C of perseverances
Temperature stirring is lower to flow back, and after drying, is scattered in 100 mL ethylene glycol, ultrasonic wave disperses 24h, obtains finely dispersed concentration and is
0.01 mol/L CNT glycolic suspension A；Sodium tungstate is dissolved completely in 100 mL deionized waters, clarified
0.1 mol of concentration/L sodium tungstate solution B；Solution B is added in solution A, under constant temperature blender with magnetic force effect, by it
It is well mixed, then appropriate hydrochloric acid is added dropwise thereto, the pH value of solution is adjusted to 1；Flowed back under the conditions of 140 DEG C of constant temperature oil baths
10 h, then be filtered by vacuum, washed, dry temperature is 110 DEG C, and soaking time is 2 h；Obtain CNT and wolframic acid
Bar-shaped compound C；Compound C is laid in corundum reaction boat, is placed in together with corundum reaction boat in tube type resistance furnace
In horizontal crystal reaction tube, 0 % oxygen and 100 % nitrogen are passed through in horizontal crystal reaction tube, flow is 60 mL/min, right
Sample is heat-treated, and heat treatment temperature is 600 DEG C, the h of heat treatment time 3, is cooled to normal temperature, is taken out, and produces length as 100
Nm tungsten oxide/carbon nano-tube nano rod.
Embodiment 2.
By a diameter of 30-200 nm of 12 mg, the number of plies is soaked in nitric acid for the CNT of 20-30 layers, in 100 DEG C of perseverances
Temperature stirring is lower to flow back, and is scattered in after drying in 100 mL ethylene glycol, ultrasonic wave disperses 24h, obtains finely dispersed concentration and is
0.01 mol/L CNT glycolic suspension A；Sodium tungstate is dissolved completely in 100 mL deionized waters, clarified
0.1 mol of concentration/L sodium tungstate solution B；Solution B is added in solution A, under constant temperature blender with magnetic force effect, by it
It is well mixed, then appropriate hydrochloric acid is added dropwise thereto, the pH value of solution is adjusted to 1；In 140 DEG C of constant temperature oil bath conditions next time
10 h are flowed, then is filtered by vacuum, washed, dry temperature is 110 DEG C, and soaking time is 2 h；Obtain CNT and tungsten
The bar-shaped compound C of acid；Compound C is laid in corundum reaction boat, is placed in together with corundum reaction boat in tube type resistance furnace
Horizontal crystal reaction tube in, 20% oxygen and 80% nitrogen are passed through in horizontal crystal reaction tube, flow is 60 mL/min, right
Sample is heat-treated, and heat treatment temperature is 600 DEG C, the h of heat treatment time 3, is cooled to normal temperature, is taken out, and produces length as 80
Nm tungsten oxide nanometer rod.
Embodiment 3.
By a diameter of 15-150 nm of 12 mg, the number of plies is soaked in nitric acid for the CNT of 10-20 layers, in 130 DEG C of perseverances
Temperature stirring is lower to flow back, and is scattered in after drying in 100 mL ethylene glycol, ultrasonic wave disperses 24h, obtains finely dispersed concentration and is
0.01 mol/L CNT glycolic suspension A；Sodium tungstate is dissolved completely in 100 mL deionized waters and ethylene glycol mixes
Close in liquid, 0.2 mol of the concentration/L clarified sodium tungstate solution B；Solution B is added in solution A, in ul-trasonic irradiation
Under, it is mixed uniformly, then appropriate hydrochloric acid is added dropwise thereto, the pH value of solution is adjusted to 3；In 120 DEG C of constant temperature oil bath bars
Flow back 6 h under part, then is filtered by vacuum, washed, and dry temperature is 100 DEG C, and soaking time is 2 h；Obtain CNT
With the bar-shaped compound C of wolframic acid；Compound C is laid in corundum reaction boat, tubular electric resistance is placed in together with corundum reaction boat
In horizontal crystal reaction tube in stove, 20% oxygen and 80% nitrogen are passed through in horizontal crystal reaction tube, flow is 100 mL/min,
Sample is heat-treated, heat treatment temperature is 600 DEG C, the h of heat treatment time 1, is cooled to normal temperature, takes out, produces, length is
60 nm tungsten oxide nanometer rod.
Embodiment 4.
By a diameter of 10-100 nm of 12 mg, the number of plies is soaked in nitric acid for the CNT of 5-10 layers, in 140 DEG C of perseverances
Temperature stirring is lower to flow back, and is scattered in after drying in 100 mL ethylene glycol, ultrasonic wave disperses 24h, obtains finely dispersed concentration and is
0.01 mol/L CNT glycolic suspension A；Sodium tungstate is dissolved completely in 100 mL deionized waters and ethylene glycol mixes
Close in liquid, 0.3 mol of the concentration/L clarified sodium tungstate solution B；Solution B is added in solution A, in ul-trasonic irradiation
Under, it is mixed uniformly, then appropriate hydrochloric acid is added dropwise thereto, the pH value of solution is adjusted to 4；In 100 DEG C of constant temperature oil bath bars
Flow back 5 h under part, then is filtered by vacuum, washed, and dry temperature is 100 DEG C, and soaking time is 1 h；Obtain CNT
With the bar-shaped compound C of wolframic acid；Compound C is laid in corundum reaction boat, tubular electric resistance is placed in together with corundum reaction boat
In horizontal crystal reaction tube in stove, 100 % oxygen are passed through in horizontal crystal reaction tube, flow is 200 mL/min, to sample
It is heat-treated, heat treatment temperature is 600 DEG C, the h of heat treatment time 1, is cooled to normal temperature, is taken out, and it is 40 nm's to produce length
Tungsten oxide nanometer rod.
Embodiment 5.
By a diameter of 2-50 nm of 12 mg, the number of plies is soaked in nitric acid for the CNT of 1-5 layers, stirred in 140 DEG C of constant temperature
Lower backflow is mixed, is scattered in after drying in 100 mL ethylene glycol, ultrasonic wave disperses 24h, obtains finely dispersed concentration as 0.01
Mol/L CNT ethylene glycol solution A；Sodium tungstate is dissolved completely in 100 mL deionized waters and ethylene glycol mixture,
0.3 mol of the concentration/L clarified sodium tungstate suspension B；Solution B is added in solution A, will under ul-trasonic irradiation
It is well mixed, then appropriate hydrochloric acid is added dropwise thereto, and the pH value of solution is adjusted into 4；In 100 DEG C of constant temperature oil bath conditions next time
4 h are flowed, then is filtered by vacuum, washed, dry temperature is 100 DEG C, and soaking time is 1 h；Obtain CNT and wolframic acid
Bar-shaped compound C；Compound C is laid in corundum reaction boat, is placed in together with corundum reaction boat in tube type resistance furnace
In horizontal crystal reaction tube, 100% oxygen is passed through in horizontal crystal reaction tube, flow is 200 mL/min, and hot place is carried out to sample
Reason, heat treatment temperature are 600 DEG C, the h of heat treatment time 1, are cooled to normal temperature, are taken out, and produce the tungsten oxide that length is 20 nm
Grain.
Claims (5)
- A kind of 1. method that tungsten oxide nanometer rod length is adjusted by oxygen, it is characterised in that comprise the following steps：（1）CNT is pre-processed：By a diameter of 2-200 nm of 1-50 mg, the number of plies is soaked for the CNT of 1-30 layers Steep in strong acid, in the 100-140 DEG C of lower backflow of constant temperature stirring, filter, dry, then be placed in 10-500 mL ethylene glycol, ultrasound Wavelength-division dissipates 8-24 h, obtains finely dispersed CNT glycolic suspension；（2）The configuration of tungsten metal salt solution：Tungsten metal salt is dissolved completely in deionized water or ethylene glycol or deionized water and second In the mixed liquor of glycol, the tungsten metal salt solution that concentration is 0.01-0.05mol/L is obtained；（3）By step（1）CNT glycolic suspension be added to step（2）Tungsten metal salt solution in, in mechanical force Under stirring condition, it is mixed uniformly, wherein the amount ratio of the material of tungsten source and CNT is 1:1-40:1, then be added dropwise thereto Appropriate hydrochloric acid, the pH value of solution is adjusted to 1-5；Flow back 5-48 h under the conditions of 100-140 DEG C of constant temperature oil bath, then carries out Vacuum filtration, washing, are dried, and wherein drying temperature is 100-150 DEG C, and drying time is 3-24 h, obtains wolframic acid/carbon nanometer Manage bar-shaped compound；（4）By step（3）Obtained compound is laid in corundum reaction boat, and tubular electric resistance is together placed in together with corundum reaction boat In horizontal crystal reaction tube in stove, sample is calcined, be passed through into horizontal crystal reaction tube different proportion oxygen and Nitrogen, heat treatment temperature are 400-800 DEG C, and heat treatment time is 0.5-12 h, and wherein gas flow is 30-500 mL/min, Oxygen content is 0-100 %, is cooled to normal temperature, is taken out, and produces the tungsten oxide nanometer rod that length is 20-800 nm.
- A kind of 2. method that tungsten oxide nanometer rod length is adjusted by oxygen according to claim 1, it is characterised in that：Step （1）Described in strong acid be hydrochloric acid, nitric acid, one kind in sulfuric acid or wherein several mixtures.
- A kind of 3. method that tungsten oxide nanometer rod length is adjusted by oxygen according to claim 1, it is characterised in that：Step （2）Described in tungsten metal salt be sodium tungstate, tungsten hexachloride, any one in ammonium metatungstate.
- A kind of 4. method that tungsten oxide nanometer rod length is adjusted by oxygen according to claim 1, it is characterised in that：Step （3）In, hydrochloric acid is introduced using microsyringe, dropper or hydrochloric acid atomizing type, the concentration of hydrochloric acid is 5-12mol/L, and dosage is 1-20mL。
- A kind of 5. method that tungsten oxide nanometer rod length is adjusted by oxygen according to claim 1, it is characterised in that：Step （3）In, the mechanical force stirring uses constant temperature blender with magnetic force or ultrasonic oscillator.
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| WO2022161460A1 (en) * | 2021-01-31 | 2022-08-04 | 黄志嘉 | Method for polymerase chain reaction |
| CN113861468B (en) * | 2021-10-11 | 2024-01-23 | 中国科学技术大学先进技术研究院 | Preparation method of photochromic tungsten oxide film and photochromic product |
| CN115094432B (en) * | 2022-05-12 | 2024-03-08 | 中国科学院金属研究所 | Preparation method of transition metal carbide/single-walled carbon nanotube composite film with integrated structure and function |
| CN116143175B (en) * | 2023-04-23 | 2023-08-08 | 崇义章源钨业股份有限公司 | Nano tungsten oxide with high specific surface area and preparation method thereof |
| CN116375091B (en) * | 2023-06-05 | 2023-08-11 | 崇义章源钨业股份有限公司 | Method for stably preparing needle-like nano tungsten oxide |
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