CN105948128A - Method for adjusting length of tungsten oxide nano-rod by means of oxygen - Google Patents
Method for adjusting length of tungsten oxide nano-rod by means of oxygen Download PDFInfo
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Abstract
The invention provides a method for adjusting the length of a tungsten oxide nano-rod by means of oxygen and belongs to the technical field of tungsten-based nano-materials. According to the method, tungsten metal salt serves as a tungsten source, a carbon nano-tube serves as a carrier, ethanediol serves as a dispersant, hydrochloric acid is added into the reaction system, tungstic acid is directly separated out of the surface of the carbon nano-tube and covers the surface of the carbon nano-tube, tungstic acid grows along the surface of the carbon nano-tube, and then a tungstic acid/carbon nano-tube rodlike composite is formed. Then, the composite is put in a high-temperature reaction region for heat treatment, an oxidizing atmosphere is introduced, the carbon nano-tube is burnt, the burning degree of the carbon nano-tube and the generation speed of carbon dioxide are controlled by controlling the gas flow and the oxygen content, the breakage degree and surface shrinkage degree of the tungsten oxide nano-rod are controlled accordingly, and therefore the purpose of shearing the tungsten oxide nano-rod is achieved.
Description
Technical field
The present invention relates to the preparation method of a kind of tungstenio technical field of nano material, a kind of by the method for oxygen regulation tungsten oxide nanometer rod length.
Background technology
The tungsten oxide with nanostructured shows special physical effect because having higher specific surface area so that its electrochromism, photochromic, sense and the field such as catalysis has wide using value.The performance of tungsten carbide is the most closely related with tungsten oxide raw material, and tungsten oxide is during carbonizing reduction, and the tungsten carbide crystal grain of generation is easily formed abnormal thick granule because mutually assembling.Therefore, if preparing the nanostructured tungsten oxide of high-specific surface area, it will improve its physical and chemical performance further, expanding its using value, particularly it is in the value in the preparation and application field of nanometer tungsten carbide.
The synthesis of nanostructured (such as nanometer rods, nanometer sheet, nanosphere, nanotube etc.) tungsten oxide mainly has the methods such as solid-bed break-up method, liquid phase deposition, vapour deposition process.At present, the common method preparing tungsten oxide is to use liquid phase method.But during liquid phase prepares wolframic acid, wolframic acid granule coalesces in automatic because of thermodynamic instability；Additionally, the free water molecule on particle surface forms hydrogen bond with free hydroxyl, then form hydrogen chain with the hydrone on adjacent particle surface, produce bridge linking effect.Thus, this wolframic acid is fired, is dehydrated further, and hydrogen bond is converted into the bridging oxygen key that intensity is high, forms hard aggregation, and granularity significantly increases, and have impact on the performance of its performance.Generally solution is to use to add surfactant to improve its stability and viscosity, yet with the addition of surfactant so that containing more surfactant and adsorbate in final prepared tungsten oxide, cause its chemical property to decline.Template is to go to control and the pattern of decorative material, size with template for main body, and then improves a kind of preparation method of material character.Utilize space confinement effect and the structure-directing effect of template, it is possible to effectively prevent the generation of nano-particle secondary agglomeration phenomenon, the synthesis size of granule, pattern, structure and arrangement etc. effectively can be modulated.Therefore; if can be in wolframic acid forming process; template or interleaving agent are provided; wolframic acid granule is mutually isolated; stop or suppress the hydrogen bond that hydrone is formed with hydroxyl on its surface; and the chemical bond force formed between granule, the tungsten oxide tool improving hard aggregation and preparation nanostructured is of great significance.
Currently, use liquid phase method to combine template, the most successfully prepare nanostructured tungsten oxide.Pham Van Tong etc. has delivered entitled " Diameter controlled synthesis of tungsten oxide nanorod bundles in " Sensors and Actuators B " (sensor and actuator B) the 183rd phase page 372 380 in 2013
highly sensitive NO2Gas sensors " (for high quick NO2The diameter control synthesis of the tungsten oxide nanometer cluster of gas sensor) literary composition.Literary composition is commented: use hydro-thermal method that the diameter of tungsten oxide nanometer cluster is regulated and controled, and as surfactant, its pattern is controlled using polymer.Due to the limitation in this preparation method, i.e. hydro-thermal method reaction is all to carry out in the high-temperature high-pressure reaction kettle sealed, and in course of reaction, the external world cannot intervene the growth of tungsten oxide particles.Additionally, tungsten oxide particles is often along the superficial growth of template so that the pattern of the tungsten oxide nanofibers the prepared heredity pattern of template.Use the template that draw ratio is bigger, then the tungsten oxide draw ratio prepared is the biggest.According to the bigger tungsten oxide fiber of this draw ratio as preparing the raw material of tungsten carbide, during its carbonizing reduction, because being mutually wound around between tungsten oxide fiber so as to get tungsten carbide particle be prone to grow up, greatly have impact on structure and the performance of tungsten carbide.If the tungsten oxide raw material used is the nano oxidized tungsten particle of high-specific surface area, then it is easier to prepare that structure is more loose, the preferable tungsten-carbide powder of dispersibility.Therefore, if being controlled the length of tungsten oxide nanofibers of preparation, it will expand its using value further, particularly it is particularly important in terms of the preparation and application field of nanometer tungsten carbide.
Summary of the invention
It is an object of the invention to provide a kind of method by oxygen regulation tungsten oxide nanometer rod length, with a diameter of 2-200 nm, the number of plies be the surface-functionalized CNT of 1-30 layer be carrier, tungsten slaine is tungsten source, hydrochloric acid is dripped in CNT glycolic suspension and tungsten slaine system, utilize strong acid weak acid principle, wolframic acid granule is made directly to separate out and along its superficial growth in carbon nano tube surface, thus form the bar-shaped complex of wolframic acid/CNT, on the one hand it is to utilize CNT tube bank wolframic acid granule is isolated and supports, wolframic acid granule is made to separate out and cover its surface on its surface, and grow along its surface, thus generate club shaped structure；On the other hand it is to utilize ethylene glycol dispersing Nano carbon tubes and increase system viscosity, controls the growth rate of wolframic acid granule, reduce intergranular secondary agglomeration.Afterwards, this complex is placed in high temperature reaction zone, is passed through oxygen and the nitrogen of different proportion, carries out heat treatment, obtain tungsten oxide nanometer rod.In heat treatment process, we control CNT burning generate the speed of carbon dioxide by controlling gas flow (30-500 mL/min) and oxygen content (0-100%), and then regulation tungsten oxide nanometer rod breaking degree, thus quickly tungsten oxide nanometer rod is sheared and form the tungsten oxide nanometer rod of different length (20-800 nm).
The present invention is achieved by the following technical solutions, and the inventive method relates to a kind of method by oxygen regulation tungsten oxide nanometer rod length, mainly comprises the steps that
(1) CNT is carried out pretreatment: by a diameter of for 1-50 mg 2-200 nm, the number of plies is that the CNT of 1-30 layer is soaked in strong acid (a kind of or the most several mixing in hydrochloric acid, nitric acid, sulphuric acid), in the 100-140 DEG C of lower backflow of constant temperature stirring, filter, it is dried, it is placed in again in 10-500 mL ethylene glycol, ultrasound wave dispersion 8-24 h, obtains finely dispersed CNT glycolic suspension.
(2) configuration of tungsten metal salt solution: tungsten slaine is dissolved completely in solvent (in deionized water, ethylene glycol or both mixed liquor), obtains the tungsten metal salt solution that concentration is 0.01-0.5 mol/L.
(3) the CNT glycolic suspension of step (1) is joined in the tungsten metal salt solution of step (2), under mechanical force stirring (constant temperature blender with magnetic force or ultrasonic oscillator) effect, it is mixed uniformly, wherein the mol ratio of tungsten slaine and CNT is 1:1-40:1, dropping the most wherein (use microsyringe, dropper or by methods such as hydrochloric acid atomizations) 1-20 mL concentration is 5-12 mol/L hydrochloric acid, and the pH value of solution is adjusted to 1-5；Reflux under the conditions of 80-140 DEG C of constant temperature oil bath 5-48 h, then carries out vacuum filtration, washing, is dried, and wherein baking temperature is 100-150 DEG C, and drying time is 3-24 h, obtains the bar-shaped complex of wolframic acid/CNT.
(4) complex that step (3) obtains is laid in corundum reaction boat, together it is placed in the horizontal crystal reaction tube in tube type resistance furnace together with corundum reaction boat, when sample is carried out roasting, oxygen and the nitrogen of different proportion it is passed through in horizontal crystal reaction tube, its flow is 30-500 mL/min, wherein oxygen content is 0-100%, and heat treatment temperature is 400-800 DEG C, and heat treatment time is 0.5-12 h.It is cooled to room temperature, takes out, obtain the tungsten oxide nanometer rod of a length of 20-800 nm.
Strong acid described in step (1) is a kind of or the most several mixing in hydrochloric acid, nitric acid, sulphuric acid.Purpose is to utilize strong acid carbon nano tube surface is carried out hydroxylating and shears, for providing substantial amounts of forming core point at its surface graft wolframic acid.
Tungsten slaine described in step (2) is any one in sodium tungstate, tungsten hexachloride, ammonium metatungstate etc..
In step (3), it is possible to use microsyringe, dropper or the method such as hydrochloric acid atomization is introduced hydrochloric acid, the concentration of hydrochloric acid is 5-12 mol/L, consumption is 1-20 mL, the purpose introducing hydrochloric acid is to utilize strong acid to prepare the principle of weak acid, i.e. utilize hydrochloric acid to prepare 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 uses tungsten slaine and hydrochloric acid as reaction solution, CNT and ethylene glycol join in reaction solution respectively as carrier and dispersant, wolframic acid directly separates out and covers its surface in carbon nano tube surface, forms the bar-shaped complex of wolframic acid/CNT along its superficial growth simultaneously.The speed that wolframic acid granule separates out can be adjusted by the ratio of regulation ethylene glycol and water, owing to ethylene glycol adds the viscosity of solution, decrease intergranular secondary agglomeration phenomenon, thus avoid the wolframic acid granule generation secondary agglomeration being newly formed and excessively grow up, it is also possible to before dropping hydrochloric acid, reaction solution is heated to more than 80 DEG C and reaches the effect that wolframic acid uniformly separates out.And the wolframic acid coverage in carbon nano tube surface can be controlled by the ratio of regulation tungsten slaine with CNT, form club shaped structure wolframic acid/carbon mano-tube composite.In high temperature reaction zone, nitrogen and oxygen mixed gas flow are 30-500 mL/min, and wherein oxygen content is 0-100 %, it is ensured that while wolframic acid dehydration, CNT and oxygen generation combustion reaction.Control the speed of CNT burning generation carbon dioxide by controlling the content of mixed gas flow and wherein oxygen, so that the breaking degree of wolframic acid nanometer rods and surface shrinkage degree are controlled, reach the purpose that tungsten oxide nanometer rod length is sheared.
There is advantages that the present invention, using CNT as template, first prepares wolframic acid/carbon nanotube rod, afterwards with liquid phase method,Wolframic acid/carbon nanotube rod is placed in the high temperature reaction zone of tube furnace, during wolframic acid presoma is dehydrated and is converted into tungsten oxide, it is passed through oxidizing atmosphere, CNT is made burning to occur and generate carbon dioxide, disappearance with CNT, wolframic acid nanometer rods fractures, thus has intervened the tungsten oxide growth along CNT tube bank surface.Content (oxygen content is 0-100%) particular by the flow (30-500 mL/min) and wherein oxidizing gas that control oxidizing atmosphere controls CNT burning degree and the shrinkage degree on tungsten oxide surface, and the speed of generation carbon dioxide, thus obtain the length tungsten oxide nanometer rod at 20-800 nm.The raw material of the present invention is easy to get, and preparation technology is simple, and technology controlling and process is succinct, and can be controlled the content of the mixed gas flow being passed through and wherein oxygen, thus the tungsten oxide nanometer obtaining a length of 20-800 nm is excellent as required.
Accompanying drawing explanation
Fig. 1 is the transmission electron microscope photo of the bar-shaped complex 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.
Detailed description of the invention
The present embodiment be premised on inventive technique scheme under implement, give detailed embodiment and process, but protection scope of the present invention be not limited to following embodiment.
Embodiment
1
。
By 12 mg a diameter of 30-200 nm, the number of plies is that the CNT of 20-30 layer is soaked in nitric acid, in 100 DEG C of lower backflows of constant temperature stirring, after drying, it is scattered in 100 mL ethylene glycol, ultrasound wave dispersion 24h, obtains the CNT glycolic suspension A that finely dispersed concentration is 0.01 mol/L；Sodium tungstate is dissolved completely in 100 mL deionized waters, obtains the sodium tungstate solution B of the concentration 0.1 mol/L of clarification；Solution B joins in solution A, under constant temperature blender with magnetic force effect, is mixed uniformly, then drips appropriate hydrochloric acid wherein, the pH value of solution is adjusted to 1；Reflux under the conditions of 140 DEG C of constant temperature oil baths 10 h, then carries out vacuum filtration, washing, and dry temperature is 110 DEG C, and temperature retention time is 2 h；Obtain CNT and wolframic acid bar-shaped complex C；Complex C is laid in corundum reaction boat, together with in the horizontal crystal reaction tube that corundum reaction boat is placed in tube type resistance furnace, horizontal crystal reaction tube is passed through 0 % oxygen and 100 % nitrogen, flow is 60 mL/min, and sample is carried out heat treatment, and heat treatment temperature is 600 DEG C, heat treatment time 3 h, it is cooled to room temperature, takes out, obtain the tungsten oxide/carbon nano-tube nano rod of a length of 100 nm.
Embodiment
2
。
By 12 mg a diameter of 30-200 nm, the number of plies is that the CNT of 20-30 layer is soaked in nitric acid, in 100 DEG C of lower backflows of constant temperature stirring, is scattered in after drying in 100 mL ethylene glycol, ultrasound wave dispersion 24h, obtains the CNT glycolic suspension A that finely dispersed concentration is 0.01 mol/L；Sodium tungstate is dissolved completely in 100 mL deionized waters, obtains the sodium tungstate solution B of the concentration 0.1 mol/L of clarification；Solution B joins in solution A, under constant temperature blender with magnetic force effect, is mixed uniformly, then drips appropriate hydrochloric acid wherein, the pH value of solution is adjusted to 1；Reflux under the conditions of 140 DEG C of constant temperature oil baths 10 h, then carries out vacuum filtration, washing, and dry temperature is 110 DEG C, and temperature retention time is 2 h；Obtain CNT and wolframic acid bar-shaped complex C；Complex C is laid in corundum reaction boat, together with in the horizontal crystal reaction tube that corundum reaction boat is placed in tube type resistance furnace, horizontal crystal reaction tube is passed through 20% oxygen and 80% nitrogen, flow is 60 mL/min, and sample is carried out heat treatment, and heat treatment temperature is 600 DEG C, heat treatment time 3 h, it is cooled to room temperature, takes out, obtain the tungsten oxide nanometer rod of a length of 80 nm.
Embodiment
3
。
By 12 mg a diameter of 15-150 nm, the number of plies is that the CNT of 10-20 layer is soaked in nitric acid, in 130 DEG C of lower backflows of constant temperature stirring, is scattered in after drying in 100 mL ethylene glycol, ultrasound wave dispersion 24h, obtains the CNT glycolic suspension A that finely dispersed concentration is 0.01 mol/L；Sodium tungstate is dissolved completely in 100 mL deionized waters and ethylene glycol mixture, obtains the sodium tungstate solution B of the concentration 0.2 mol/L of clarification；Solution B joins in solution A, under ul-trasonic irradiation, is mixed uniformly, then drips appropriate hydrochloric acid wherein, the pH value of solution is adjusted to 3；Reflux under the conditions of 120 DEG C of constant temperature oil baths 6 h, then carries out vacuum filtration, washing, and dry temperature is 100 DEG C, and temperature retention time is 2 h；Obtain CNT and wolframic acid bar-shaped complex C；Complex C is laid in corundum reaction boat, together with in the horizontal crystal reaction tube that corundum reaction boat is placed in tube type resistance furnace, being passed through 20% oxygen and 80% nitrogen in horizontal crystal reaction tube, flow is 100 mL/min, and sample is carried out heat treatment, heat treatment temperature is 600 DEG C, heat treatment time 1 h, is cooled to room temperature, takes out, obtain, the tungsten oxide nanometer rod of a length of 60 nm.
Embodiment
4
。
By 12 mg a diameter of 10-100 nm, the number of plies is that the CNT of 5-10 layer is soaked in nitric acid, in 140 DEG C of lower backflows of constant temperature stirring, is scattered in after drying in 100 mL ethylene glycol, ultrasound wave dispersion 24h, obtains the CNT glycolic suspension A that finely dispersed concentration is 0.01 mol/L；Sodium tungstate is dissolved completely in 100 mL deionized waters and ethylene glycol mixture, obtains the sodium tungstate solution B of the concentration 0.3 mol/L of clarification；Solution B joins in solution A, under ul-trasonic irradiation, is mixed uniformly, then drips appropriate hydrochloric acid wherein, the pH value of solution is adjusted to 4；Reflux under the conditions of 100 DEG C of constant temperature oil baths 5 h, then carries out vacuum filtration, washing, and dry temperature is 100 DEG C, and temperature retention time is 1 h；Obtain CNT and wolframic acid bar-shaped complex C；Complex C is laid in corundum reaction boat, together with in the horizontal crystal reaction tube that corundum reaction boat is placed in tube type resistance furnace, horizontal crystal reaction tube is passed through 100 % oxygen, flow is 200 mL/min, and sample is carried out heat treatment, and heat treatment temperature is 600 DEG C, heat treatment time 1 h, it is cooled to room temperature, takes out, obtain the tungsten oxide nanometer rod of a length of 40 nm.
Embodiment
5
。
By 12 mg a diameter of 2-50 nm, the number of plies is that the CNT of 1-5 layer is soaked in nitric acid, in 140 DEG C of lower backflows of constant temperature stirring, is scattered in after drying in 100 mL ethylene glycol, ultrasound wave dispersion 24h, obtains the CNT ethylene glycol solution A that finely dispersed concentration is 0.01 mol/L；Sodium tungstate is dissolved completely in 100 mL deionized waters and ethylene glycol mixture, obtains the sodium tungstate suspension B of the concentration 0.3 mol/L of clarification；Solution B joins in solution A, under ul-trasonic irradiation, is mixed uniformly, then drips appropriate hydrochloric acid wherein, the pH value of solution is adjusted to 4；Reflux under the conditions of 100 DEG C of constant temperature oil baths 4 h, then carries out vacuum filtration, washing, and dry temperature is 100 DEG C, and temperature retention time is 1 h；Obtain CNT and wolframic acid bar-shaped complex C；Complex C is laid in corundum reaction boat, together with in the horizontal crystal reaction tube that corundum reaction boat is placed in tube type resistance furnace, horizontal crystal reaction tube is passed through 100% oxygen, flow is 200 mL/min, and sample is carried out heat treatment, and heat treatment temperature is 600 DEG C, heat treatment time 1 h, it is cooled to room temperature, takes out, obtain the tungsten oxide particles of a length of 20 nm.
Claims (7)
1. the method being regulated tungsten oxide nanometer rod length by oxygen, it is characterised in that: the present invention is with a diameter of 2-200
Nm, the number of plies be the surface-functionalized CNT of 1-30 layer be carrier, with tungsten slaine for tungsten source, ethylene glycol is dispersant, hydrochloric acid is dripped in this reaction system, utilize the principle of strong acid weak acid, make wolframic acid directly separate out and cover its surface in carbon nano tube surface, form the bar-shaped complex of wolframic acid/CNT along its superficial growth simultaneously；On the one hand utilize ethylene glycol dispersing Nano carbon tubes and increase the viscosity of system, controlling the growth rate of wolframic acid granule, decrease intergranular secondary agglomeration；On the other hand utilize CNT tube bank wolframic acid granule is isolated and supports, make wolframic acid granule separate out and cover its surface on its surface, and grow along its surface, so that complex is club shaped structure；Afterwards, this complex is placed in high temperature reaction zone and carries out heat treatment, and be passed through oxidizing atmosphere, make CNT burn, owing to the disappearance of CNT result in fractureing and surface shrinkage of tungsten oxide nanometer rod；By controlling the content of mixed gas flow and wherein oxygen, the length making tungsten oxide nanometer excellent is controlled.
The most according to claim 1 a kind of by the method for oxygen regulation tungsten oxide nanometer rod length, it is characterised in that to comprise the following steps:
(1) CNT is carried out pretreatment: by a diameter of for 1-50 mg 2-200 nm, the number of plies is that the CNT of 1-30 layer is soaked in strong acid, in the 100-140 DEG C of lower backflow of constant temperature stirring, filter, it is dried, it is placed in again in 10-500 mL ethylene glycol, ultrasound wave dispersion 8-24 h, obtains finely dispersed CNT glycolic suspension；
(2) configuration of tungsten metal salt solution: be dissolved completely in the mixed liquor of deionized water or ethylene glycol or deionized water and ethylene glycol by tungsten slaine, obtains the tungsten metal salt solution that concentration is 0.01-0.5mol/L；
(3) the CNT glycolic suspension of step (1) is joined in the tungsten metal salt solution of step (2), under mechanical force stirring condition, it is mixed uniformly, wherein the amount of the material of tungsten source and CNT is than for 1:1 40:1, drip appropriate hydrochloric acid the most wherein, the pH value of solution is adjusted to 1-5；Reflux under the conditions of 100-140 DEG C of constant temperature oil bath 5-48 h, then carries out vacuum filtration, washing, is dried, and wherein baking temperature is 100-150 DEG C, and drying time is 3-24 h, obtains the bar-shaped complex of wolframic acid/CNT；
(4) complex that step (3) obtains is laid in corundum reaction boat, together it is placed in the horizontal crystal reaction tube in tube type resistance furnace together with corundum reaction boat, when sample is carried out roasting, oxygen and the nitrogen of different proportion it is passed through in horizontal crystal reaction tube, heat treatment temperature is 400-800 DEG C, and heat treatment time is 0.5-12 h, is cooled to room temperature, take out, obtain the tungsten oxide nanometer rod of a length of 20-800 nm.
The method of a kind of oxygen the most according to claim 2 regulation tungsten oxide nanometer rod length, it is characterised in that: the strong acid described in step (1) is a kind of or the most several mixing in hydrochloric acid, nitric acid, sulphuric acid.
The method of a kind of oxygen the most according to claim 2 regulation tungsten oxide nanometer rod length, it is characterised in that: the tungsten slaine described in step (2) is any one in sodium tungstate, tungsten hexachloride, ammonium metatungstate etc..
The method of a kind of oxygen the most according to claim 2 regulation tungsten oxide nanometer rod length, it is characterized in that: in described step (3), using microsyringe, dropper or the methods such as hydrochloric acid atomization are introduced hydrochloric acid, the concentration of hydrochloric acid is 5-12 mol/L, and consumption is 1-20 mL.
The method of a kind of oxygen the most according to claim 2 regulation tungsten oxide nanometer rod length, it is characterised in that: in step (3), the stirring of described mechanical force uses constant temperature blender with magnetic force or ultrasonic oscillator.
The method of a kind of oxygen the most according to claim 2 regulation tungsten oxide nanometer rod length, it is characterised in that: in step (4), the flow of described oxygen and nitrogen is 30-500 mL/min, and wherein oxygen content is 0-100%.
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| 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 |
| CN115094432A (en) * | 2022-05-12 | 2022-09-23 | 中国科学院金属研究所 | Preparation method of structure function integrated transition metal carbide/single-walled carbon nanotube composite film |
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| CN116143175A (en) * | 2023-04-23 | 2023-05-23 | 崇义章源钨业股份有限公司 | Nano tungsten oxide with high specific surface area and preparation method thereof |
| 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 |
| CN116375091A (en) * | 2023-06-05 | 2023-07-04 | 崇义章源钨业股份有限公司 | Method for stably preparing needle-like nano tungsten oxide |
| 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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