CN103351028A - Preparation method for continuously producing multi-shape nano tungsten trioxide material - Google Patents
Preparation method for continuously producing multi-shape nano tungsten trioxide material Download PDFInfo
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- CN103351028A CN103351028A CN2013103363214A CN201310336321A CN103351028A CN 103351028 A CN103351028 A CN 103351028A CN 2013103363214 A CN2013103363214 A CN 2013103363214A CN 201310336321 A CN201310336321 A CN 201310336321A CN 103351028 A CN103351028 A CN 103351028A
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Abstract
The invention discloses a preparation method for continuously producing a multi-shape nano tungsten trioxide material. The preparation method comprises the following steps of: 1, placing a piece of carbon cloth on the inner wall, close to an air outlet end, of a quartz glass tube, and putting the glass tube into a tubular furnace; 2, heating the glass tube to a specified temperature in the tubular furnace; 3, pushing a ceramic crucible containing ammonium paratungstate to a constant temperature area in the glass tube, and blowing argon into the glass tube; 4, preserving heat for 40-60 minutes, then closing the tubular furnace, and stopping blowing argon into the glass tube; 5, taking the carbon cloth out of the glass tube, and collecting a reaction product deposited on the carbon cloth to obtain multi-shape nano tungsten trioxide particles; 6, repeating the steps 1-5 for a plurality of times to realize continuous production. According to the preparation method provided by the invention, a technology combining high-temperature calcination with vapor deposition is adopted, the multi-shape nano tungsten trioxide particles are obtained by controlling the reaction temperature and carrier gas flow, the processing raw material is low in price, the process is simple, and the product is high in purity, so that the preparation method is suitable for continuously producing nano tungsten trioxide materials with different shape requirements.
Description
Technical field
The invention belongs to the manufacturing technology field of functional materials, relate to a kind of production technique of nanometer tungsten oxide material, specifically, relate to a kind of continuous production multi-morphology nano tungstic oxide material preparation method.
Background technology
Tungstic oxide (WO
3) be a kind of important N-shaped conductor oxidate, multiple crystalline structure is arranged, studied widely owing to having unique physical and chemical property, and obtained certain application at electrochromism, photochromic, sensing and catalytic field.In order further to utilize WO
3Excellent properties, widen its Application Areas, best technological approaches is to reduce its grain-size.Tradition WO
3The preparation of nano-powder is with Powdered ammonium paratungstate (APTxH
2O) be placed on to calcine on fixed stove or the rotary kiln and solid state reaction occurs make super-fine powder, perhaps make super-fine powder by again pulverizing.Wei Shaohong etc. put into retort furnace in 500 ℃ of lower high-temperature calcination 3h with a certain amount of ammonium tungstate, obtain WO behind the naturally cooling
3Micro mist, and then the process grinding technics obtains median size at the pure WO of 50-60nm
3Nano-powder.Huang Shizhen etc. are with (NH
4)
6W
7O
246H
2O is high-temp combustion 2-3h in stove, obtains the WO of 10-100nm
3Powder.High friend is good to be waited at O
2Under/Ar mixed gas the condition, in 700 ℃ the ammonium paratungstate thermal degradation has been prepared WO
3, and analyzed WO
3Catalyzer is at electron acceptor Fe
3+Photochemical catalyzing oxygen evolution activity under the solution system.Along with the increase of Ar content in the mixed gas, oxygen relative deficiency, WO
3The oxygen room increases, and its photochemical catalysis oxygen evolution activity also obviously improves.I. M. hereby glug according to (I. M. Szilagyi) etc. first with APT4H
2O is at H
2Thermal treatment obtains (NH through 6h in 400 ℃ under the atmosphere
4)
0.33-xWO
3-y(HATB), then take HATB as presoma, finally obtain hexagonal W O by conditioned reaction temperature and change reaction atmosphere
3The nanoparticle agglomerates body.Above-mentioned with APTxH
2O is that presoma adopts the solid phase decomposition method to prepare WO
3Though the experimental technique of super-fine powder is simple, the production cycle is long, cost is high, energy consumption is large, the WO of production
3Purity and granularity be difficult to control, the powder that generates is simultaneously easily reunited, and needs again to pulverize.In addition, with APT4H
2O is presoma, also can prepare nanostructure WO by liquid phase method
3Li Xiancai etc. are take ammonium paratungstate as presoma, and take deionized water as solvent, successfully preparing specific surface area by hydrothermal synthesis method is 15.36m
2The WO of/g
3Nano particle.But when adopting liquid phase method, often (NH can residually be arranged in the product
4)
xWO
3Perhaps (NH
4)
+, perhaps produce other impurity product, need further aftertreatment with purified product.
Studies show that in a large number, vapor phase process is one of effective means for preparing at present nanostructure.Can separate out the solid of various forms by gas phase deposition technology, the form of precipitate has film, whisker and particle, and vapour deposition process is not high to the concentration requirement of reactant, and the purity of product is higher.But adopt conventional vapour deposition process, the output of product is very limited, owing to collecting product under high vacuum or high temperature, can not realize continuous production.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of continuous production multiform looks tungstic oxide is with APTxH
2O is starting material, adopts high-temperature calcination in conjunction with gas phase deposition technology, take argon gas as carrier gas, collects powder at low-temperature region, has successfully realized different morphologies WO
3The continuous production of nano particle.
For achieving the above object, the invention provides a kind of continuous production multi-morphology nano tungstic oxide material preparation method, the method comprises following steps:
Step 1 is got the quartz glass tube that comprises inlet mouth and air outlet, places carbon cloth at quartz glass tube near the inner wall surrounding of air outlet end, and this quartz glass tube traverse that carbon cloth is housed is placed tube furnace;
Step 2 makes the diamond heating quartz glass tube to assigned temperature;
Step 3 pushes to the ceramic crucible that fills ammonium paratungstate in the above-mentioned Glass tubing, makes it to be in the flat-temperature zone that is heated to assigned temperature, is blown into argon gas;
Step 4 behind the insulation 40min-60min, is closed tube furnace, stops to be blown into argon gas;
Step 5 is taken out carbon cloth, collects the reaction product of deposition on it, obtains the nano tungsten trioxide particle of multiform looks, and takes out ceramic crucible;
Step 6, repeating step 1-5 several times: namely again place carbon cloth at the Glass tubing inner wall surrounding, the crucible that fills ammonium paratungstate is moved to the flat-temperature zone, again open argon gas, the reaction of beginning next round realizes producing continuously.
Above-mentioned continuous production multi-morphology nano tungstic oxide material preparation method, wherein, described step 1 also comprises the step of cleaning the silica glass inside pipe wall, and the purpose of cleaning is to remove the last time residual product of preparation, and the words of not cleaning may pollute the preparation that continues.
Above-mentioned continuous production multi-morphology nano tungstic oxide material preparation method, wherein, described silica glass length of tube is 1-1.5m, diameter is 0.3-0.5m.
Above-mentioned continuous production multi-morphology nano tungstic oxide material preparation method, wherein, described carbon cloth is placed on the place apart from flat-temperature zone 0.3-0.5m, too closely can obtain thin especially nano needle material apart from the flat-temperature zone, size and pattern apart from material too far away are all inhomogeneous, are the optimal distances that obtains by experiment apart from flat-temperature zone 0.3-0.5m.
Above-mentioned continuous production multi-morphology nano tungstic oxide material preparation method, wherein, in the described step 2, the temperature rise rate of heated Tube-furnace is 50 ℃/min, described assigned temperature is 1250 ℃-1400 ℃.
Above-mentioned continuous production multi-morphology nano tungstic oxide material preparation method, wherein, in the described step 3, ammonium paratungstate is dispersed in the ceramic crucible, and Uniform Dispersion is in order to guarantee that raw material is heated evenly.
Above-mentioned continuous production multi-morphology nano tungstic oxide material preparation method, wherein, in the described step 3, argon flow amount is 1L/min-6L/min.
Above-mentioned continuous production multi-morphology nano tungstic oxide material preparation method, wherein, described multi-morphology nano tungstic oxide material comprises following form and specification: torispherical tungstic oxide particle, diameter are 100nm-700nm; Spherical tungstic oxide particle, diameter is 20-200nm; Octahedral bodily form tungstic oxide particle, octahedra catercorner length is less than 1 μ m; The irregular tungstic oxide particle of polyhedron, the polyhedron catercorner length is about 10nm-2 μ m.Wherein, torispherical and spherical tungstic oxide particle can be used as the precursor synthesis nano tungsten carbide hard alloy; Octahedra tungstic oxide can be used as highly sensitive gas sensitive and makes gas sensor; Irregular tungstic oxide particle can be as the organic molecule in the sorbent material planar water or as the photocatalyst for degrading toxic organic compound.
The present invention combines high-temperature calcination technology and gas phase deposition technology, take argon gas as carrier gas, adopt carbon cloth to collect powder at low-temperature region, can produce continuously the nano level tungstic oxide particle of variform, solved traditional method and prepared the problem that nano tungsten trioxide yields poorly.The present invention has utilized aboundresources, cheap raw material, provides that a kind of price is suitable, excellent property, nano tungsten trioxide continuous production method that output is larger, and easy and simple to handle, cost is low, has great application prospect.
Description of drawings
Fig. 1 is the structural representation of the device that adopts of the preparation method of continuous production multiform looks tungstic oxide of the present invention.
Fig. 2 is when 1250 ℃ of Heating temperatures, argon flow amount 2L/min, X-ray diffraction (XRD) collection of illustrative plates of the nano tungsten trioxide product of collection.
Fig. 3 a, 3b are when 1250 ℃ of Heating temperatures, argon flow amount 2L/min, and the shape appearance figure of the nano tungsten trioxide product of collection (scanning electron microscope, SEM), wherein, Fig. 3 a is that magnification is 12500 SEM figure, Fig. 3 b is that magnification is 50000 SEM figure.
Fig. 4 is when 1300 ℃ of Heating temperatures, argon flow amount 2L/min, the shape appearance figure of the nano tungsten trioxide product of collection.
Fig. 5 is when 1350 ℃ of Heating temperatures, argon flow amount 2L/min, the shape appearance figure of the nano tungsten trioxide product of collection.
Fig. 6 is when 1400 ℃ of Heating temperatures, argon flow amount 2L/min, the shape appearance figure of the nano tungsten trioxide product of collection.
Fig. 7 is when 1350 ℃ of Heating temperatures, argon flow amount 1L/min, the shape appearance figure of the nano tungsten trioxide product of collection.
Fig. 8 is when 1350 ℃ of Heating temperatures, argon flow amount 4L/min, the shape appearance figure of the nano tungsten trioxide product of collection.
Fig. 9 is when 1350 ℃ of Heating temperatures, argon flow amount 6L/min, the shape appearance figure of the nano tungsten trioxide product of collection.
Embodiment
For technique means, creation characteristic that the present invention is realized, reach purpose and effect is easy to understand, below in conjunction with the drawings and specific embodiments, further set forth the present invention.
The device that the preparation method of continuous production multiform looks tungstic oxide of the present invention adopts as shown in Figure 1, this device comprises quartz glass tube 10, this quartz glass tube 10 comprises inlet mouth 11 and air outlet 12,12 1 ends are provided with carbon cloth 30 in the air outlet, the method that carbon cloth 30 is set is: carbon cloth is rolled into cylindric, is directly pasting in the form of a ring glass tube walls and putting into Glass tubing, attention can not be blocked exit end with carbon cloth, because airshed is larger, the words of blocking affect gas and discharge.This quartz glass tube 10 passes tube furnace 20, so that the middle part of quartz glass tube 10 is positioned at the flat-temperature zone of tube furnace, carbon cloth 30 is 0.3-0.5m apart from the distance of this flat-temperature zone.This device also comprises ceramic crucible 40, and these ceramic crucible 40 interior Uniform Dispersions have ammonium paratungstate 50; After tube furnace 20 heating quartz glass tube 10 reaches assigned temperature to the flat-temperature zone, the ceramic crucible 40 that fills ammonium tungstate 50 pushed place this flat-temperature zone.Simultaneously, the inlet mouth 11 by quartz glass tube 10 passes into argon gas, by the flat-temperature zone, discharges finally by air outlet 12.
Wherein, carbon cloth is commercially available, selects carbon cloth to collect the target nano tungsten trioxide, the one, and high temperature resistant because of it, the 2nd, the convenient powder of collecting.The carbon cloth of all specifications can, but to cut out the carbon cloth of suitable dimension according to the size of Glass tubing.Powder on the carbon cloth is easy to collect, and can reuse after the powder on the carbon cloth is cleaned out.
Embodiment 1
With APT4H
2O is presoma, and the method by thermal decomposed deposition prepares WO
3Nano particle.First with APT4H
2O is dispersed in Al
2O
3In the ceramic crucible, it is the quartz glass tube of 30mm that crucible is placed internal diameter, at the Glass tubing inwall apart from the exit end at tube furnace flat-temperature zone (namely being arranged in the Glass tubing position of tube furnace) 0.3-0.5m place around placing carbon cloth (namely, carbon cloth is rolled into cylindric, directly put in the form of a ring Glass tubing, can not block exit end with carbon cloth, because airshed is larger, the words of blocking affect gas and discharge); Again Glass tubing is placed tube furnace, the reaction unit schematic diagram as shown in Figure 1.With the temperature rise rate heated Tube-furnace to 1250 of 50 ℃/min ℃, when temperature reaches 1250 ℃, crucible is pushed into the tube furnace flat-temperature zone to be heated, and open argon gas to flow 2L/min, behind the insulation 30min, close tube furnace, stop to be blown into argon gas, the air cooling tube furnace is collected the Tungsten oxide 99.999 powder on the carbon cloth to room temperature.XRD figure is composed (Fig. 2) and is shown, product is pure WO
3, without any impurity product.The pattern of product is shown in the scanning electron microscope diagram of Fig. 3 a, 3b, wherein, Fig. 3 a is that magnification is 12500 SEM figure, Fig. 3 b is that magnification is 50000 SEM figure, can find out, product is mainly powder by the less torispherical granulometric composition of size, and the diameter of particle is between 120-620nm, and these torispherical particles are joined together to form the chain form structure.Under these processing condition, the deposition of product (quality of the product of namely collecting and precursor A PT4H
2The ratio of O quality) be about 30%.
In the present embodiment crucible is placed on first the inlet mouth end of Glass tubing, wait be heated to assigned temperature (1250 ℃) after, it is pushed into the flat-temperature zone, be for easy to operate.Also can wait be heated to assigned temperature (1250 ℃) after, put into again crucible, then directly be pushed into the flat-temperature zone.But be put into the flat-temperature zone before can not heating, because tube furnace has certain heating rate, be heated to assigned temperature and need the regular hour, and when being heated to lesser temps (more than 800 ℃), presoma in the crucible also can evaporate, then deposit on the carbon cloth, but the pattern of this moment is uncontrollable, affects purity and the dimensional homogeneity of final product.
Embodiment 2
With APT4H
2O is dispersed in Al
2O
3In the ceramic crucible, it is the quartz glass tube of 30mm that crucible is placed internal diameter, again Glass tubing is placed tube furnace.With the temperature rise rate heated Tube-furnace to 1300 of 50 ℃/min ℃, when temperature reaches 1300 ℃, crucible is pushed into the tube furnace flat-temperature zone heats, and open argon gas to flow 2L/min, behind the insulation 30min, close tube furnace, stop to be blown into argon gas, the air cooling tube furnace is to room temperature, collect the Tungsten oxide 99.999 powder on the carbon cloth, its scanning electronic microscope result finds out that from the morphology observation result product that obtains is the nanometer torispherical particle of size uniform as shown in Figure 4, and granular size is 200-400nm.Under these processing condition, the deposition of product (quality of the product of namely collecting and precursor A PT4H
2The ratio of O quality) be about 50%.
Embodiment 3
With APT4H
2O is dispersed in Al
2O
3In the ceramic crucible, it is the quartz glass tube of 30mm that crucible is placed internal diameter, again Glass tubing is placed tube furnace.With the temperature rise rate heated Tube-furnace to 1350 of 50 ℃/min ℃, when temperature reaches 1350 ℃, crucible is pushed into the tube furnace flat-temperature zone heats, and open argon gas to flow 2L/min, behind the insulation 30min, close tube furnace, stop to be blown into argon gas, the air cooling tube furnace is to room temperature, collect the Tungsten oxide 99.999 powder on the carbon cloth, its scanning electronic microscope result finds out that from the morphology observation result product that obtains is nanometer torispherical particle as shown in Figure 5, and granular size is 200-700nm.Under these processing condition, the deposition of product (quality of the product of namely collecting and precursor A PT4H
2The ratio of O quality) be about 70%.
Embodiment 4
With APT4H
2O is dispersed in Al
2O
3In the ceramic crucible, it is the quartz glass tube of 50mm that crucible is placed internal diameter, again Glass tubing is placed tube furnace.With the temperature rise rate heated Tube-furnace to 1400 of 50 ℃/min ℃, when temperature reaches 1400 ℃, crucible is pushed into the tube furnace flat-temperature zone heats, and open argon gas to flow 2L/min, behind the insulation 30min, close tube furnace, stop to be blown into argon gas, the air cooling tube furnace is to room temperature, collect the Tungsten oxide 99.999 powder on the carbon cloth, its scanning electronic microscope result finds out that from the morphology observation result product that obtains mainly is octahedral structure as shown in Figure 6, and octahedra diagonal lines diameter is at 300-750nm.Under these processing condition, the deposition of product (quality of the product of namely collecting and precursor A PT4H
2The ratio of O quality) be about 70%.
Embodiment 5
With APT4H
2O is dispersed in Al
2O
3In the ceramic crucible, it is the quartz glass tube of 30mm that crucible is placed internal diameter, again Glass tubing is placed tube furnace.With the temperature rise rate heated Tube-furnace to 1350 of 50 ℃/min ℃, when temperature reaches 1350 ℃, crucible is pushed into the tube furnace flat-temperature zone to be heated, and open argon gas to flow 1L/min, behind the insulation 30min, close tube furnace, stop to be blown into argon gas, the air cooling tube furnace is to room temperature, collect the Tungsten oxide 99.999 powder on the carbon cloth, its scanning electronic microscope result finds out that from the morphology observation result product that obtains is the irregular tungstic oxide particle of polyhedron as shown in Figure 7, and the polyhedron catercorner length is about 10nm-2 μ m.Under these processing condition, the deposition of product (quality of the product of namely collecting and precursor A PT4H
2The ratio of O quality) be about 75%.
Embodiment 6
With APT4H
2O is dispersed in Al
2O
3In the ceramic crucible, it is the quartz glass tube of 30mm that crucible is placed internal diameter, again Glass tubing is placed tube furnace.With the temperature rise rate heated Tube-furnace to 1350 of 50 ℃/min ℃, when temperature reaches 1350 ℃, crucible is pushed into the tube furnace flat-temperature zone heats, and open argon gas to flow 4L/min, behind the insulation 30min, close tube furnace, stop to be blown into argon gas, the air cooling tube furnace is to room temperature, collect the Tungsten oxide 99.999 powder on the carbon cloth, its scanning electronic microscope result finds out that from the morphology observation result product that obtains is the nanometer spherical tungstic oxide particle of size uniform as shown in Figure 8, and diameter is 20-200nm.Under these processing condition, the deposition of product (quality of the product of namely collecting and precursor A PT4H
2The ratio of O quality) be about 70%.
Embodiment 7
With APT4H
2O is dispersed in Al
2O
3In the ceramic crucible, it is the quartz glass tube of 30mm that crucible is placed internal diameter, again Glass tubing is placed tube furnace.With the temperature rise rate heated Tube-furnace to 1350 of 50 ℃/min ℃, when temperature reaches 1350 ℃, crucible is pushed into the tube furnace flat-temperature zone heats, and open argon gas to flow 6L/min, behind the insulation 30min, close tube furnace, stop to be blown into argon gas, the air cooling tube furnace is to room temperature, collect the Tungsten oxide 99.999 powder on the carbon cloth, its scanning electronic microscope result finds out that from the morphology observation result product that obtains is the nanometer spherical tungstic oxide particle of size uniform as shown in Figure 9, and diameter is 20-100nm.Under these processing condition, the deposition of product (quality of the product of namely collecting and precursor A PT4H
2The ratio of O quality) be about 65%.
By above-described embodiment as can be known, when temperature when lower (as being 1250 ℃, 1300 ℃), the deposition of product (ratio of the quality of the product of namely collecting and precursor A PT4H2O quality) is lower, and when temperature during greater than 1350 ℃, the product deposition can reach 70%; In addition, the pattern of product is also different during differing temps, and shown in Fig. 7-9, embodiment 3,5-7, along with the increase of gas flow, the size of product reduces gradually, and product is tending towards forming spheroidal particle.
Different processing condition obtain the product of different-shape, and the product of different-shape can be used in different fields.Generally speaking, sphere is reasonable.When temperature of reaction is 1350 ℃, when gas flow is 4-6L/min, can obtain the ball shaped nano tungstic oxide of size uniform.
Although content of the present invention has been done detailed introduction by above preferred embodiment, will be appreciated that above-mentioned description should not be considered to limitation of the present invention.After those skilled in the art have read foregoing, for multiple modification of the present invention with to substitute all will be apparent.Therefore, protection scope of the present invention should be limited to the appended claims.
Claims (8)
1. produce continuously multi-morphology nano tungstic oxide material preparation method for one kind, it is characterized in that, the method comprises following steps:
Step 1, get the quartz glass tube (10) that comprises inlet mouth (11) and air outlet (12), place carbon cloth (30) at quartz glass tube (10) near the inner wall surrounding of air outlet (12) end, this quartz glass tube traverse that carbon cloth is housed is placed tube furnace (20);
Step 2 makes tube furnace (20) heating quartz glass tube (10) to assigned temperature;
Step 3, the ceramic crucible (40) that will fill ammonium paratungstate (50) pushes in the above-mentioned Glass tubing, makes it to be in the flat-temperature zone that is heated to assigned temperature, is blown into argon gas;
Step 4 behind the insulation 40min-60min, is closed tube furnace (20), stops to be blown into argon gas;
Step 5 is taken out carbon cloth (30), collects the reaction product of deposition on it, obtains the nano tungsten trioxide particle of multiform looks, and takes out ceramic crucible (40);
Step 6, repeating step 1-5 several times: namely again place carbon cloth at the Glass tubing inner wall surrounding, the crucible that fills ammonium paratungstate is moved to the flat-temperature zone, again open argon gas, the reaction of beginning next round realizes producing continuously.
2. continuous production multi-morphology nano tungstic oxide material preparation method as claimed in claim 1 is characterized in that, described step 1 also comprises the step of cleaning the silica glass inside pipe wall.
3. continuous production multi-morphology nano tungstic oxide material preparation method as claimed in claim 2 is characterized in that, described silica glass length of tube is 1-1.5m, and diameter is 0.3-0.5m.
4. continuous production multi-morphology nano tungstic oxide material preparation method as claimed in claim 1 is characterized in that, described carbon cloth is placed on the place apart from flat-temperature zone 0.3-0.5m.
5. continuous production multi-morphology nano tungstic oxide material preparation method as claimed in claim 1 is characterized in that, in the described step 2, the temperature rise rate of heated Tube-furnace is 50 ℃/min, and described assigned temperature is 1250 ℃-1400 ℃.
6. continuous production multi-morphology nano tungstic oxide material preparation method as claimed in claim 1 is characterized in that, in the described step 3, ammonium paratungstate (50) is dispersed in the ceramic crucible (40).
7. such as claim 1 or 6 described continuous production multi-morphology nano tungstic oxide material preparation methods, it is characterized in that, in the described step 3, argon flow amount is 1L/min-6L/min.
8. continuous production multi-morphology nano tungstic oxide material preparation method as claimed in claim 1 is characterized in that, described multi-morphology nano tungstic oxide material comprises following form and specification: torispherical tungstic oxide particle, diameter are 100nm-700nm; Spherical tungstic oxide particle, diameter is 20-200nm; Octahedral bodily form tungstic oxide particle, octahedra catercorner length is less than 1 μ m; The irregular tungstic oxide particle of polyhedron, the polyhedron catercorner length is about 10nm-2 μ m.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104909410A (en) * | 2015-06-18 | 2015-09-16 | 江西稀有金属钨业控股集团有限公司 | Preparation method of low-specific-surface tungsten trioxide |
| CN105642274A (en) * | 2016-01-25 | 2016-06-08 | 河南科技学院 | Octahedral structure WO3 photocatalyst and preparation method thereof |
| CN111715209A (en) * | 2020-05-18 | 2020-09-29 | 浙江工业大学 | Gas phase preparation method of tungsten trioxide/graphite felt composite material |
| CN112846211A (en) * | 2020-12-31 | 2021-05-28 | 崇义章源钨业股份有限公司 | High-compact-strength tungsten powder and preparation method thereof |
| CN113130905A (en) * | 2021-04-16 | 2021-07-16 | 陕西科技大学 | Ultra-small cobalt sulfide nanosheet/carbon cloth composite material and preparation method thereof |
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| WO2012129782A1 (en) * | 2011-03-30 | 2012-10-04 | 厦门金鹭特种合金有限公司 | Preparation method of industrial purple nano-needle tungsten oxide |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104909410A (en) * | 2015-06-18 | 2015-09-16 | 江西稀有金属钨业控股集团有限公司 | Preparation method of low-specific-surface tungsten trioxide |
| CN105642274A (en) * | 2016-01-25 | 2016-06-08 | 河南科技学院 | Octahedral structure WO3 photocatalyst and preparation method thereof |
| CN105642274B (en) * | 2016-01-25 | 2018-07-06 | 河南科技学院 | A kind of octahedral structure WO3 photochemical catalysts and preparation method thereof |
| CN111715209A (en) * | 2020-05-18 | 2020-09-29 | 浙江工业大学 | Gas phase preparation method of tungsten trioxide/graphite felt composite material |
| CN111715209B (en) * | 2020-05-18 | 2023-04-07 | 浙江工业大学 | Gas phase preparation method of tungsten trioxide/graphite felt composite material |
| CN112846211A (en) * | 2020-12-31 | 2021-05-28 | 崇义章源钨业股份有限公司 | High-compact-strength tungsten powder and preparation method thereof |
| CN113130905A (en) * | 2021-04-16 | 2021-07-16 | 陕西科技大学 | Ultra-small cobalt sulfide nanosheet/carbon cloth composite material and preparation method thereof |
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