The invention discloses a method for preparing a tungsten oxide nano single crystal by a sol-gel method. The method comprises the following steps of: preparing macromolecular liquor which can form sol-gel; mixing the macromolecular liquor with ammonium metatungstate liquor; insulating for a certain time at the temperature in the range of 500-900 DEG C; and then performing furnace cooling to obtain yellow powder WO3 nano single crystal powder.

The average size of the WO3 nano single crystal rod prepared by the invention is as follows: 200-500nm in length and 10-30nm in diameter. The nano single crystal rod is stable and uniform and can be used for preparing high quality one-dimensional WO3 compound materials.


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The invention relates to a method for preparing tungsten trioxide by utilizing tungsten concentrate.

The method comprises the steps of: mixing and calcining tungsten concentrate and silicon dioxide to obtain calcined product containing the tungsten trioxide. By utilizing the method, the tungsten trioxide can be prepared in one step by utilizing the tungsten concentrate, so that the process flow can be shortened, the waste acid and alkaline liquid caused by the utilization of sodium hydroxide and hydrochloric acid in the prior art can be effectively avoided, the environment is free from being polluted, and high-efficient and clean production and zero-emission of waste water and waste gas can be realized.

A method for preparing the tungsten tungsten trioxide, characterized by comprising: dividing the concentrates were mixed with crab and calcined silica, to obtain a tungsten trioxide containing fired product.




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The invention discloses a manufacturing method of tungsten oxide through holes.

The manufacturing method of the tungsten oxide through holes comprises the following steps:

(1) Forming tungsten through holes according to an existing technology, filling tungsten, and carrying out tungsten planarization.

(2) Forming tungsten oxide through oxidation.

(3) Depositing a layer of oxidation film or a dielectric substance layer which can achieve the same effect on the surface of the tungsten oxide formed in the step (2) by adopting chemical vapor deposition.

(4) Grinding the oxidation film or the dielectric substance layer which can achieve the same effect to expose the tungsten oxide by adopting a grinding mode or a method of dry method back carving, and thus forming the tungsten oxide through holes.

The manufacturing method of the tungsten oxide through holes solves the problem of leakage access formed between a top metal layer and a tungsten through hole titanium nitrogen compound barrier layer, and can improve a resistive random access memory erase operation window and reliability.


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Provided is a preparation method of industrial purple nano-needle tungsten oxide, wherein ammonium paratungstate 5(NH4)2O⋅12WO3⋅5H2O, tungstic acid mWO3⋅nH2O (m≥1, n≥1), or oxides of tungsten WOx (2≤x≤3) is used as raw material, and a declined rolling furnace pipe is employed. At the inlet of the furnace pipe, the raw material is conveyed from the inlet into the heated furnace pipe by a feeder unit, and is moved gradually from a low temperature area to a high temperature area under the rotation of the declined furnace pipe; the raw material is reduced by H2 at the high temperature area, to obtain purple nano-needle tungsten oxide WO2.72 , the obtained tungsten oxide WO2.72 is moved gradually toward the outlet under the rotation of the declined furnace pipe, and is discharged from the outlet, as well cooled to about room temperature.

The method for preparing a nano-needle purple tungsten oxide, wherein is paratungstate 5 (NH 4) 2 O · 12WO 3 · 5H 2 O as raw materials, the following steps:

A, With a feed device from the feed end of the tungsten Chung-ammonium 5 (NH 4 of 5) 2 O Visual & 12WO 3 · 5H 2 O from the feed inlet pushed into to the heated furnace tube, in the role of rotation of the tilt furnace tube, gradually from low temperature zone to move to the high temperature zone;

B, Ammonium paratungstate (NH 4) 2 O · 12WO 3 · 5H 2 O was heated to decomposition of the tungsten trioxide WO 3, ammonia NH 3, and water vapor H 2 O;

C, In the furnace tube so that ammonia NH 3 is thermally decomposed to generate a reducing gas of hydrogen H 2;

D, The material in the rotation of the furnace tube inclined to continue to move to the high-temperature region, when the when material temperature continues, the tungsten trioxide WO 3 is hydrogen H 2 gradual reduction generated purple oxide of tungsten WO 2.72.




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Preparation of ultrafine kind of tungsten oxide template method steps as follows:

(1) 1-50mg a diameter of 2-30nm, the number of layers of 1-30 layers of carbon nanotubes added to 50-30mL of anhydrous ethanol, ultrasonic dispersion 24h , to obtain a solution A;

(2) 250mg of sodium tungstate crystals were dissolved in the 50-100mL volume ratio of 2:3 mixture of ethanol and distilled water, and then added dropwise at a concentration of 36.5% hydrochloric acid 0.1-20mL, a precipitate B;

(3) A and mixture B, dispersing 5-48h, filtered and dried to give a carbon nanotube / tungsten oxide precursor C, will be placed in a horizontal quartz reactor, wherein the charge to the oxygen, the reaction temperature is 400-1100 ℃, holding time 10-24h, cooling, to obtain a particle size of the tungsten oxide particles of 10-500nm. The present invention is easy to get raw materials, low cost, environmental pollution.  

Preparation process is simple, small particles of tungsten oxide obtained high purity, uniform distribution.




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The invention, relating to the field of tungsten trioxide crystals, concretely discloses a method for preparing tungsten trioxide crystals with controllable growth of the crystal surfaces. The method is characterized by using tungsten boride as a precursor by wet chemical process and carrying out hydrothermal growth of the crystal surfaces to expose tungsten trioxide crystals with different proportions, so that the problem of providing tungsten trioxide catalysts with different redox abilities for different reaction systems can be solved; putting the precursor in a reaction vessel filled with an aqueous nitric acid solution, and carrying out heat treatment to obtain crystal surface-dominated tungsten trioxide crystals {002}; putting the precursor in a reaction vessel filled with a hydrofluoric acid solution or a hydrofluoric acid ethanol solution or a mixed solution of aqueous hydrofluoric acid and ethanol, carrying out heat treatment to obtain cubic hydrogen tungsten bronze crystals, and heating the hydrogen tungsten bronze crystals in air to obtain tungsten trioxide crystals with identical crystal surface proportion {002}, {200}, {020}. According to the invention, tungsten trioxide crystals with regular morphology, different crystal surface proportions, and good ability of oxygen production by water splitting can be prepared.

A tungsten trioxide controlled crystal growth plane preparation, characterized in dry: without any treatment with a commercial tungsten boride precursors, put it in a reaction vessel equipped with a nitric acid aqueous solution, the reaction After sealing the autoclave, a heat treatment oven, remove the reacted sample, washed with deionized water and dried, resulting in the nitric acid system, to give (002) crystal plane dominated crane trioxide crystals; or without any treatment in a commercial Crane boride as the precursor, put it with hydrofluoric acid or hydrofluoric acid aqueous solution or hydrofluoric acid in water, alcohol ko, ko alcohol mixed solution of a reaction vessel, the reaction was sealed, into the oven heating treatment, the reaction samples taken, washed with deionized water and drying, heat treatment in air, resulting in three crystal hydrofluoric acid systems face in equal proportions to obtain tungsten trioxide crystals.




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The invention provides a synthesis method of tungsten trioxide, belongs to the technical field of inorganic synthesis chemistry, and particularly relates to the synthesis method of the tungsten trioxide. The synthesis method comprises the following steps of: taking sodium tungstate dihydrate and sodium chloride as raw materials; utilizing hydrochloric acid to adjust a pH (Potential of Hydrogen) value of a reaction system to adjust the pH value to 1.5-3.0; carrying out hydrothermal reaction at 170-190 DEG C for 22-28 hours; and washing, centrifuging and drying to obtain tungsten trioxide powder. The obtained tungsten trioxide powder has different shapes and different photoelectric properties. According to the synthesis method disclosed by the invention, a one-step hydrothermal synthesis method is adopted, so that the operation is simple, the repetitiveness is good and the raw material cost is low; and the pH value is simply adjusted to obtain the tungsten trioxide powder with the different shapes and the different photoelectric properties, and the photocatalytic degradation efficiency on an organic dye is higher.

A method of synthesis of tungsten trioxide, the synthesis process is as follows: the sodium tungstate dihydrate and sodium chloride were added at a molar ratio of 1:2 in distilled water, the sodium tungstate dihydrate in distilled water at a concentration range of O. 016mol / L "0. 067mol / L between the ultrasonic 5min, under magnetic stirring, using hydrochloric acid to adjust pH of the solution 1. Γ3. O, stirring was continued for lh, to obtain a precursor solution; said precursor solution was transferred to the reactor, at 17 (Tl90 ° C hydrothermal reaction of 22 ~ 28h, cooled to room temperature, the resulting products were washed with distilled water and ethanol, centrifuged and dried to obtain the tungsten trioxide powder.




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The invention relates to nanoscale tungsten oxide (WO3) powder and a pyrolysing preparation method thereof, wherein an optimized raw material composition consisting of ammonium paratungstate (APT), citric acid and ammonia in corresponding proportion is adopted, the molar ratio of APT and citric acid is 1.5, and parameters of a preparation process matched are used. The flow of oxygen based on per gram of precursor is 55ml/min, and the thermal treatment temperature is 520 DEG C, so that WO3 nanopowder with uniformly distributed grain size is obtained.

A pyrolysis Method tungsten oxide (WO3) nano powder, characterized in that: prepared by the following steps:

First, the selection of particle size of about 5μπι purity ammonium paratungstate (APT) as a reaction raw material, distilled water was added to the reaction vessel , and the mixture was stirred using a magnetic stirrer, a solution of citric acid was added with stirring;
Secondly, waiting citric acid solution evenly dissolved and mixed, while stirring, high-purity ammonium paratungstate (APT) to the reaction vessel;

Third, high dried Fourth, the reaction solution was placed in the evaporation vessel was concentrated and concentrated to give a concentrated solution in the drying apparatus at 150-160 ° C under;

Fourth,pure after addition of aqueous ammonia, ammonium paratungstate (APT) addition was complete, the reaction solution was stirred to obtain a uniform to obtain a precursor;

Fifth, the precursors were pulverized in a milling device, and then placed in a crucible of oxygen through the heat treatment is performed to give the final tungsten oxide (WO3) nanopowder; wherein said high purity ammonium paratungstate (APT) purity greater than 99.9wt%, the amount of citric acid was added to a solution of ammonium paratungstate (APT) and the calculated molar ratio of citric acid to 3; the ammonia concentration of 30%; the stirring speed was 180-200r/min; When the heat treatment, the precursor calculated per g of oxygen flow 50_60ml/min, a temperature of 500-520 ° C, time is 1.2-1.5h0.




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The invention relates to a method for dissolving ammonium paratungstate and/or tungsten oxide.

The method for dissolving the ammonium paratungstate and/or the tungsten oxide comprises the following steps:

(1) Mixing the ammonium paratungstate and/or the tungsten oxide with ammonia water to obtain a mixture;

(2) Stirring and heating the obtained mixture so as to completely dissolve the ammonium paratungstate and/or the tungsten oxide and obtain the solution containing ammonium tungstate.

By the method, unqualified products generated in the tungsten smelting process can be recycled with low cost, the basis is provided for research and development of a new tungsten smelting technology and new products, and the method is short in process flow, high in efficiency and simple in equipment and operation.




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The invention provides a preparation method of hollow porous tungsten oxide spheres and belongs to the field of functional materials.

The method comprises the following steps of:

(1) Dissolving ammonium tungstate and/or ammonium metatungstate in water and stirring thoroughly to produce a solution with concentration of 1 g/L to 200 g/L;

(2) Preparing hollow powder of ammonium tungstate, ammonium metatungstate or a mixture thereof by the spray drying of spray-drying equipment;

(3) Putting the powder in an electric furnace, heating up to a temperature of 400 DEG C to 1000 DEG C, and preserving heat for 15 minutes to 180 minutes to obtain hollow porous tungsten oxide spheres.

The method needs simple equipment, shortens the process flow, increases the preparation efficiency and is simple and feasible for preparing porous tungsten oxide nano-spheres. The specific surface area of the hollow porous tungsten oxide spheres prepared by the method reaches 15 m<2>/g to 30 m<2>/g. The preparation method has good prospects for industrial applications.


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