CN104556038A - Synthetic method of spherical tungsten carbide powder - Google Patents
Synthetic method of spherical tungsten carbide powder Download PDFInfo
- Publication number
- CN104556038A CN104556038A CN201510032570.3A CN201510032570A CN104556038A CN 104556038 A CN104556038 A CN 104556038A CN 201510032570 A CN201510032570 A CN 201510032570A CN 104556038 A CN104556038 A CN 104556038A
- Authority
- CN
- China
- Prior art keywords
- synthetic method
- calcine
- spherical
- hours
- tungsten
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Landscapes
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a synthetic method of spherical tungsten carbide powder. The synthetic method comprises the steps of preparing a spherical skeleton by taking a glucose solution as a carbon source template; and then preparing the spherical tungsten carbide powder by taking a soluble tungsten salt such as WCl6, ammonium metatungstate (AMT), sodium tungstate and potassium tungstate as a tungsten source at a certain technical condition and molar ratio.
Description
Technical field
The present invention relates to a kind of synthetic method of tungsten carbide powder, especially a kind of synthetic method of spherical carbide tungsten powder.
Technical background
Spherical WC powder, has high-hardness, wearable, acid-fast alkali-proof, high chemical stability, has potential using value widely in anode of fuel cell, cathode catalyst material, in gas sensor, petroleum catalyst, photocatalyst material.
The existing preparation method preparing tungsten carbide powder directly carries out high-temperature calcination tungsten powder and carbon black, and the tungsten carbide powder out-of-shape obtained, can not meet the requirement of special dimension.
Summary of the invention
The object of the present invention is to provide a kind of synthetic method of spherical carbide tungsten powder, the present invention adopts glucose solution as carbon source template, prepares spherical skeleton using soluble tungsten salt as tungsten source, as WCl
6, ammonium metawolframate (AMT), sodium wolframate, potassium wolframate etc. under certain technical qualification and mol ratio condition, prepare the spherical wolfram carbide powder of high-hardness, wearable, acid-fast alkali-proof, high chemical stability.
The present invention is achieved like this, a kind of synthetic method of spherical carbide tungsten powder, be the soluble tungsten source of 1:20-40 and the D/W of mass concentration 5-10% by mol ratio, react 24 hours in 200 DEG C of autoclaves, air-dry under temperature 80-100 DEG C of condition after filtration, then calcine in 800-1000 DEG C of logical hydrogen 14 pipe furnace 8-10 hour preparation reduction before aggressiveness, then in 1000-1500 DEG C of molybdenum wire furnace, calcine 3-5 hour, carry out carbonization, to obtain final product.
Wherein soluble tungsten source is WCl
6, ammonium metawolframate, sodium wolframate, one of any in potassium wolframate.
Technological merit of the present invention: synthesis is simple, and be easy to industrialization, product purity is high, and (tungsten carbide content is greater than 90%, WC
2content is less than 1%, and uncombined carbon is less than 2%), the spherical tungsten carbide of high rigidity (mohs hardness is 9), high abrasion, acid-fast alkali-proof, high chemical stability.
figure of description
Fig. 1 and Fig. 2 is the spherical wolfram carbide powder SEM figure of high-hardness, wearable, acid-fast alkali-proof, high chemical stability.
Embodiment
Embodiment 1
A kind of synthetic method of spherical carbide tungsten powder, be the soluble tungsten source of 1:20 and the D/W of mass concentration 5% by mol ratio, react 24 hours in 200 DEG C of autoclaves, air-dry under temperature 80 DEG C of conditions after filtration, again in 800 DEG C of logical hydrogen 14 pipe furnaces calcine 8 hours preparation reduction before aggressiveness, then calcine 3 hours in 1000 DEG C of molybdenum wire furnaces, carry out carbonization, to obtain final product.
Wherein soluble tungsten source is WCl
6.
Embodiment 2
A kind of synthetic method of spherical carbide tungsten powder, be the soluble tungsten source of 1:30 and the D/W of mass concentration 7% by mol ratio, react 24 hours in 200 DEG C of autoclaves, air-dry under temperature 90 DEG C of conditions after filtration, again in 900 DEG C of logical hydrogen 14 pipe furnaces calcine 9 hours preparation reduction before aggressiveness, then in 1200 DEG C of molybdenum wire furnaces, calcine 3-5 hour, carry out carbonization, to obtain final product.
Wherein soluble tungsten source is ammonium metawolframate.
Embodiment 3
A kind of synthetic method of spherical carbide tungsten powder, be the soluble tungsten source of 1:25 and the D/W of mass concentration 8% by mol ratio, react 24 hours in 200 DEG C of autoclaves, air-dry under temperature 85 DEG C of conditions after filtration, again in 950 DEG C of logical hydrogen 14 pipe furnaces calcine 9 hours preparation reduction before aggressiveness, then calcine 4 hours in 1300 DEG C of molybdenum wire furnaces, carry out carbonization, to obtain final product.
Wherein soluble tungsten source is sodium wolframate.
Embodiment 4
A kind of synthetic method of spherical carbide tungsten powder, be the soluble tungsten source of 1:40 and the D/W of mass concentration 10% by mol ratio, react 24 hours in 200 DEG C of autoclaves, air-dry under temperature 100 DEG C of conditions after filtration, again in 1000 DEG C of logical hydrogen 14 pipe furnaces calcine 10 hours preparation reduction before aggressiveness, then calcine 5 hours in 1500 DEG C of molybdenum wire furnaces, carry out carbonization, to obtain final product.
Wherein soluble tungsten source is potassium wolframate.
Embodiment 5
A kind of synthetic method of spherical carbide tungsten powder, be the soluble tungsten source of 1:15 and the D/W of mass concentration 4% by mol ratio, react 24 hours in 200 DEG C of autoclaves, air-dry under temperature 70 C condition after filtration, again in 700 DEG C of logical hydrogen 14 pipe furnaces calcine 7 hours preparation reduction before aggressiveness, then calcine 2 hours in 900 DEG C of molybdenum wire furnaces, carry out carbonization, to obtain final product.
Wherein soluble tungsten source is ammonium metawolframate.
Embodiment 6
A kind of synthetic method of spherical carbide tungsten powder, be the soluble tungsten source of 1:45 and the D/W of mass concentration 11% by mol ratio, react 24 hours in 200 DEG C of autoclaves, air-dry under temperature 120 DEG C of conditions after filtration, again in 1100 DEG C of logical hydrogen 14 pipe furnaces calcine 11 hours preparation reduction before aggressiveness, then calcine 6 hours in 1600 DEG C of molybdenum wire furnaces, carry out carbonization, to obtain final product.
Wherein soluble tungsten source is WCl
6.
The spherical wolfram carbide powder purity that each embodiment obtains is as shown in the table:
As can be seen from upper table data, the purity of the embodiment 1-4 within present invention process scope is apparently higher than the embodiment 5 and 6 outside processing range, especially best with the purity of embodiment 2, the specific processing parameter of visible employing the present invention, improves the purity of spherical tungsten carbide.
Claims (3)
1. the synthetic method of a spherical carbide tungsten powder, it is characterized by: be the soluble tungsten source of 1:20-40 and the D/W of mass concentration 5-10% by mol ratio, react 24 hours in 200 DEG C of autoclaves, air-dry under temperature 80-100 DEG C of condition after filtration, calcine in 800-1000 DEG C of logical hydrogen 14 pipe furnace again 8-10 hour preparation reduction before aggressiveness, then in 1000-1500 DEG C of molybdenum wire furnace, calcine 3-5 hour, carry out carbonization, to obtain final product.
2. the synthetic method of a kind of spherical carbide tungsten powder as claimed in claim 1, is characterized by: wherein soluble tungsten source is WCl
6, ammonium metawolframate, sodium wolframate, one of any in potassium wolframate.
3. the synthetic method of a kind of spherical carbide tungsten powder as claimed in claim 1 or 2, it is characterized by: be the soluble tungsten source of 1:30 and the D/W of mass concentration 7% by mol ratio, react 24 hours in 200 DEG C of autoclaves, air-dry under temperature 90 DEG C of conditions after filtration, again in 900 DEG C of logical hydrogen 14 pipe furnaces calcine 9 hours preparation reduction before aggressiveness, then in 1200 DEG C of molybdenum wire furnaces, calcine 3-5 hour, carry out carbonization, to obtain final product;
Wherein soluble tungsten source is ammonium metawolframate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510032570.3A CN104556038B (en) | 2015-01-23 | 2015-01-23 | A kind of synthetic method of spherical carbide tungsten powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510032570.3A CN104556038B (en) | 2015-01-23 | 2015-01-23 | A kind of synthetic method of spherical carbide tungsten powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104556038A true CN104556038A (en) | 2015-04-29 |
| CN104556038B CN104556038B (en) | 2016-08-31 |
Family
ID=53073245
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510032570.3A Active CN104556038B (en) | 2015-01-23 | 2015-01-23 | A kind of synthetic method of spherical carbide tungsten powder |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104556038B (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105016341A (en) * | 2015-07-15 | 2015-11-04 | 浙江大学 | Hollow carbide nanosphere with high specific surface area and preparation method thereof |
| CN108794928A (en) * | 2018-06-22 | 2018-11-13 | 安徽索亚装饰材料有限公司 | A kind of anti-mildew PVC foam Wallpaper paste material |
| CN108899559A (en) * | 2018-06-19 | 2018-11-27 | 华东师范大学 | A kind of anode of fuel cell hydrogen oxidation catalyst and preparation method thereof |
| CN110054188A (en) * | 2018-05-11 | 2019-07-26 | 南方科技大学 | Nano silicon carbide tungsten particle and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102887512A (en) * | 2012-10-18 | 2013-01-23 | 南昌大学 | Method for preparing nano-tungsten carbide |
-
2015
- 2015-01-23 CN CN201510032570.3A patent/CN104556038B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102887512A (en) * | 2012-10-18 | 2013-01-23 | 南昌大学 | Method for preparing nano-tungsten carbide |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105016341A (en) * | 2015-07-15 | 2015-11-04 | 浙江大学 | Hollow carbide nanosphere with high specific surface area and preparation method thereof |
| CN110054188A (en) * | 2018-05-11 | 2019-07-26 | 南方科技大学 | Nano silicon carbide tungsten particle and preparation method thereof |
| CN108899559A (en) * | 2018-06-19 | 2018-11-27 | 华东师范大学 | A kind of anode of fuel cell hydrogen oxidation catalyst and preparation method thereof |
| CN108899559B (en) * | 2018-06-19 | 2021-10-12 | 华东师范大学 | Fuel cell anode hydrogen oxidation catalyst and preparation method thereof |
| CN108794928A (en) * | 2018-06-22 | 2018-11-13 | 安徽索亚装饰材料有限公司 | A kind of anti-mildew PVC foam Wallpaper paste material |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104556038B (en) | 2016-08-31 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104556038B (en) | A kind of synthetic method of spherical carbide tungsten powder | |
| CN103539210B (en) | A kind of preparation method of cobalt molybdate crystallite | |
| CN102310199B (en) | Method for preparing WC-Co nano composite powder by in situ reduction and carbonization | |
| CN110228797B (en) | Method for preparing two-dimensional molybdenum nitride or tungsten nitride nanosheets at low cost | |
| Bion et al. | The role of preparation route upon the ambient pressure ammonia synthesis activity of Ni2Mo3N | |
| CN103920887B (en) | A kind of method preparing WC-Co powder used for hot spraying | |
| CN105174244B (en) | A kind of preparation method of CNT | |
| CN105217633A (en) | A kind of preparation method with the nano silicon carbide two molybdenum sheet sprills of regular hexagon structure | |
| CN105036195B (en) | A kind of tungsten disulfide/molybendum disulfide complexes and preparation method thereof | |
| Singh et al. | Direct synthesis of nanocrystalline tungsten carbide from scheelite ore by solid state reaction method | |
| CN104174414B (en) | A kind of molybdenum bisuphide/titanium dioxide compound and preparation method thereof | |
| CN107855133A (en) | A kind of method for preparing support type little particle Au catalyst | |
| Yang et al. | Synthesis of ultrafine WC-10Co composite powders with carbon boat added and densification by sinter-HIP | |
| CN104528787A (en) | Method for preparing small-particle-size aluminium oxide powder | |
| CN108866418A (en) | A kind of preparation method of oxide dispersion intensifying iron-cobalt-nickel medium entropy alloy | |
| Zhou et al. | Preparation of Ni–Mo–C/Ti (C, N) coated powders and its influence on the microstructure and mechanical properties of Ti (C, N)-based cermets | |
| CN102699337B (en) | Method for synthesizing and preparing hard alloy powder by mixing original powder and regenerated powder | |
| Ma et al. | Advanced inorganic nitride nanomaterials for renewable energy: a mini review of synthesis methods | |
| Rico et al. | Synthesis and ammonolysis of nickel and cobalt tungstates and their characterisation | |
| CN105603233A (en) | Novel NiAl-based self-lubricating material using Ag and Mo-B-O-Si four-element platy crystal as composite lubricating phase and reinforcing phase and preparation method of novel NiAl-based self-lubricating material | |
| CN105154169A (en) | Tungsten disulfide/molybdenum disulfide/montmorillonite compound and preparation method thereof | |
| CN104190913A (en) | WC mixed powder production method used for producing fine-particle alloy | |
| CN107746057B (en) | Preparation method of superfine molybdenum carbide | |
| CN108163857A (en) | A kind of method that molybdenum carbide is prepared using carbon thermal reduction molybdenum sulfide | |
| CN106583707B (en) | A kind of preparation method of the super thick WC-Co composite powder of high fluidity |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |