CN105217633B - Method for preparing nano molybdenum carbide (Mo2C) flake powder with regular-hexagon structure - Google Patents
Method for preparing nano molybdenum carbide (Mo2C) flake powder with regular-hexagon structure Download PDFInfo
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Abstract
The invention relates to a method for preparing nano molybdenum carbide (Mo2C) flake powder with a regular-hexagon structure. According to the method, water-soluble ammonium dimolybdate (or ammonium heptamolybdate) and glucose (or saccharose) are respectively adopted as a molybdenum source raw material and a carbon source raw material; and through precursor solution drying, molecular-level uniform mixing of all elements in a reactant system is realized, the temperature for carbothermal reduction reaction is lowered, the reaction time for the carbothermal reduction reaction is shortened, and the synthesis of nano Mo2C is realized. In addition, during the reaction, a molten halogenating agent provides a uniformly-heated stable-state system for a reaction system, so that the homogeneous growth of regular-hexagonal nano flaky Mo2C is promoted.
Description
Technical field
The invention belongs to inorganic non-metallic powder body material preparation field, and in particular to a kind of that there is regular hexagon laminated structure
Two molybdenum powder of nano silicon carbide preparation method.
Background technology
Dimolybdenum carbide（Mo2C）The features such as because having high fusing point, hardness height, good electrical and thermal conductivity performance and good corrosion resistance,
The fields such as various high temperature resistants, wear-resisting and chemical resistant material are had been widely used at present.Mo2C is mutually added to frequently as second
The wearability of workpiece can be improved in ferrous materials, also can be added to WC base cemented carbides and Ti (C, N as important component）Base
Improve microscopic structure and mechanical property in cermet system.In addition, can also be individually used for making wear-resistant, anti scuffing coating.
Mo2C also because of electronic structure and catalysis characteristics which has similar noble metal, is described as " quasi- platinum catalyst ", has been widely used as hydrogen
The reaction of participation such as alkane isomerization, unsaturated hydrocarbonsHydrogenation, the reaction such as hydrodesulfurization and denitrogenation and synthesis ammonia catalyst, it is special
Be not molybdenum the expensive metal of carbide it is cheap and and with excellent anti-sulfur poisonous performance, therefore Mo2C catalyst quite induces one to look steadily
Mesh.
The synthesis of carbide is generally required to be carried out at high temperature.According to the difference of type of feed, the powder stock master containing molybdenum
There are three classes：Elemental metals molybdenum, the oxide of molybdenum（Such as MoO3）With the presoma of molybdenum（Such as ammonium molybdate）.Obviously, by molybdenum powder and carbon
The mixture high temperature cabonization of powder is not actual, and the temperature not only reacted is high, and expensive starting materials.By MoO3Powder is mixed with carbon dust
Carbon thermal reduction is synthesis Mo afterwards2The topmost commercial run of C powder；The method is due to adopting MoO3Powder is raw material, cost compared with
It is low, but synthesis temperature is still higher, such as the Chinese patent of Application No. 96115598.1《The production method of molybdenum carbide》Disclose
A kind of production method：By MoO3Mix with C powder, at 1600 DEG C, carbon thermal reduction 2h prepares Mo of the phosphorus content more than 12%2C powder
End.Carbon thermal reduction synthesis Mo is carried out using the presoma of molybdenum for raw material2C powder, its cost of material are minimum, and can obviously reduce
Reaction temperature, beneficial to the synthesis of nanometer powder, such as document《Materials Research Bulletin, Volume 43,
Issues 8–9, 2008, Pages 2036-2041》It is raw material that report Manish Patel et al. utilize ammonium molybdate and sucrose
The carbon thermal reduction at 1200 DEG C is prepared for nanometer powder.
In these methods, there is a problem of that some cannot overcome, such as 1）Building-up process is generally in vacuum, or H2、Ar
Deng carrying out in protective atmosphere；2）Carbon thermal reduction institute calorific requirement is mainly provided by heating element heater radiant heat transfer, and product is heated
Inside and outside inequality；3）The Mo of synthesis2C-shape is irregular, the powdered substance that particle size distribution range is wider, brings all to practical application
Inconvenience more.
The content of the invention
For deficiencies of the prior art, it is an object of the invention to provide a kind of raw material is heated evenly, reacts
Temperature is low and finished product have regular hexagon structure two molybdenum sheet sprills of nano silicon carbide preparation method.
To achieve these goals, the technical solution used in the present invention is as follows：
A kind of preparation method of the two molybdenum sheet sprills of nano silicon carbide with regular hexagon structure, comprises the following steps：
1）Ammonium molybdate, carbonaceous reducing agent are placed in distilled water as raw material, stir to being completely dissolved that to obtain presoma molten
Liquid；Wherein, totally 50 parts of two kinds of material quality numbers, ammonium molybdate is 27.94-30.39 parts, and carbonaceous reducing agent is 19.61-22.06
Part；The chemical equation that this preparation method is subsequently related to is 2MoO3 (s)+7C (s)=Mo2C (s)+6CO (g), thus it is theoretical
The mol ratio of upper Mo and C is 2：7, prepare ammonium molybdate, carbonaceous reducing agent accordingly.Consider the carbonaceous such as glucose also in practice
Former agent has carbon depletion in thermal decomposition process, therefore C needs suitably excessively, and the amount of being actually added into of usual C is more slightly higher than theoretical mixed carbon comtent,
For 2：8~10.Carbon has two as reducing agent Main Function：One is MoO3Simple substance Mo is reduced into, two are given birth to simple substance Mo carbonizations
Into Mo2C。
2）By step 1）The precursor solution for obtaining is placed in air dry oven, is dried 2-5h, obtains at 60-120 DEG C
Powder presoma compound；
3）By step 2）The powder presoma compound for obtaining is placed in quartz tube furnace, in the bar of inert gas shielding
Under part, 0.5-1h is calcined at 300-400 DEG C, obtain " molybdenum oxide carbon " mixing that each element is well mixed in molecular level
Thing；Described inert gas is argon gas；
4）By step 3）" molybdenum oxide carbon " mixture for obtaining is filled into ceramic crucible, then is covered simultaneously with halogenating agent powder
Crucible is filled, the addition of halogenating agent powder is completely covered " molybdenum oxide carbon " mixing in ceramic crucible with which in melting
Thing is defined；Then crucible is placed in heating furnace, is incubated 1-4h at a temperature of 750-950 DEG C, so that above-mentioned substance is in ceramics
Carry out reducing in crucible, carburizing reagent generate carbonization synthetic product；Described halogenating agent be sodium chloride, potassium chloride, calcium chloride,
The mixture of one or any two kinds in barium chloride；
The halogenating agent of melting is mainly reaction system and provides a stable state system of being uniformly heated, so as to promote positive six side
The nano-sheet Mo of shape2The homoepitaxial of C.
5）By step 4）The carbonization synthetic product of generation distillation water washing 25min, then vacuum filtration, to remove halogenating agent
The impurity of water is dissolved in other, above-mentioned " washing-vacuum filtration " operation is circulated 3-5 time altogether；The solid product that will be obtained after suction filtration
Be placed in drying box and 2-5h be dried in 60-100 DEG C, obtain the two molybdenum sheet sprills of nano silicon carbide with regular hexagon structure.
Wherein, step 1）Described in carbonaceous reducing agent be glucose or sucrose；Step 1）Described in ammonium molybdate be two
Ammonium molybdate or ammonium heptamolybdate.
Step 4）Described in heating furnace be Muffle furnace, tube furnace or vacuum drying oven；Step 4）Described reduction, carburizing reagent
Carry out under vacuum atmosphere, reducing atmosphere, inert atmosphere or air atmosphere.
Compared with prior art, the present invention has the advantages that：
1st, the present invention adopts water-soluble ammonium dimolybdate（Or ammonium heptamolybdate）, glucose（Or sucrose）Respectively as molybdenum source
And carbon source raw material, each element in reactant system is realized by precursor solution drying and is well mixed in molecule rank, dropped
Low carbothermic reduction reaction temperature simultaneously shortens the reaction time, realizes a nanometer Mo2The synthesis of C.In addition during the course of the reaction, melt
The halogenating agent for melting provides a stable state system of being uniformly heated for reaction system, so as to promote orthohexagonal nano-sheet
Mo2The homoepitaxial of C.Therefore, this unique synthetic technology based on " presoma+dissolved salt reaction " is prepared with regular hexagon
Nanometer Mo of structure2The key point of C flakelike powders.
2nd, using ammonium molybdate, carbonaceous reducing agent, halogenating agent as raw material, abundance, price are low, cost-effective for the present invention.
3rd, reduction of the invention, carburizing reagent can be carried out under vacuum or reducing atmosphere or inert atmosphere, can also be
Carry out under air atmosphere, realize that condition is simple, it is easy to accomplish；Meanwhile, maximum temperature is also less than 950 DEG C, relative to existing
Have technology 1200 DEG C are substantially reduced, and have both been reduced energy consumption, have been also improved security.
4th, nanometer Mo prepared by the present invention2C powder, its profile have the flakelike powder feature of regular hexagon structure, piece
Thickness degree is 20-80nm, and the orthohexagonal length of side is 100-500nm, and through washing purification processes, impurity content is few.
5th, the method for the invention process is simple, it is without the need for carrying out ball milling mixing to different component raw material, easy to operate, it is adapted to
Industrialized production.
Description of the drawings
Fig. 1 is nanometer Mo prepared by embodiments of the invention one2C powder is micro- under field emission scanning electron microscope
Pattern picture.
Specific embodiment
The present invention is described in further detail with reference to specific embodiment.
Embodiment one
The two molybdenum sheet sprills of nano silicon carbide with regular hexagon structure are prepared as follows, following step is specifically included
Suddenly：
1）Ammonium dimolybdate 28.61g, glucose 21.39g is dissolved in 250ml distilled water, stir to being completely dissolved and obtain
Precursor solution；
2）By step 1）The precursor solution for obtaining is placed in air dry oven, is dried 5h, obtains powder at 60 DEG C
Presoma compound；
3）By step 2）The powder presoma compound for obtaining is placed in quartz tube furnace, in the condition of argon gas protection
Under, 1h is calcined at 300 DEG C, obtain " molybdenum oxide carbon " mixture that each element is well mixed in molecular level；
4）Take step 3）" molybdenum oxide carbon " mixture for obtaining fills 1/2 volume of ceramic crucible, and with mol ratio 1:1
NaCl and KCl mixed-powders cover and fill crucible upper strata；Then crucible is placed in Muffle furnace, in air atmosphere in
Being incubated 2h at a temperature of 900 DEG C carries out reducing, carburizing reagent generates carbonization synthetic product；
5）By step 4）The carbonization synthetic product of generation 0.5L distills water washing 25min, then vacuum filtration, circulates above-mentioned
" washing-vacuum filtration " is operated 3 times；The solid product obtained after suction filtration is placed in drying box and 5h is dried in 60 DEG C, had
There are the two molybdenum sheet sprills of nano silicon carbide of regular hexagon structure.The powder apperance has the flakelike powder of regular hexagon structure special
Levy, lamellar spacing is 50-70nm, the orthohexagonal length of side is 300-500nm, as shown in Figure 1.
Embodiment two
The two molybdenum sheet sprills of nano silicon carbide with regular hexagon structure are prepared as follows, following step is specifically included
Suddenly：
1）Ammonium dimolybdate 30.39g, sucrose 19.61g is dissolved in 250ml distilled water, stir to before being completely dissolved and obtain
Drive liquid solution；
2）By step 1）The precursor solution for obtaining is placed in air dry oven, is dried 4h, obtains powder at 80 DEG C
Presoma compound；
3）By step 2）The powder presoma compound for obtaining is placed in quartz tube furnace, in the condition of argon gas protection
Under, 1h is calcined at 300 DEG C, obtain " molybdenum oxide carbon " mixture that each element is well mixed in molecular level；
4）Take step 3）" molybdenum oxide carbon " mixture for obtaining fills 1/3 volume of ceramic crucible, and with mol ratio 1:1
NaCl and BaCl2Mixed-powder is covered and fills crucible upper strata；Then crucible is placed in vacuum drying oven, in 950 DEG C of temperature
Lower insulation 1h carries out reducing, carburizing reagent generate carbonization synthetic product；
5）By step 4）The carbonization synthetic product of generation 0.5L distills water washing 25min, then vacuum filtration, circulates above-mentioned
" washing-vacuum filtration " is operated 3 times；The solid product obtained after suction filtration is placed in drying box and 3h is dried in 80 DEG C, had
There are the two molybdenum sheet sprills of nano silicon carbide of regular hexagon structure.The powder apperance has the flakelike powder of regular hexagon structure special
Levy, lamellar spacing is 60-80nm, the orthohexagonal length of side is 400-500nm.
Embodiment three
The two molybdenum sheet sprills of nano silicon carbide with regular hexagon structure are prepared as follows, following step is specifically included
Suddenly：
1）Ammonium heptamolybdate 27.94g, glucose 22.06g is dissolved in 250ml distilled water, stir to being completely dissolved and obtain
Precursor solution；
2）By step 1）The precursor solution for obtaining is placed in air dry oven, is dried 3h, obtains powder at 100 DEG C
Presoma compound；
3）By step 2）The powder presoma compound for obtaining is placed in quartz tube furnace, in the condition of argon gas protection
Under, 0.5h is calcined at 400 DEG C, obtain " molybdenum oxide carbon " mixture that each element is well mixed in molecular level；
4）Take step 3）" molybdenum oxide carbon " mixture for obtaining fills 1/2 volume of ceramic crucible, and is covered with KCl powder
Cover and fill crucible upper strata；Then crucible is placed in quartz tube furnace, 3h is incubated at a temperature of 800 DEG C in hydrogen atmosphere
Carry out reducing, carburizing reagent generate carbonization synthetic product；
5）By step 4）The carbonization synthetic product of generation 0.5L distills water washing 25min, then vacuum filtration, circulates above-mentioned
" washing-vacuum filtration " is operated 4 times；The solid product obtained after suction filtration is placed in drying box and 2h is dried in 100 DEG C, had
There are the two molybdenum sheet sprills of nano silicon carbide of regular hexagon structure.The powder apperance has the flakelike powder of regular hexagon structure special
Levy, lamellar spacing is 30-60nm, the orthohexagonal length of side is 200-400nm.
Example IV
The two molybdenum sheet sprills of nano silicon carbide with regular hexagon structure are prepared as follows, following step is specifically included
Suddenly：
1）Ammonium heptamolybdate 29.63g, sucrose 20.37g is dissolved in 250ml distilled water, stir to before being completely dissolved and obtain
Drive liquid solution；
2）By step 1）The precursor solution for obtaining is placed in air dry oven, is dried 2h, obtains powder at 120 DEG C
Presoma compound；
3）By step 2）The powder presoma compound for obtaining is placed in quartz tube furnace, in the condition of argon gas protection
Under, 0.5h is calcined at 400 DEG C, obtain " molybdenum oxide carbon " mixture that each element is well mixed in molecular level；
4）Take step 3）" molybdenum oxide carbon " mixture for obtaining fills 1/4 volume of ceramic crucible, and uses NaCl powder
Cover and fill crucible upper strata；Then crucible is placed in quartz tube furnace, is incubated at a temperature of 750 DEG C in argon gas atmosphere
4h carries out reducing, carburizing reagent generate carbonization synthetic product；
5）By step 4）The carbonization synthetic product of generation 0.5L distills water washing 25min, then vacuum filtration, circulates above-mentioned
" washing-vacuum filtration " is operated 5 times；The solid product obtained after suction filtration is placed in drying box and 2h is dried in 100 DEG C, had
There are the two molybdenum sheet sprills of nano silicon carbide of regular hexagon structure.The powder apperance has the flakelike powder of regular hexagon structure special
Levy, lamellar spacing is 20-50nm, the orthohexagonal length of side is 100-300nm.
The micro- knot of two molybdenum powder of nano silicon carbide prepared by the method for present invention offer can be found by above-described embodiment
Structure profile has the flakelike powder feature of regular hexagon structure, and lamellar spacing is 20-80nm, and the orthohexagonal length of side is 100-
500nm, through washing purification processes, impurity content is few.
The present invention adopts water-soluble ammonium dimolybdate（Or ammonium heptamolybdate）, glucose（Or sucrose）Respectively as molybdenum source and
Carbon source raw material, realizes each element in reactant system by precursor solution drying and is well mixed in molecule rank, reduce
Carbothermic reduction reaction temperature simultaneously shortens the reaction time, realizes the synthesis of two molybdenum of nano silicon carbide.In addition during the course of the reaction,
The halogenating agent of melting provides a stable state system of being uniformly heated for reaction system, so as to promote orthohexagonal nanometer sheet
Shape Mo2The homoepitaxial of C.Therefore, this unique synthetic technology based on " presoma+dissolved salt reaction " is prepared with positive six side
Nanometer Mo of shape structure2The key point of C flakelike powders.
The reduction of the present invention, carburizing reagent can be carried out under vacuum or reducing atmosphere or inert atmosphere, can also be in sky
Carry out under gas atmosphere, realize that condition is simple, change in prior art in vacuum, or H2, carry out in the protective atmosphere such as Ar
Critical conditions, it is easy to accomplish.Meanwhile, in the present invention, highest reaction temperature is only 950 DEG C, compared to what is adopted in prior art
1200 DEG C of reaction temperature reduces extremely many, This reduces both energy consumption, also improves security.
The above embodiment of the present invention is only example to illustrate the invention, and is not the enforcement to the present invention
The restriction of mode.For those of ordinary skill in the field, other can also be made not on the basis of the above description
With the change and variation of form.Here all of embodiment cannot be exhaustive.It is every to belong to technical scheme
It is amplified obvious change or change still in protection scope of the present invention row.
Claims (4)
1. a kind of preparation method of the two molybdenum sheet sprills of nano silicon carbide with regular hexagon structure, it is characterised in that include with
Lower step：
1）Ammonium molybdate, carbonaceous reducing agent are placed in distilled water as raw material, are stirred to being completely dissolved and is obtained precursor solution；Its
In, totally 50 parts of two kinds of material quality numbers, ammonium molybdate are 27.94-30.39 parts, and carbonaceous reducing agent is 19.61-22.06 parts；Its
In, described carbonaceous reducing agent is glucose or sucrose；
2）By step 1）The precursor solution for obtaining is placed in air dry oven, is dried 2-5h, obtains powder at 60-120 DEG C
Shape presoma compound；
3）By step 2）The powder presoma compound for obtaining is placed in quartz tube furnace, in the condition of inert gas shielding
Under, 0.5-1h is calcined at 300-400 DEG C, obtain " molybdenum oxide carbon " mixing that each element is well mixed in molecular level
Thing；Described inert gas is argon gas；
4）By step 3）" molybdenum oxide carbon " mixture for obtaining loads ceramic crucible, then is covered with halogenating agent powder and by crucible
Fill, the addition of the halogenating agent powder can be complete by " molybdenum oxide carbon " mixture in ceramic crucible in melting with which
All standing is defined；Then crucible is placed in heating furnace, is incubated 1-4h at a temperature of 750-950 DEG C, so that above-mentioned substance exists
Carry out reducing in ceramic crucible, carburizing reagent generate carbonization synthetic product；Described halogenating agent is sodium chloride, potassium chloride, chlorine
Change the mixture of one or any two kinds in calcium, barium chloride；
5）By step 4）The carbonization synthetic product of generation distillation water washing 25min, then vacuum filtration, with remove halogenating agent and its
He is dissolved in the impurity of water, and above-mentioned " washing-vacuum filtration " operation is circulated 3-5 time altogether；The solid product obtained after suction filtration is placed in
2-5h is dried in 60-100 DEG C in drying box, the two molybdenum sheet sprills of nano silicon carbide with regular hexagon structure are obtained.
2. the preparation method of the two molybdenum sheet sprills of nano silicon carbide with regular hexagon structure according to claim 1, its
It is characterised by, step 1）Described in ammonium molybdate be ammonium dimolybdate or ammonium heptamolybdate.
3. the preparation method of the two molybdenum sheet sprills of nano silicon carbide with regular hexagon structure according to claim 1, its
It is characterised by, step 4）Described in heating furnace be Muffle furnace, tube furnace or vacuum drying oven.
4. the preparation method of the two molybdenum sheet sprills of nano silicon carbide with regular hexagon structure according to claim 1, its
It is characterised by, step 4）Described reduction, carburizing reagent are under vacuum atmosphere, reducing atmosphere, inert atmosphere or air atmosphere
Carry out.
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| CN105742608B (en) * | 2016-04-19 | 2018-07-17 | 陕西科技大学 | A kind of Mo2C/CNTs nanometer sheet electrode materials and preparation method thereof |
| CN105858663B (en) * | 2016-06-08 | 2017-11-28 | 太原理工大学 | A kind of preparation method of bowl-shape carbon and carbonization molybdenum composite material |
| CN106495158B (en) * | 2016-11-28 | 2019-06-28 | 中国科学院重庆绿色智能技术研究院 | A kind of preparation method and products thereof of ultra-thin carbonization molybdenum material |
| CN106672921B (en) * | 2016-12-26 | 2019-01-15 | 华中科技大学 | A kind of preparation method of two-dimensional metallic compound-material |
| CN108866633B (en) * | 2018-07-25 | 2020-04-28 | 四川理工学院 | Nano VC crystal whisker and preparation method thereof |
| CN109126844B (en) * | 2018-08-31 | 2021-05-25 | 厦门理工学院 | Molybdenum carbide nanosheet and preparation method and application thereof |
| CN110878418B (en) * | 2018-09-06 | 2021-08-24 | 天津大学 | Self-supporting molybdenum carbide and preparation method and application thereof |
| CN109227924B (en) * | 2018-09-13 | 2020-11-06 | 孙习习 | Ceramic material synthesis equipment |
| CN112028041A (en) * | 2020-09-03 | 2020-12-04 | 中国科学院地球化学研究所 | Carbon thermal reduction preparation method of MoP, product and application |
| CN113277514A (en) * | 2021-06-18 | 2021-08-20 | 信阳师范学院 | Transition metal carbide Mo2Preparation method of material C |
| CN115819085B (en) * | 2022-12-30 | 2023-09-29 | 山东大学 | Preparation method of aqueous phase precursor of high-entropy rare earth diboron carbide nano powder |
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