CN105217633A - A kind of preparation method with the nano silicon carbide two molybdenum sheet sprills of regular hexagon structure - Google Patents
A kind of preparation method with the nano silicon carbide two molybdenum sheet sprills of regular hexagon structure Download PDFInfo
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Abstract
The present invention relates to a kind of preparation method with the nano silicon carbide two molybdenum sheet sprills of regular hexagon structure, the method adopts water-soluble ammonium dimolybdate (or Ammonium Heptamolybdate), glucose (or sucrose) respectively as molybdenum source and carbon source raw material, achieve each element in reactant system by precursor solution drying to mix in molecule rank, reduce carbothermic reduction reaction temperature and shorten the reaction times, achieving nanometer Mo
2the synthesis of C.In addition in reaction process, the halogenating agent of melting is that reaction system provides a stable state system of being heated uniformly, thus facilitates orthohexagonal nano-sheet Mo
2the homoepitaxial of C.
Description
Technical field
The invention belongs to inorganic non-metallic powder body material preparation field, be specifically related to a kind of preparation method with nano silicon carbide two molybdenum powder of regular hexagon sheet structure.
Background technology
Dimolybdenum carbide (Mo
2c) because having that fusing point is high, hardness is high, electrical and thermal conductivity performance is good and the feature such as erosion resistance is good, the fields such as various high temperature resistant, wear-resisting and chemical resistant material have been widely used at present.Mo
2c Chang Zuowei second-phase adds the wear resistance that can improve workpiece in ferrous materials to, also can be used as important component and adds in WC base cemented carbide and Ti (C, N) based ceramic metal system and improve microstructure and mechanical property.In addition, also can separately for making wear-resistant, anti scuffing coating.Mo
2c also because of electronic structure and catalysis characteristics that it has similar precious metal, is described as " accurate platinum catalyst ", is widely used as the reaction of hydrogen participation as alkane isomerization, unsaturated hydrocarbons
hydrogenation, hydrogenating desulfurization and the reaction such as denitrogenation and synthetic ammonia the carbide price of catalyzer, particularly molybdenum cheap and there is again excellent anti-sulfur poisonous performance compared with precious metal, therefore Mo
2c catalyst is quite noticeable.
The synthesis of carbide generally needs at high temperature to carry out.According to the difference of type of feed, the powder stock containing molybdenum mainly contains three classes: elemental metals molybdenum, and the oxide compound of molybdenum is (as MoO
3) and the presoma (as ammonium molybdate) of molybdenum.Obviously, by unactual for the mixture high temperature cabonization of molybdenum powder and carbon dust, the temperature of not only reacting is high, and expensive starting materials.By MoO
3after powder mixes with carbon dust, Mo is synthesized in carbothermic reduction
2the topmost commercial run of C powder; The method is owing to adopting MoO
3powder is raw material, and cost is lower, but synthesis temperature is still higher, and the Chinese patent " production method of molybdenum carbide " being 96115598.1 as application number discloses a kind of production method: by MoO
3with the mixing of C powder, at 1600 DEG C, carbothermic reduction 2h prepares the Mo that carbon content is greater than 12%
2c powder.The presoma of molybdenum is utilized to synthesize Mo for raw material carries out carbothermic reduction
2c powder, its raw materials cost is minimum, and obviously can reduce temperature of reaction, be beneficial to the synthesis of nanometer powder, as document " MaterialsResearchBulletin, Volume43, Issues8 – 9,2008, Pages2036-2041 " report that the people such as ManishPatel utilize ammonium molybdate and sucrose to prepare nanometer powder for raw material carbothermic reduction at 1200 DEG C.
In these methods, all there is the problem that some cannot overcome, as 1) building-up process is usually in vacuum, or H
2, carry out in the protective atmosphere such as Ar; 2) carbothermic reduction institute heat requirement provides primarily of heating unit radiative transfer, and reaction product is heated inside and outside inequality; 3) Mo synthesized
2the powdery substance that C out-of-shape, particle size distribution range are wider, brings inconvenience to practical application.
Summary of the invention
For prior art above shortcomings, the object of the present invention is to provide that a kind of raw material is heated evenly, temperature of reaction is low and finished product has the preparation method of the nano silicon carbide two molybdenum sheet sprills of regular hexagon structure.
To achieve these goals, the technical solution used in the present invention is as follows:
There is a preparation method for the nano silicon carbide two molybdenum sheet sprills of regular hexagon structure, comprise the following steps:
1) ammonium molybdate, carbonaceous reducing agent are placed in distilled water as raw material, are stirred to dissolving completely and obtain precursor solution; Wherein, two kinds of raw materials quality numbers totally 50 parts, ammonium molybdate is 27.94-30.39 part, and carbonaceous reducing agent is 19.61-22.06 part; The follow-up chemical equation related to of this preparation method is 2MoO
3(s)+7C (s)=Mo
2c (s)+6CO (g), therefore the mol ratio of Mo and C is 2:7 in theory, prepares ammonium molybdate, carbonaceous reducing agent accordingly.Consider in reality that the carbonaceous reducing agents such as glucose have carbon depletion in thermal decomposition process, therefore C needs are suitably excessive, the actual add-on of usual C is slightly higher than theoretical mixed carbon comtent, is 2:8 ~ 10.Carbon has two: one to be MoO as reductive agent Main Function
3be reduced into simple substance Mo, two is generate Mo with simple substance Mo carbonization
2c.
2) precursor solution that step 1) obtains is placed in air dry oven, dry 2-5h at 60-120 DEG C, obtains Powdered presoma compound;
3) by step 2) the Powdered presoma compound that obtains is placed in quartz tube furnace, and under the condition of protection of inert gas, at 300-400 DEG C, calcine 0.5-1h, obtain " molybdenum oxide-carbon " mixture that each element mixes in molecular level; Described rare gas element is argon gas;
4) " molybdenum oxide-carbon " mixture step 3) obtained is filled into ceramic crucible, cover with halogenating agent powder and filled by crucible, the add-on of halogenating agent powder is as the criterion with its " molybdenum oxide-carbon " mixture covered completely in ceramic crucible when melting; Then crucible is placed in process furnace, at 750-950 DEG C of temperature, is incubated 1-4h, carry out to make above-mentioned substance reducing in ceramic crucible, carburizing reagent Formed is combined to product; Described halogenating agent is the mixture of one or any two kinds in sodium-chlor, Repone K, calcium chloride, bariumchloride;
The halogenating agent of melting is mainly reaction system provides a stable state system of being heated uniformly, thus facilitates orthohexagonal nano-sheet Mo
2the homoepitaxial of C.
5) by the carbonization synthetic product distilled water wash 25min that step 4) generates, then vacuum filtration, to remove halogenating agent and other water-soluble impurity, above-mentioned " washing-vacuum filtration " operates circulation altogether 3-5 time; The solid product obtained after suction filtration is placed in loft drier in 60-100 DEG C of dry 2-5h, obtains the nano silicon carbide two molybdenum sheet sprills with regular hexagon structure.
Wherein, the carbonaceous reducing agent described in step 1) is glucose or sucrose; Ammonium molybdate described in step 1) is ammonium dimolybdate or Ammonium Heptamolybdate.
Process furnace described in step 4) is retort furnace, tube furnace or vacuum oven; Reduction described in step 4), carburizing reagent are carried out under vacuum atmosphere, reducing atmosphere, inert atmosphere or air atmosphere.
Compared with prior art, the present invention has following beneficial effect:
1, the present invention adopts water-soluble ammonium dimolybdate (or Ammonium Heptamolybdate), glucose (or sucrose) respectively as molybdenum source and carbon source raw material, achieve each element in reactant system by precursor solution drying to mix in molecule rank, reduce carbothermic reduction reaction temperature and shorten the reaction times, achieving nanometer Mo
2the synthesis of C.In addition in reaction process, the halogenating agent of melting is that reaction system provides a stable state system of being heated uniformly, thus facilitates orthohexagonal nano-sheet Mo
2the homoepitaxial of C.Therefore, this unique synthetic technology based on " presoma+dissolved salt reaction " is the nanometer Mo that preparation has regular hexagon structure
2the key point of C plate.
2, the present invention is using ammonium molybdate, carbonaceous reducing agent, halogenating agent as raw material, and abundance, price are low, cost-saving.
3, reduction of the present invention, carburizing reagent can be carried out under vacuum or reducing atmosphere or inert atmosphere, also can carry out in air atmosphere, and realization condition is simple, are easy to realize; Meanwhile, maximum temperature is also no more than 950 DEG C, greatly reduces, both reduced energy consumption, and also improved security relative to 1200 DEG C of prior art.
4, the nanometer Mo prepared by the present invention
2c powder, its profile has the plate feature of regular hexagon structure, and lamellar spacing is 20-80nm, and the orthohexagonal length of side is 100-500nm, and through washing purification processes, foreign matter content is few.
5, the method for the invention technique is simple, without the need to carrying out ball milling mixing to different components raw material, easy to operate, is applicable to suitability for industrialized production.
Accompanying drawing explanation
Fig. 1 is nanometer Mo prepared by embodiments of the invention one
2the microstructure picture of C powder under field emission scanning electron microscope.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in further detail.
embodiment one
Preparation has the nano silicon carbide two molybdenum sheet sprills of regular hexagon structure as follows, specifically comprises the following steps:
1) by ammonium dimolybdate 28.61g, glucose 21.39g, be dissolved in 250ml distilled water, be stirred to dissolving completely and obtain precursor solution;
2) precursor solution that step 1) obtains is placed in air dry oven, dry 5h at 60 DEG C, obtains Powdered presoma compound;
3) by step 2) the Powdered presoma compound that obtains is placed in quartz tube furnace, and under the condition of argon shield, at 300 DEG C, calcine 1h, obtain " molybdenum oxide-carbon " mixture that each element mixes in molecular level;
4) get 1/2 volume of " molybdenum oxide-carbon " mixture filling ceramic crucible that step 3) obtains, and cover with NaCl and the KCl mixed powder of mol ratio 1:1 and fill crucible upper strata; Then crucible is placed in retort furnace, in air atmosphere, at 900 DEG C of temperature, is incubated that 2h carries out reducing, carburizing reagent Formed is combined to product;
5) by the carbonization synthetic product 0.5L distilled water wash 25min that step 4) generates, then vacuum filtration, circulate above-mentioned " washing-vacuum filtration " operates 3 times; The solid product obtained after suction filtration is placed in loft drier in 60 DEG C of dry 5h, obtains the nano silicon carbide two molybdenum sheet sprills with regular hexagon structure.This powder apperance has the plate feature of regular hexagon structure, and lamellar spacing is 50-70nm, and the orthohexagonal length of side is 300-500nm, as shown in Figure 1.
embodiment two
Preparation has the nano silicon carbide two molybdenum sheet sprills of regular hexagon structure as follows, specifically comprises the following steps:
1) by ammonium dimolybdate 30.39g, sucrose 19.61g, be dissolved in 250ml distilled water, be stirred to dissolving completely and obtain precursor solution;
2) precursor solution that step 1) obtains is placed in air dry oven, dry 4h at 80 DEG C, obtains Powdered presoma compound;
3) by step 2) the Powdered presoma compound that obtains is placed in quartz tube furnace, and under the condition of argon shield, at 300 DEG C, calcine 1h, obtain " molybdenum oxide-carbon " mixture that each element mixes in molecular level;
4) 1/3 volume that " molybdenum oxide-carbon " mixture that step 3) obtains fills ceramic crucible is got, and with NaCl and BaCl of mol ratio 1:1
2mixed powder covers and fills crucible upper strata; Then crucible is placed in vacuum oven, at 950 DEG C of temperature, is incubated that 1h carries out reducing, carburizing reagent Formed is combined to product;
5) by the carbonization synthetic product 0.5L distilled water wash 25min that step 4) generates, then vacuum filtration, circulate above-mentioned " washing-vacuum filtration " operates 3 times; The solid product obtained after suction filtration is placed in loft drier in 80 DEG C of dry 3h, obtains the nano silicon carbide two molybdenum sheet sprills with regular hexagon structure.This powder apperance has the plate feature of regular hexagon structure, and lamellar spacing is 60-80nm, and the orthohexagonal length of side is 400-500nm.
embodiment three
Preparation has the nano silicon carbide two molybdenum sheet sprills of regular hexagon structure as follows, specifically comprises the following steps:
1) by Ammonium Heptamolybdate 27.94g, glucose 22.06g, be dissolved in 250ml distilled water, be stirred to dissolving completely and obtain precursor solution;
2) precursor solution that step 1) obtains is placed in air dry oven, dry 3h at 100 DEG C, obtains Powdered presoma compound;
3) by step 2) the Powdered presoma compound that obtains is placed in quartz tube furnace, and under the condition of argon shield, at 400 DEG C, calcine 0.5h, obtain " molybdenum oxide-carbon " mixture that each element mixes in molecular level;
4) get 1/2 volume of " molybdenum oxide-carbon " mixture filling ceramic crucible that step 3) obtains, and cover with KCl powder and fill crucible upper strata; Then crucible is placed in quartz tube furnace, in hydrogen atmosphere, at 800 DEG C of temperature, is incubated that 3h carries out reducing, carburizing reagent Formed is combined to product;
5) by the carbonization synthetic product 0.5L distilled water wash 25min that step 4) generates, then vacuum filtration, circulate above-mentioned " washing-vacuum filtration " operates 4 times; The solid product obtained after suction filtration is placed in loft drier in 100 DEG C of dry 2h, obtains the nano silicon carbide two molybdenum sheet sprills with regular hexagon structure.This powder apperance has the plate feature of regular hexagon structure, and lamellar spacing is 30-60nm, and the orthohexagonal length of side is 200-400nm.
embodiment four
Preparation has the nano silicon carbide two molybdenum sheet sprills of regular hexagon structure as follows, specifically comprises the following steps:
1) by Ammonium Heptamolybdate 29.63g, sucrose 20.37g, be dissolved in 250ml distilled water, be stirred to dissolving completely and obtain precursor solution;
2) precursor solution that step 1) obtains is placed in air dry oven, dry 2h at 120 DEG C, obtains Powdered presoma compound;
3) by step 2) the Powdered presoma compound that obtains is placed in quartz tube furnace, and under the condition of argon shield, at 400 DEG C, calcine 0.5h, obtain " molybdenum oxide-carbon " mixture that each element mixes in molecular level;
4) get 1/4 volume of " molybdenum oxide-carbon " mixture filling ceramic crucible that step 3) obtains, and cover with NaCl powder and fill crucible upper strata; Then crucible is placed in quartz tube furnace, in argon gas atmosphere, at 750 DEG C of temperature, is incubated that 4h carries out reducing, carburizing reagent Formed is combined to product;
5) by the carbonization synthetic product 0.5L distilled water wash 25min that step 4) generates, then vacuum filtration, circulate above-mentioned " washing-vacuum filtration " operates 5 times; The solid product obtained after suction filtration is placed in loft drier in 100 DEG C of dry 2h, obtains the nano silicon carbide two molybdenum sheet sprills with regular hexagon structure.This powder apperance has the plate feature of regular hexagon structure, and lamellar spacing is 20-50nm, and the orthohexagonal length of side is 100-300nm.
The microstructure profile of nano silicon carbide two molybdenum powder that can be found prepared by method provided by the invention by above-described embodiment has the plate feature of regular hexagon structure, lamellar spacing is 20-80nm, the orthohexagonal length of side is 100-500nm, and through washing purification processes, foreign matter 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, achieve each element in reactant system by precursor solution drying to mix in molecule rank, reduce carbothermic reduction reaction temperature and shorten the reaction times, achieving the synthesis of nano silicon carbide two molybdenum.In addition in reaction process, the halogenating agent of melting is that reaction system provides a stable state system of being heated uniformly, thus facilitates orthohexagonal nano-sheet Mo
2the homoepitaxial of C.Therefore, this unique synthetic technology based on " presoma+dissolved salt reaction " is the nanometer Mo that preparation has regular hexagon structure
2the key point of C plate.
Reduction of the present invention, carburizing reagent can be carried out under vacuum or reducing atmosphere or inert atmosphere, also can carry out in air atmosphere, and realization condition is simple, changes in vacuum in prior art, or H
2, the critical conditions of carrying out in the protective atmosphere such as Ar, be easy to realize.Meanwhile, temperature of reaction the highest in the present invention is only 950 DEG C, and the temperature of reaction of 1200 DEG C that adopt in prior art reduces extremely many, This reduces both energy consumption, also improves security.
The above embodiment of the present invention is only for example of the present invention is described, and is not the restriction to embodiments of the present invention.For those of ordinary skill in the field, other multi-form change and variations can also be made on the basis of the above description.Here cannot give exhaustive to all embodiments.Every belong to technical scheme of the present invention the apparent change of amplifying out or variation be still in the row of protection scope of the present invention.
Claims (5)
1. there is a preparation method for the nano silicon carbide two molybdenum sheet sprills of regular hexagon structure, it is characterized in that, comprise the following steps:
1) ammonium molybdate, carbonaceous reducing agent are placed in distilled water as raw material, are stirred to dissolving completely and obtain precursor solution; Wherein, two kinds of raw materials quality numbers totally 50 parts, ammonium molybdate is 27.94-30.39 part, and carbonaceous reducing agent is 19.61-22.06 part;
2) precursor solution that step 1) obtains is placed in air dry oven, dry 2-5h at 60-120 DEG C, obtains Powdered presoma compound;
3) by step 2) the Powdered presoma compound that obtains is placed in quartz tube furnace, and under the condition of protection of inert gas, at 300-400 DEG C, calcine 0.5-1h, obtain " molybdenum oxide-carbon " mixture that each element mixes in molecular level; Described rare gas element is argon gas;
4) " molybdenum oxide-carbon " mixture step 3) obtained loads ceramic crucible, cover with halogenating agent powder and filled by crucible, " molybdenum oxide-carbon " mixture in ceramic crucible can cover and is as the criterion when melting with it by the add-on of described halogenating agent powder completely; Then crucible is placed in process furnace, at 750-950 DEG C of temperature, is incubated 1-4h, carry out to make above-mentioned substance reducing in ceramic crucible, carburizing reagent Formed is combined to product; Described halogenating agent is the mixture of one or any two kinds in sodium-chlor, Repone K, calcium chloride, bariumchloride;
5) by the carbonization synthetic product distilled water wash 25min that step 4) generates, then vacuum filtration, to remove halogenating agent and other water-soluble impurity, above-mentioned " washing-vacuum filtration " operates circulation altogether 3-5 time; The solid product obtained after suction filtration is placed in loft drier in 60-100 DEG C of dry 2-5h, obtains the nano silicon carbide two molybdenum sheet sprills with regular hexagon structure.
2. the preparation method with the nano silicon carbide two molybdenum sheet sprills of regular hexagon structure according to claim 1, it is characterized in that, the carbonaceous reducing agent described in step 1) is glucose or sucrose.
3. the preparation method with the nano silicon carbide two molybdenum sheet sprills of regular hexagon structure according to claim 1, it is characterized in that, the ammonium molybdate described in step 1) is ammonium dimolybdate or Ammonium Heptamolybdate.
4. the preparation method with the nano silicon carbide two molybdenum sheet sprills of regular hexagon structure according to claim 1, it is characterized in that, the process furnace described in step 4) is retort furnace, tube furnace or vacuum oven.
5. the preparation method with the nano silicon carbide two molybdenum sheet sprills of regular hexagon structure according to claim 1, it is characterized in that, the reduction described in step 4), carburizing reagent are carried out under vacuum atmosphere, reducing atmosphere, inert atmosphere or air atmosphere.
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| CN105858663A (en) * | 2016-06-08 | 2016-08-17 | 太原理工大学 | Preparation method of bowl-shaped carbon-molybdenum carbide composite material |
| CN106495158A (en) * | 2016-11-28 | 2017-03-15 | 中国科学院重庆绿色智能技术研究院 | A kind of preparation method of ultra-thin carbonization Mo and products thereof |
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| 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 |
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| 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 |
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