CN106629850B - A kind of preparation method of centimetres monocrystalline molybdenum trioxide nano band - Google Patents
A kind of preparation method of centimetres monocrystalline molybdenum trioxide nano band Download PDFInfo
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- CN106629850B CN106629850B CN201611071670.8A CN201611071670A CN106629850B CN 106629850 B CN106629850 B CN 106629850B CN 201611071670 A CN201611071670 A CN 201611071670A CN 106629850 B CN106629850 B CN 106629850B
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- C01G39/02—Oxides; Hydroxides
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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Abstract
The present invention provides a kind of preparation methods of centimetres monocrystalline molybdenum trioxide nano band, which is characterized in that includes the following steps：（1）Molybdenum source is fixed in crucible；（2）By Y2O3Powder uniform fold is on the surface of the molybdenum source；（3）Crucible is placed in the coil of magnetic levitation melting stove, opens power initiation magnetic suspension stove, be warming up in 1000 DEG C ~ 2000 DEG C, keep the temperature 80 s ~ 300s；（4）Power supply is closed, crucible is taken out after being cooled to room temperature, white group flocculent substance is collected in crucible, which is centimetres monocrystalline molybdenum trioxide nano band.The molybdenum trioxide band that this method obtains is centimetres, and quality is high, and is prepared for magnanimity, and required temperature is moderate, and energy consumption is few, can realize that inexpensive high-volume quickly prepares MoO 3 monocrystal band.
Description
Technical field
The present invention relates to chemical preparation field more particularly to a kind of preparation methods of centimetres monocrystalline molybdenum trioxide.
Background technology
Molybdenum and molybdenum alloy material not only have good high temperature strength and hardness, and with good conduction, heat conduction,
The performances such as anticorrosive, therefore it is widely used in the industrial circles such as chemical, metallurgical machinery and aerospace.Molybdenum trioxide
(MoO3) be not only to prepare the primary raw material of molybdenum and molybdenum alloy material, and itself also there is electrochromism, photochromic, light to urge
Change the characteristics such as degradation and air-sensitive, therefore in many such as synthesizing sensitive element, catalyst, fast-ionic conductor and potential battery electrodes
There is specific use in terms of functional material.Skin effect, small-size effect, the quantum size effect shown due to nano material
And the performances such as quantum tunneling effect so that nano-sized molybdenum oxide is in battery electrode material, catalyst, flat-panel monitor, resistance cigarette
The fields such as agent, sensor, luminescence generated by light colour development material are with a wide range of applications.
Though at present there are many molybdenum trioxide preparation method these methods equipment it is more complicated, preparation condition ratio
It is harsher.
The content of the invention
For above-mentioned technical problem, the object of the present invention is to provide inexpensive high-volume quickly to prepare MoO 3 monocrystal item
The preparation method of band.The molybdenum trioxide band that this method obtains is centimetres, and quality is high, and is prepared for magnanimity, required temperature
Moderate, energy consumption is few, can realize that inexpensive high-volume quickly prepares MoO 3 monocrystal band.
Technical scheme is as follows：
A kind of preparation method of centimetres monocrystalline molybdenum trioxide nano band, includes the following steps：
（1）Molybdenum source is fixed in crucible；Molybdenum source is first trimmed to suitable shape and then molybdenum source is fixed on appropriate ruler
In very little crucible, it is immovable to notice that molybdenum source is placed in crucible rear molybdenum source；
（2）By Y2O3Powder is covered on the surface of the molybdenum source；
（3）Crucible is placed in the coil of magnetic levitation melting stove, opens power initiation magnetic suspension stove, be warming up to 1000 DEG C
In ~ 2000 DEG C, 10 seconds ~ 100 minutes are kept the temperature；
（4）Power supply is closed, crucible is taken out after being cooled to room temperature, there will be white group on the sidewall of crucible above molybdenum source at this time
Flocculent substance generates, which is centimetres monocrystalline molybdenum trioxide nano band.
Wherein, the Y2O3Molten condition is presented when being warming up to 1000 DEG C or more in powder.
Wherein, the Y2O3Powder and the mass ratio of the molybdenum source are 0:1~100:1.
Wherein, the molybdenum source is conductive flitch containing molybdenum materials, further included before crucible is put into the surface of the molybdenum plate into
The processing step that row polishing clears the pollution off.
Wherein, step（3）Described in magnetic suspension stove heating power be 0.1 more than KW power.
Wherein, the step（3）Middle soaking time and crucible material, structure, the type of cooling, crucible intrinsic inductance and
The size of required oxidation molybdenum single crystal is related.
Wherein, step（1）In, the material of the crucible is metal oxide, high-thermal conductive metal material, aluminate, metatitanic acid
The non-electromagnetic shielding material such as salt and silicate.
Wherein, the structure of the crucible is individual layer sidewall of crucible, double crucible wall or multilayer sidewall of crucible.
Wherein, the type of cooling of the crucible is water cooling or natural cooling.
Wherein, section footpath of the molybdenum source is in 0.1 more than mm.
The beneficial effects of the invention are as follows：
（1）The present invention generates rapidly a large amount of molybdenum steam using magnetic suspension auxiliary law, and oxidation molybdenum single crystal can be rapidly rather
It is formed in clock, obtains the highly oriented single crystal of layer structure；
（2）The present invention can prepare the nano band of MoO 3 monocrystal of centimetres, and quality is high, and required temperature is moderate,
Energy consumption is few, can realize that inexpensive high-volume quickly prepares nano band of MoO 3 monocrystal；
（3）The present invention can realize prepared by the magnanimity of MoO 3 monocrystal.
Description of the drawings
Fig. 1 is molybdenum trioxide nano band entity microspur photo obtained in the method for the present invention example 1；
Fig. 2 is molybdenum trioxide nano band polarization microscope photo obtained in the method for the present invention example 1；
Fig. 3 is molybdenum trioxide nano band electron scanning micrograph obtained in the method for the present invention example 1；
Fig. 4 is the X-ray photoelectron spectroscopic analysis of molybdenum trioxide nano band obtained in the method for the present invention example 1；
Fig. 5 is molybdenum trioxide nano band entity microspur photo obtained in the method for the present invention example 2；
Fig. 6 is molybdenum trioxide nano band polarization microscope photo obtained in the method for the present invention example 2；
Fig. 7 is molybdenum trioxide nano band electron scanning micrograph obtained in the method for the present invention example 2;
Fig. 8 is molybdenum trioxide nano band polarization microscope photo obtained in the method for the present invention example 3.
Specific embodiment
Embodiment 1
A kind of preparation method of centimetres monocrystalline molybdenum trioxide nano band, is as follows：
（1）4.37 g molybdenum plates is taken to be horizontally placed in the crucible that volume is 20 ml, weigh 0.60g Y2O3Powder uniform fold
In molybdenum plate upper surface；
（2）Crucible is positioned in magnetic levitation melting stove coil, power initiation magnetic suspension stove is opened, is warming up to by 40s
1600 DEG C ~ 1650 DEG C, the heating power of magnetic suspension stove is 19.2 KW, keeps the temperature 140 s；
（3）Power supply is closed, crucible is taken out after being cooled to room temperature, white group flocculent substance is collected in crucible, this is li
Rice magnitude monocrystalline molybdenum trioxide nano band.
Embodiment 2
A kind of preparation method of centimetres monocrystalline molybdenum trioxide nano band, is as follows：
（1）5.18 g molybdenum plates is taken to be horizontally placed in the crucible that volume is 20 ml, weigh 0.89 g Y2O3Powder uniform fold
In molybdenum plate upper surface；
（2）Crucible is positioned in magnetic levitation melting stove coil, power initiation magnetic suspension stove is opened, is warming up to by 60s
1700 DEG C ~ 1800 DEG C, the heating power of magnetic suspension stove is 23.6 KW, keeps the temperature 140 s；
（3）Power supply is closed, crucible is taken out after being cooled to room temperature, white group flocculent substance is collected in crucible, this is li
Rice magnitude monocrystalline molybdenum trioxide nano band.
Embodiment 3
A kind of preparation method of centimetres monocrystalline molybdenum trioxide nano band, is as follows：
（1）2.42 g molybdenum plates is taken to be horizontally placed in the crucible that volume is 10 ml, weigh 0.55 g Y2O3Powder uniform fold
In molybdenum plate upper surface；
（2）Crucible is positioned in magnetic levitation melting stove coil, opens power initiation magnetic suspension stove, is heated up by 120 s
To 1800 ~ 1900 DEG C, the heating power of magnetic suspension stove is 24.6 KW, keeps the temperature 140 s；
（3）Power supply is closed, crucible is taken out after being cooled to room temperature, white group flocculent substance is collected in crucible, this is li
Rice magnitude monocrystalline molybdenum trioxide nano band.
Embodiment 4
A kind of preparation method of centimetres monocrystalline molybdenum trioxide nano band, is as follows：
（1）3.0 g molybdenum plates is taken to be horizontally placed in the crucible that volume is 20 ml, weigh 0.60 g Y2O3Powder uniform fold
In molybdenum plate upper surface；
（2）Crucible is positioned in magnetic levitation melting stove coil, power initiation magnetic suspension stove is opened, is warming up to by 50 s
1800 ~ 1900 DEG C, the heating power of magnetic suspension stove is 22.9 KW, keeps the temperature 300 s；
（3）Power supply is closed, crucible is taken out after being cooled to room temperature, white group flocculent substance is collected in crucible, this is li
Rice magnitude monocrystalline molybdenum trioxide nano band.
Embodiment 5
A kind of preparation method of centimetres monocrystalline molybdenum trioxide nano band, is as follows：
（1）4.35g molybdenum plates is taken to be horizontally placed in the crucible that volume is 20ml, 0.67g Y2O3 powder uniform folds is weighed and exists
Molybdenum plate upper surface；
（2）Crucible is positioned in magnetic levitation melting stove coil, opens power initiation magnetic suspension stove, heat up power
19.8KW is warming up to 1900 DEG C by 30s, keeps the temperature 120s；
（3）Power supply is closed, crucible is taken out after being cooled to room temperature, white group flocculent substance is collected in crucible, this is li
Rice magnitude monocrystalline molybdenum trioxide nano band.
Embodiment 6
A kind of preparation method of centimetres monocrystalline molybdenum trioxide nano band, is as follows：
（1）3.0 g molybdenum plates is taken to be horizontally placed in the crucible that volume is 10 ml, weigh 0.30 g Y2O3Powder uniform fold
In molybdenum plate upper surface；
（2）Crucible is positioned in magnetic levitation melting stove coil, power initiation magnetic suspension stove is opened, is warming up to by 60 s
1000 DEG C ~ 1100 DEG C, the heating power of magnetic suspension stove is 23.6 KW, keeps the temperature 80 s；
（3）Power supply is closed, crucible is taken out after being cooled to room temperature, white group flocculent substance is collected in crucible, this is li
Rice magnitude monocrystalline molybdenum trioxide nano band.
Embodiment 7
A kind of preparation method of centimetres monocrystalline molybdenum trioxide nano band, is as follows：
（1）2.52 g molybdenum plates is taken to be horizontally placed in the crucible that volume is 10 ml, weigh 25 g Y2O3Powder is covered in molybdenum plate
Upper surface；
（2）Crucible is positioned in magnetic levitation melting stove coil, open power initiation magnetic suspension stove, be warming up to 1200 DEG C ~
1300 DEG C, the heating power of magnetic suspension stove is 12.4 KW, keeps the temperature 10 minutes；
（3）Power supply is closed, crucible is taken out after being cooled to room temperature, collects white group flocculent substance in crucible, this is centimetre
Magnitude monocrystalline molybdenum trioxide nano band.
Embodiment 8
A kind of preparation method of centimetres monocrystalline molybdenum trioxide nano band, is as follows：
（1）3.55 g molybdenum plates is taken to be horizontally placed in the crucible that volume is 20 ml, weigh 350 g Y2O3Powder is covered in molybdenum
Plate upper surface；
（2）Crucible is positioned in magnetic levitation melting stove coil, open power initiation magnetic suspension stove, be warming up to 1800 DEG C ~
1900 DEG C, the heating power of magnetic suspension stove is 28.9 KW, keeps the temperature 20 minutes；
（3）Power supply is closed, crucible is taken out after being cooled to room temperature, white group flocculent substance is collected in crucible, this is li
Rice magnitude monocrystalline molybdenum trioxide nano band.
Embodiment 9
A kind of preparation method of centimetres monocrystalline molybdenum trioxide nano band, is as follows：
（1）5.43 g molybdenum plates is taken to be horizontally placed in the crucible that volume is 20 ml, weigh 150.2 g Y2O3Powder is covered in
Molybdenum plate upper surface；
（2）Crucible is positioned in magnetic levitation melting stove coil, open power initiation magnetic suspension stove, be warming up to 1800 DEG C ~
1900 DEG C, the heating power of magnetic suspension stove is 37.2 KW, keeps the temperature 50 minutes；
（3）Power supply is closed, crucible is taken out after being cooled to room temperature, white group flocculent substance is collected in crucible, this is li
Rice magnitude monocrystalline molybdenum trioxide nano band.
Embodiment 10
A kind of preparation method of centimetres monocrystalline molybdenum trioxide nano band, is as follows：
（1）5.25 g molybdenum plates is taken to be horizontally placed in the crucible that volume is 20 ml, weigh 100.1 g Y2O3Powder is covered in
Molybdenum plate upper surface；
（2）Crucible is positioned in magnetic levitation melting stove coil, open power initiation magnetic suspension stove, be warming up to 1100 DEG C ~
1150 DEG C, the heating power of magnetic suspension stove is 15.3 KW, keeps the temperature 100 minutes；
（3）Power supply is closed, crucible is taken out after being cooled to room temperature, white group flocculent substance is collected in crucible, this is li
Rice magnitude monocrystalline molybdenum trioxide nano band.
Embodiment described above only expresses the several embodiments of the present invention, and description is more specific and detailed, but simultaneously
Cannot the limitation to the scope of the claims of the present invention therefore be interpreted as.It should be pointed out that for those of ordinary skill in the art
For, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to the guarantor of the present invention
Protect scope.Therefore, the protection domain of patent of the present invention should be subject to claim.
Claims (9)
1. a kind of preparation method of centimetres monocrystalline molybdenum trioxide nano band, which is characterized in that include the following steps：
（1）Molybdenum source is fixed in crucible；
（2）By Y2O3Powder is covered on the surface of the molybdenum source, and the molybdenum source is conductive flitch containing molybdenum materials；
（3）Crucible is placed in the coil of magnetic levitation melting stove, open power initiation magnetic suspension stove, be warming up to 1000 DEG C ~
In 2000 DEG C, 10 seconds ~ 100 minutes are kept the temperature；
（4）Power supply is closed, crucible is taken out after being cooled to room temperature, white group flocculent substance is collected in crucible, which is
For centimetres monocrystalline molybdenum trioxide nano band.
2. preparation method according to claim 1, which is characterized in that the Y2O3Powder is being warming up to 1000 DEG C or more
When, molten condition is presented.
3. preparation method according to claim 1, which is characterized in that the Y2O3Powder and the mass ratio of the molybdenum source are
0.1:1~98.59:1。
4. preparation method according to claim 1, which is characterized in that further included before crucible is put into the molybdenum source
Surface carries out the processing step that polishing clears the pollution off.
5. preparation method according to claim 1, which is characterized in that step（3）Described in magnetic suspension stove heating power
For 0.1 more than KW power.
6. preparation method according to claim 1, which is characterized in that the step（3）Middle soaking time and crucible material,
Structure, the type of cooling, crucible intrinsic inductance and it is required oxidation molybdenum single crystal size it is related.
7. according to the preparation method described in claim 1 to 6 any one, which is characterized in that step（1）In, the crucible
Material is metal oxide, high-thermal conductive metal material, aluminate, titanate and silicate.
8. preparation method according to claim 7, which is characterized in that the structure of the crucible is individual layer sidewall of crucible, bilayer
Sidewall of crucible or multilayer sidewall of crucible.
9. preparation method according to claim 6, which is characterized in that the type of cooling of the crucible is water cooling or naturally cold
But.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1382634A (en) * | 2002-03-15 | 2002-12-04 | 清华大学 | Process for synthesizing nano band of MoO3 monocrystal |
| JP2004203720A (en) * | 2002-12-26 | 2004-07-22 | National Institute For Materials Science | Molybdenum trioxide nano belt and method of manufacturing the same |
| CN102139923A (en) * | 2011-04-29 | 2011-08-03 | 西安工程大学 | Method for preparing molybdenum trioxide material with orthorhombic phase single crystal nano belt structure |
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2016
- 2016-11-29 CN CN201611071670.8A patent/CN106629850B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1382634A (en) * | 2002-03-15 | 2002-12-04 | 清华大学 | Process for synthesizing nano band of MoO3 monocrystal |
| JP2004203720A (en) * | 2002-12-26 | 2004-07-22 | National Institute For Materials Science | Molybdenum trioxide nano belt and method of manufacturing the same |
| CN102139923A (en) * | 2011-04-29 | 2011-08-03 | 西安工程大学 | Method for preparing molybdenum trioxide material with orthorhombic phase single crystal nano belt structure |
Non-Patent Citations (1)
| Title |
|---|
| Characteristics of molybdenum trioxide nanobelts prepared by thermal evaporation technique;T. Siciliano et al.;《Materials Chemistry and Physics》;20091231;第114卷;第687页右栏最后一段和第691页左栏最后一段 * |
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