CN107840368A - A kind of nanometer sheet self assembly sub-micrometer flower-shape M-phase vanadium dioxide powder and preparation method thereof - Google Patents
A kind of nanometer sheet self assembly sub-micrometer flower-shape M-phase vanadium dioxide powder and preparation method thereof Download PDFInfo
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- CN107840368A CN107840368A CN201711224637.9A CN201711224637A CN107840368A CN 107840368 A CN107840368 A CN 107840368A CN 201711224637 A CN201711224637 A CN 201711224637A CN 107840368 A CN107840368 A CN 107840368A
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Abstract
A kind of nanometer sheet self assembly sub-micrometer flower-shape M-phase vanadium dioxide powder and preparation method thereof, the present invention has synthesized the nanometer sheet self assembly sub-micrometer flower-shape hypovanadic oxide powder of high-purity using a step hydrothermal reaction at low temperature, and this method course of reaction is simple, temperature is low, easily-controllable and do not need large scale equipment and the reaction condition of harshness.When above-mentioned product is applied as lithium ion battery negative material with production oxygen elctro-catalyst, it can show excellent chemical property and electrocatalysis characteristic.The sub-micro popped rice that the nanometer sheet self assembly sub-micrometer flower-shape M-phase vanadium dioxide powder as made of the preparation method of the present invention is about 1 μm by uniform diameter forms, part sub-micro popped rice is assembled, the nanometer sheet that it is about 10nm by thickness that sub-micro popped rice, which is, is assembled in a manner of intercalation, and nanometer sheet shows the characteristic along the growth of (011) high preferred orientation.
Description
Technical field
The present invention relates to a kind of M-phase vanadium dioxide powder and preparation method thereof, and in particular to a kind of nanometer sheet self assembly is sub-
Flower-shaped M-phase vanadium dioxide powder of micron and preparation method thereof.
Background technology
Vanadium dioxide is a kind of complicated polycrystalline material with a variety of adjustable functions.Up to now, it has been reported that
It is equal more than the vanadium dioxide of 10 kinds of crystalline phases, including B phases, M phases, R phases, A phases and C.In these vanadium dioxide, due to crystallizing
The reversible transition of one-level metallic state and semiconductor form can be realized under room temperature condition, M phase hypovanadic oxides are widely used
[Liang S,Shi Q,Zhu H,et al.One-Step Hydrothermal Synthesis of W-Doped VO2(M)
Nanorods with a Tunable Phase-Transition Temperature for Infrared Smart
Windows[J].2016,1(6):1139-1148.].Although having there is the synthesis that substantial amounts of researcher reports vanadium dioxide,
It is but but very rare as the report of reaction raw materials using sodium metavanadate and thioacetamide.At present, answering on M phase hypovanadic oxides
[Li Dengbing, Li Ming, Pan Jing, the preparation of the monodispersed M phase hypovanadic oxides nano particles of is waited with infrared detector is concentrated mainly on
Method:, CN104071843A [P] .2014.], intelligent temperature control film, gas sensor, catalyst, thermochromism [Liu Xiangli,
King is into moving a kind of methods using a large amount of m phase vanadium dioxide nanowires of pulsed laser deposition technique fast-growth of:,CN
104762605A [P] .2015.] and switch etc. field, be rarely reported on its application as lithium ion battery negative material.
It is mostly spherical, bar-shaped to synthesize the pattern of M phase hypovanadic oxides, and rare nanometer sheet independently fills the report of micron floriform appearance.
The content of the invention
It is an object of the invention to provide a kind of course of reaction is simple, temperature is low, easily-controllable and do not need large scale equipment and severe
Carve nanometer sheet self assembly sub-micrometer flower-shape M-phase vanadium dioxide powder of reaction condition and preparation method thereof.
To reach above-mentioned purpose, preparation method of the invention is：
Step 1：Take 0.8~1.2g sodium metavanadates and 1.6~2.0g thioacetamides at the same be added to 55~65ml go from
In sub- water, magnetic agitation or ultrasonic disperse obtain half settled solution A；
Step 2：Then 0.4~0.6mol/L ammonia spirit is added dropwise dropwise into solution A, until solution ph reaches
10~10.2, obtain solution B；
Step 3：Seal, liner is loaded on solid in outer kettle after solution B is poured into reaction liner by 55~65% packing ratio
It is placed in after fixed in homogeneous reaction instrument, by room temperature being heated to 155~165 DEG C under 5~15r/min speed conditions, to carry out hydro-thermals anti-
Should；
Step 4：Reactor is naturally cooled to room temperature by hydro-thermal reaction after terminating, by product after water and alcohol alternately clean
Collect product；
Step 5：The product of collection is placed in the cold well of freeze drier and freezed, then by the product after freezing
It is placed in pallet, covers seal closure, be evacuated down to 10~20Pa, collection product obtains nanometer sheet from group after drying 12~18h
Fill sub-micrometer flower-shape M-phase vanadium dioxide powder.
The step 1 magnetic agitation or ultrasonic time are 55~65min, and speed of agitator is 800~1000r/min.
Ammonia spirit will be added dropwise in solution A dropwise under the conditions of the step 2 regulation continuous magnetic agitations of pH, control ammonia
The rate of addition of the aqueous solution is 0.05~0.07ml/min, drips previous drop ammonia spirit, and stirring is until solution ph is stable
Afterwards, then next drop ammonia spirit is instilled, until reacting liquid pH value is adjusted to 10.1~10.2.
The step 3 the hydro-thermal reaction time is 23~25h.
The cleaning of the step 4 is carried out using suction filtration or centrifugation.
The collection of the step 4 is carried out using suction filtration or centrifugation.
The freezing conditions of the step 5 are：- 60~-40 DEG C, freeze 2~5 hours.
The step 5 product seals before being put into pallet and being dried, with preservative film to it, and to preservative film
Carry out pricking hole processing, to ensure to its abundant drying under lower pressure.
The nanometer sheet self assembly sub-micrometer flower-shape M-phase vanadium dioxide powder as made of the preparation method of the present invention is by uniform
Diameter be about 1 μm sub-micro popped rice composition, part sub-micro popped rice assembled, and it by thickness is about 10nm that sub-micro popped rice, which is,
Nanometer sheet is assembled in a manner of intercalation, and nanometer sheet shows the characteristic along the growth of (011) high preferred orientation.
The present invention has synthesized the nanometer sheet self assembly sub-micrometer flower-shape vanadium dioxide of high-purity using a step hydrothermal reaction at low temperature
Powder, this method course of reaction is simple, temperature is low, it is easily-controllable and do not need large scale equipment and harshness reaction condition.When will be upper
State product apply for lithium ion battery negative material and production oxygen elctro-catalyst when, it can show excellent chemical property and
Electrocatalysis characteristic.
Specifically have the beneficial effect that：
(1) present invention using a step hydro-thermal reaction due to directly synthesizing final product, thus has low synthesis temperature
Degree, simple synthesis path, it is not necessary to large scale equipment and harsh reaction condition；
(2) present invention used in vanadium source be sodium metavanadate, sulphur source be thioacetamide, both raw materials are Common materials,
Raw material is cheap and easy to get, and cost is low, and yield is high, and reaction is easily-controllable, environmentally friendly without post-processing, can be adapted to extensive life
Production；
(3) the M phase hypovanadic oxide nanometer sheets prepared by the present invention have extra small thickness (~10nm), can not only produce
Larger specific surface area, but also more surface-active sites can be provided, and then chemical property can be lifted and electricity is urged
Change performance.In addition, this extra small thickness can not only shorten charge transfer path, but also can be provided for the storage of lithium ion
More avtive spots, so as to lifting the specific capacity of material and high rate performance.Meanwhile the titanium dioxide of this extra small thickness
Vanadium surface can expose more polyoxy and provide sufficient guarantee for production oxygen performance；
(4) self-assembled structures that the unique nanometer sheet of the M-phase vanadium dioxide powder prepared by the present invention is connected with each other, a side
Face can play good restraining function, and the on the other hand expansion and contraction also to nanometer sheet provides cushion space, so as to
Greatly to alleviate the Volume Changes of nanometer sheet, its cyclical stability is finally significantly improved；
(5) the unique intercalation shape sub-micron floral structure of M-phase vanadium dioxide powder prepared by the present invention can ensure electrolyte/
Electrolyte fully contacts with vanadium dioxide, then reduces electrochemical reaction/electro-catalysis resistance, further improving performance；
(6) M phase hypovanadic oxides nanometer sheet of the present invention has the characteristic along the growth of (011) high preferred orientation, its larger crystal face
Spacing can be the offer more fully boundary space of electrochemical reaction and electrocatalytic reaction；
(7) present invention needs the packing ratio in strict control course of reaction, and higher packing ratio can promote S2-Ion exchange
Oxygen in vanadic acid root, so as to produce VS2.Relatively low packing ratio is advantageous to S2 2-Formation, so as to cause VS4Generation.Therefore, instead
Synthesis of the packing ratio for pure phase M phase hypovanadic oxides is answered to play conclusive effect.
(8) present invention also needs to strictly control pH value in reaction simultaneously, compared with high pH value thioacetamide hydrolysis can be made big
The S of amount2-, so as to promote VS2Formed, while higher pH value can make a large amount of OH in solution be present-, so as to form VOOH.It is relatively low
PH value can make the substantial amounts of H of thioacetamide hydrolysis2S, so as to promote VS4Formed.Therefore, higher relatively low pH value is all unfavorable
In the synthesis of pure phase M phase hypovanadic oxides.
(9) concentration of ammonia spirit and regulative mode can directly affect depositing for V sources and S sources in precursors in the present invention
In state, so as to influence the generation to be chemically reacted in water-heat process, ultimately resulting in can be with the presence of this many dephasign in product.
If in addition, after changing weak base ammoniacal liquor into highly basic sodium hydroxide, sodium hydroxide, which is fully hydrolyzed caused OH-, can induce VOOH shape
Into.
(10) present invention does not introduce any template or surface-active during three-dimensional self-assembled structures are synthesized
Agent, whole self assembling process be by reaction raw materials self-template effect control, thus entirely react it is simple, easily-controllable, efficient and
Low cost；
(11) present invention prepare product chemistry composition it is homogeneous, purity is high, pattern is uniform, it is as negative electrode of lithium ion battery
Excellent performance can be shown when material and electro-catalysis regenerative agent.When being applied to lithium ion battery negative material, performance
Go out excellent chemical property, in 0.01~3.0 voltage range, 30,50,100,200,500,1000mAg-1Electric current
Under density, up to 324,254,207,163,102,65mAhg are shown-1Specific capacity；When returning to 30mAg-1Electric current
Under density, still there is 309mAhg-1Capacity be kept.
Brief description of the drawings
Fig. 1 is X-ray diffraction (XRD) figure that the embodiment of the present invention 1 prepares product.
Fig. 2 is (other conditions are identical with embodiment 1) institute after packing ratio in the embodiment of the present invention 1 is adjusted into 70%
Obtain the XRD of product.
Fig. 3 is (other conditions is identical with embodiment 1) after packing ratio in the embodiment of the present invention 1 is adjusted into 50%,
The XRD of products therefrom.
Fig. 4 is low power ESEM (SEM) figure that the embodiment of the present invention 1 prepares product.
Fig. 5 is the high power SEM figures that the embodiment of the present invention 1 prepares product.
Fig. 6 is the super-high power SEM figures that the embodiment of the present invention 1 prepares product.
Fig. 7 is low power transmission electron microscope (TEM) figure that the embodiment of the present invention 1 prepares product.
Fig. 8 is the high power TEM figures that the embodiment of the present invention 1 prepares product.
Fig. 9 is the super-high power TEM figures that the embodiment of the present invention 1 prepares product.
Figure 10 is the HRTEM figures that the embodiment of the present invention 1 prepares product.
Figure 11 is the high rate performance when embodiment of the present invention 1 prepares product as lithium ion battery negative material.
Embodiment
The present invention is described in further detail below in conjunction with the accompanying drawings.
Embodiment 1：
Step 1：Take 1.0g sodium metavanadates and 1.8g thioacetamides while be added in 60ml deionized waters, in 900r/
Magnetic agitation 60min obtains half settled solution A under min speed conditions；
Step 2：0.5mol/L ammonia spirits will be added drop-wise under the conditions of magnetic agitation in solution A dropwise, control ammonia spirit
Rate of addition be 0.06ml/min, drip previous drop ammonia spirit, after stirring is until solution ph is stable, then instill next
Ammonia spirit is dripped, until reacting liquid pH value is adjusted to 10.1, obtains solution B；
Step 3：Sealed after solution B is poured into reaction liner by 60% packing ratio, liner is rearmounted loaded on being fixed in outer kettle
In homogeneous reaction instrument, 160 DEG C of hydro-thermal reaction 24h are heated to by room temperature under 5r/min speed conditions；
Step 4：Reactor is naturally cooled to room temperature by hydro-thermal reaction after terminating, by product through water and alcohol alternately cleaning 3 times
After collect product；
Described cleaning and collection is carried out using suction filtration；
Step 5：The product of collection is placed in the cold well of freeze drier under the conditions of -40 DEG C and freezes 2 hours, then
Product after freezing is placed in pallet it sealed with preservative film, and preservative film is carried out to prick hole processing, covered afterwards
Seal closure, 12Pa is evacuated down to, collection product obtains nanometer sheet self assembly sub-micrometer flower-shape M phase hypovanadic oxides after drying 12h
Powder.
The diffraction maximum of synthesized product and the standard card (PDF# of M phase hypovanadic oxides are can be clearly seen that from Fig. 1
82-0661) fit like a glove, the product for illustrating synthesis is pure phase M phase hypovanadic oxides.In addition, smooth elongated diffraction maximum explanation should
Product has good crystallinity, and diffraction peak intensity corresponding to (011) crystal face is most strong, shows that the product has significant edge
(011) characteristic of high preferred orientation growth.
From figure 2 it can be seen that products therefrom is vanadium disulfide, when showing to increase reaction-filling ratio to 70%, product by
Vanadium dioxide is converted into vanadium disulfide, and reaction high pressure will promote S caused by higher packing ratio2-Replace in vanadium dioxide
Oxygen.Therefore, higher packing ratio is unfavorable for the synthesis of M phase hypovanadic oxides.
From figure 3, it can be seen that the main thing of products therefrom is mutually four vanadic sulfides, and along with sulphur simple substance dephasign, show
When reducing reaction-filling ratio to 50%, product is converted into four vanadic sulfides by vanadium dioxide, and relatively low packing ratio promotes S2 2-'s
Formed, then promote VS4Formation.Therefore, relatively low packing ratio is also unfavorable for the synthesis of M phase hypovanadic oxides.
Figure 4, it is seen that products therefrom is made up of uniform spherical structure, there is higher pattern uniformity,
Part-spherical is assembled.
From figure 5 it can be seen that the spherical structure of products therefrom shows sub-micrometer flower-shape, the diameter of micro-flowers is about 1 μ
m。
From fig. 6 it can be seen that the sub-micrometer flower-shape structure of products therefrom be by nanometer sheet in a manner of intercalation self assembly and
Into the thickness of nanometer sheet is about 10nm.
It can be seen from figure 7 that products therefrom has solid micron flower-like structure, and the diameter of micro-flowers is about 1 μm.
As can be seen from Figure 8, the micron floral structure of products therefrom is that self assembly forms in a manner of intercalation by nanometer sheet, and
The thickness of nanometer sheet is about 10nm.
It can be seen in figure 9 that the nanometer sheet of products therefrom has ultra-thin thickness.
The lattice fringe corresponding to M phase hypovanadic oxides is can be clearly seen that from Figure 10, it is higher to show that the product has
Crystallinity.
It can be seen from fig. 11 that in 0.01~3.00 voltage range, 30,50,100,200,500,
1000mAg-1Current density under, M phase hypovanadic oxides show up to 324,254,207,163,102,65mAhg-1Ratio
Capacity；When returning to 30mAg-1Current density under, still have 309mAhg-1Capacity be kept.
Embodiment 2：
Step 1：Take 0.8g sodium metavanadates and 1.7g thioacetamides while be added in 58ml deionized waters,
Magnetic agitation 55min obtains half settled solution A under 1000r/min speed conditions；
Step 2：0.4mol/L ammonia spirits will be added drop-wise under the conditions of magnetic agitation in solution A dropwise, control ammonia spirit
Rate of addition be 0.05ml/min, drip previous drop ammonia spirit, after stirring is until solution ph is stable, then instill next
Ammonia spirit is dripped, until reacting liquid pH value is adjusted to 10.2, obtains solution B；
Step 3：Sealed after solution B is poured into reaction liner by 55% packing ratio, liner is rearmounted loaded on being fixed in outer kettle
In homogeneous reaction instrument, 158 DEG C of hydro-thermal reaction 25h are heated to by room temperature under 8r/min speed conditions；
Step 4：Reactor is naturally cooled to room temperature by hydro-thermal reaction after terminating, by product through water and alcohol alternately cleaning 5 times
After collect product；
Described cleaning and collection is carried out using centrifugation；
Step 5：The product of collection is placed in the cold well of freeze drier under the conditions of -55 DEG C and freezes 4 hours, then
Product after freezing is placed in pallet it sealed with preservative film, and preservative film is carried out to prick hole processing, covered afterwards
Seal closure, 15Pa is evacuated down to, collection product obtains nanometer sheet self assembly sub-micrometer flower-shape M phase hypovanadic oxides after drying 15h
Powder.
Embodiment 3：
Step 1：Take 1.2g sodium metavanadates and 1.9g thioacetamides while be added in 55ml deionized waters, in 800r/
Magnetic agitation 65min obtains half settled solution A under min speed conditions；
Step 2：0.45mol/L ammonia spirits will be added drop-wise under the conditions of magnetic agitation in solution A dropwise, control ammoniacal liquor is molten
The rate of addition of liquid is 0.07ml/min, drips previous drop ammonia spirit, after stirring is until solution ph is stable, then is instilled down
One drop ammonia spirit, until reacting liquid pH value is adjusted to 10.1, obtains solution B；
Step 3：Sealed after solution B is poured into reaction liner by 65% packing ratio, liner is rearmounted loaded on being fixed in outer kettle
In homogeneous reaction instrument, 162 DEG C of hydro-thermal reaction 23h are heated to by room temperature under 12r/min speed conditions；
Step 4：Reactor is naturally cooled to room temperature by hydro-thermal reaction after terminating, by product through water and alcohol alternately cleaning 4 times
After collect product；
Described cleaning and collection is carried out using suction filtration；
Step 5：The product of collection is placed in the cold well of freeze drier under the conditions of -50 DEG C and freezes 3 hours, then
Product after freezing is placed in pallet it sealed with preservative film, and preservative film is carried out to prick hole processing, covered afterwards
Seal closure, 18Pa is evacuated down to, collection product obtains nanometer sheet self assembly sub-micrometer flower-shape M phase hypovanadic oxides after drying 17h
Powder.
Embodiment 4：
Step 1：Take 0.9g sodium metavanadates and 1.6g thioacetamides while be added in 62ml deionized waters, ultrasound point
Scattered 55min obtains half settled solution A；
Step 2：0.55mol/L ammonia spirits will be added drop-wise under the conditions of magnetic agitation in solution A dropwise, control ammoniacal liquor is molten
The rate of addition of liquid is 0.07ml/min, drips previous drop ammonia spirit, after stirring is until solution ph is stable, then is instilled down
One drop ammonia spirit, until reacting liquid pH value is adjusted to 10.2, obtains solution B；
Step 3：Sealed after solution B is poured into reaction liner by 58% packing ratio, liner is rearmounted loaded on being fixed in outer kettle
In homogeneous reaction instrument, 155 DEG C of hydro-thermal reaction 25h are heated to by room temperature under 15r/min speed conditions；
Step 4：Reactor is naturally cooled to room temperature by hydro-thermal reaction after terminating, by product through water and alcohol alternately cleaning 6 times
After collect product；
Described cleaning and collection is carried out using suction filtration；
Step 5：The product of collection is placed in the cold well of freeze drier under the conditions of -60 DEG C and freezes 5 hours, then
Product after freezing is placed in pallet it sealed with preservative film, and preservative film is carried out to prick hole processing, covered afterwards
Seal closure, 20Pa is evacuated down to, collection product obtains nanometer sheet self assembly sub-micrometer flower-shape M phase hypovanadic oxides after drying 14h
Powder.
Embodiment 5：
Step 1：Take 1.1g sodium metavanadates and 2.0g thioacetamides while be added in 65ml deionized waters, ultrasound point
Scattered 65min obtains half settled solution A；
Step 2：0.6mol/L ammonia spirits will be added drop-wise under the conditions of magnetic agitation in solution A dropwise, control ammonia spirit
Rate of addition be 0.05ml/min, drip previous drop ammonia spirit, after stirring is until solution ph is stable, then instill next
Ammonia spirit is dripped, until reacting liquid pH value is adjusted to 10.2, obtains solution B；
Step 3：Sealed after solution A is poured into reaction liner by 62% packing ratio, liner is rearmounted loaded on being fixed in outer kettle
In homogeneous reaction instrument, 165 DEG C of hydro-thermal reaction 23h are heated to by room temperature under 10r/min speed conditions；
Step 4：Reactor is naturally cooled to room temperature by hydro-thermal reaction after terminating, by product through water and alcohol alternately cleaning 5 times
After collect product；
Described cleaning and collection is carried out using suction filtration；
Step 5：The product of collection is placed in the cold well of freeze drier under the conditions of -45 DEG C and freezes 4 hours, then
Product after freezing is placed in pallet it sealed with preservative film, and preservative film is carried out to prick hole processing, covered afterwards
Seal closure, 10Pa is evacuated down to, collection product obtains nanometer sheet self assembly sub-micrometer flower-shape M phase hypovanadic oxides after drying 18h
Powder.
Claims (9)
- A kind of 1. preparation method of nanometer sheet self assembly sub-micrometer flower-shape M-phase vanadium dioxide powder, it is characterised in that：Step 1：Take 0.8~1.2g sodium metavanadates and 1.6~2.0g thioacetamides while be added to 55~65ml deionized waters In, magnetic agitation or ultrasonic disperse obtain half settled solution A；Step 2：Then 0.4~0.6mol/L ammonia spirit is added dropwise dropwise into solution A, until solution ph reach 10~ 10.2, obtain solution B；Step 3：Seal, liner is loaded in outer kettle after fixing after solution B is poured into reaction liner by 55~65% packing ratio It is placed in homogeneous reaction instrument, 155~165 DEG C of progress hydro-thermal reactions is heated to by room temperature under 5~15r/min speed conditions；Step 4：Reactor is naturally cooled to room temperature by hydro-thermal reaction after terminating, and product is collected after water and alcohol alternately clean Product；Step 5：The product of collection is placed in the cold well of freeze drier and freezed, be then placed in the product after freezing In pallet, seal closure is covered, is evacuated down to 10~20Pa, collection product obtains nanometer sheet self assembly Asia after drying 12~18h The flower-shaped M-phase vanadium dioxide powder of micron.
- 2. the preparation method of nanometer sheet self assembly sub-micrometer flower-shape M-phase vanadium dioxide powder according to claim 1, it is special Sign is：The step 1 magnetic agitation or ultrasonic time are 55~65min, and speed of agitator is 800~1000r/min.
- 3. the preparation method of nanometer sheet self assembly sub-micrometer flower-shape M-phase vanadium dioxide powder according to claim 1, it is special Sign is：Ammonia spirit will be added dropwise in solution A dropwise under the conditions of the step 2 regulation continuous magnetic agitations of pH, control ammoniacal liquor The rate of addition of solution is 0.05~0.07ml/min, drips previous drop ammonia spirit, after stirring is until solution ph is stable, Next drop ammonia spirit is instilled again, until reacting liquid pH value is adjusted to 10.1~10.2.
- 4. the preparation method of nanometer sheet self assembly sub-micrometer flower-shape M-phase vanadium dioxide powder according to claim 1, it is special Sign is：The step 3 the hydro-thermal reaction time is 23~25h.
- 5. the preparation method of nanometer sheet self assembly sub-micrometer flower-shape M-phase vanadium dioxide powder according to claim 1, it is special Sign is：The cleaning of the step 4 is carried out using suction filtration or centrifugation.
- 6. the preparation method of nanometer sheet self assembly sub-micrometer flower-shape M-phase vanadium dioxide powder according to claim 1, it is special Sign is：The collection of the step 4 is carried out using suction filtration or centrifugation.
- 7. the preparation method of nanometer sheet self assembly sub-micrometer flower-shape M-phase vanadium dioxide powder according to claim 1, it is special Sign is：The freezing conditions of the step 5 are：- 60~-40 DEG C, freeze 2~5 hours.
- 8. the preparation method of nanometer sheet self assembly sub-micrometer flower-shape M-phase vanadium dioxide powder according to claim 1, it is special Sign is：The step 5 product is sealed before being put into pallet and being dried, with preservative film to it, and preservative film is entered Row pricks hole processing, to ensure to its abundant drying under lower pressure.
- A kind of 9. nanometer sheet self assembly sub-micrometer flower-shape M phase hypovanadic oxide powder made of preparation method as claimed in claim 1 Body, it is characterised in that：The sub-micro popped rice that hypovanadic oxide powder is about 1 μm by uniform diameter forms, and part sub-micro popped rice enters Aggregation is gone, the nanometer sheet that it is about 10nm by thickness that sub-micro popped rice, which is, is assembled in a manner of intercalation, and nanometer sheet is shown Along the characteristic of (011) high preferred orientation growth.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109939699A (en) * | 2019-04-16 | 2019-06-28 | 湘潭大学 | A kind of molybdenum doping vanadium disulfide micron floral material and its preparation method and application |
| CN112209442A (en) * | 2020-10-16 | 2021-01-12 | 成都先进金属材料产业技术研究院有限公司 | Method for preparing M-phase vanadium dioxide nano powder by salt-assisted ultrasonic pyrolysis method |
| CN113184906A (en) * | 2021-05-13 | 2021-07-30 | 陕西科技大学 | One-step hydrothermal method for preparing V2O3Method of nanosphere |
| CN113213543A (en) * | 2021-05-13 | 2021-08-06 | 陕西科技大学 | MnO (MnO)2/V2O3Process for preparing nano composite material |
| CN113247951A (en) * | 2021-05-13 | 2021-08-13 | 陕西科技大学 | Self-assembly sheet VS2Preparation method of/S nanosheet |
| CN115058728A (en) * | 2022-07-13 | 2022-09-16 | 陕西科技大学 | Sheet V 4 O 9 Self-assembly nano ball-flower self-supporting electrode material and preparation method thereof |
| CN115092961A (en) * | 2022-07-14 | 2022-09-23 | 贵州大学 | Preparation method and application of hydroxyl vanadium oxide with hollow spherical shell structure |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109939699A (en) * | 2019-04-16 | 2019-06-28 | 湘潭大学 | A kind of molybdenum doping vanadium disulfide micron floral material and its preparation method and application |
| CN109939699B (en) * | 2019-04-16 | 2022-04-05 | 湘潭大学 | Molybdenum-doped vanadium disulfide micrometer flower material and preparation method and application thereof |
| CN112209442A (en) * | 2020-10-16 | 2021-01-12 | 成都先进金属材料产业技术研究院有限公司 | Method for preparing M-phase vanadium dioxide nano powder by salt-assisted ultrasonic pyrolysis method |
| CN112209442B (en) * | 2020-10-16 | 2022-07-29 | 成都先进金属材料产业技术研究院股份有限公司 | Method for preparing M-phase vanadium dioxide nano powder by salt-assisted ultrasonic pyrolysis method |
| CN113184906A (en) * | 2021-05-13 | 2021-07-30 | 陕西科技大学 | One-step hydrothermal method for preparing V2O3Method of nanosphere |
| CN113213543A (en) * | 2021-05-13 | 2021-08-06 | 陕西科技大学 | MnO (MnO)2/V2O3Process for preparing nano composite material |
| CN113247951A (en) * | 2021-05-13 | 2021-08-13 | 陕西科技大学 | Self-assembly sheet VS2Preparation method of/S nanosheet |
| CN115058728A (en) * | 2022-07-13 | 2022-09-16 | 陕西科技大学 | Sheet V 4 O 9 Self-assembly nano ball-flower self-supporting electrode material and preparation method thereof |
| CN115058728B (en) * | 2022-07-13 | 2023-06-20 | 陕西科技大学 | Flaky V 4 O 9 Self-assembled nanometer flower ball self-supporting electrode material and preparation method thereof |
| CN115092961A (en) * | 2022-07-14 | 2022-09-23 | 贵州大学 | Preparation method and application of hydroxyl vanadium oxide with hollow spherical shell structure |
| CN115092961B (en) * | 2022-07-14 | 2023-12-22 | 贵州大学 | Preparation method and application of hollow spherical shell structured vanadium oxyhydroxide |
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