CN108163892A - A kind of single agents autoreaction prepares octahedra crystal form Ta2O5The method of nano particle - Google Patents
A kind of single agents autoreaction prepares octahedra crystal form Ta2O5The method of nano particle Download PDFInfo
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- CN108163892A CN108163892A CN201810216220.6A CN201810216220A CN108163892A CN 108163892 A CN108163892 A CN 108163892A CN 201810216220 A CN201810216220 A CN 201810216220A CN 108163892 A CN108163892 A CN 108163892A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G35/00—Compounds of tantalum
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/41—Particle morphology extending in three dimensions octahedron-like
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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Abstract
The invention discloses single agents autoreactions to prepare octahedra crystal form Ta2O5The method of nano particle, includes the following steps：(1) it is soluble in water to choose potassium floutaramite powder, potassium floutaramite weak solution is placed in pretreated noble metal pipe, sealed；(2) the noble metal pipe of sealing is placed in hydrothermal reaction kettle, sealing, it is 200~500 DEG C to adjust the temperature in hydrothermal reaction kettle, and inert gas or deionized water is used to adjust in hydrothermal reaction kettle pressure as 50~200MPa, reaction 12~for 24 hours is hydrolyzed, reaction kettle is cooled to room temperature after reaction；(3) hydrothermal reaction kettle is opened, the noble metal pipe after taking-up reaction is simultaneously opened, and recycles residual solution, collects sample, and octahedra crystal form Ta is obtained after washing, drying2O5Nano particle.This method is using single agents as synthesis material, and of low cost, energy consumption is small, pollution-free, the Ta prepared2O5Nano particle crystal form is intact, in octahedral build.
Description
Technical field
The invention belongs to technical field of nano material, and in particular to a kind of single agents autoreaction prepares octahedra crystal form
Ta2O5The method of nano particle.
Background technology
Ta2O5As a kind of typical wide band gap semiconducter (energy gap 3.9eV), there is the characteristics of many prominent, such as
Good chemical stability, thermal stability, high-dielectric coefficient, high-melting-point, high mechanical properties, high-biocompatibility and it is easy to half
The features such as conductor integrated circuit/technique is mutually compatible with makes it in chemical reaction vessel, medical instrument, capacitor, integrated circuit, face
The fields such as material degradation, sewage disposal and photocatalysis suffer from being widely applied prospect.
At present about Ta2O5Film report is more, and preparation method is also varied；For Ta2O5The preparation of particle is similarly
People is caused to pay close attention to, such as Chen Ying in 2009 to Ta2O5Nano particle is studied, and shows Ta2O5With TiO2Similar near purple
Good photocatalysis performance is shown under the irradiation of outer light, this causes in Ta2O5Reach empty in the research and utilization of photocatalysis field
Preceding development.
Ta common at present2O5Preparation method has radio frequency sputtering method, sol-gal process, chemical vapor infiltration and pulse to swash
Photodeposition.Such as 2010, using ethanol tantalum as raw material, oleic acid made surfactant and has successfully prepared 20- Huang H. et al.
25nm Ta2O5Nano particle, but the sufficiently complex preparation flow of whole preparation process is long；Anandan S. etc. 2012 with
Hydro-thermal method is successfully prepared to obtain the Ta of 20-30nm2O5Particle, diethanol amine is used as stabilizer in experiment；In Li J in 2013
Et al. employ a kind of simpler method for the first time and prepared Ta2O5Nano particle, ethanol tantalum and alcohol are stirred by they
Light alcohol after uniformly, after alcohol burn totally afterwards the white particle that obtains grain size is prepared in calcining under the conditions of 800 DEG C again
It is distributed as the Ta of 500-1000nm2O5Particle.Ta made above2O5Perhaps program is complicated for the method for nano particle, perhaps cost
Height, perhaps energy consumption is larger, perhaps has pollution, and the Ta prepared to environment2O5Nano particle crystal form is also to be improved, this is certain
Ta is constrained in degree2O5Utilization of the nano material in industrial production and development.
Invention content
The purpose of the present invention is to provide a kind of single agents autoreactions to prepare octahedra crystal form Ta2O5The side of nano particle
Method, this method is using single agents as synthesis material, and of low cost, energy consumption is small, pollution-free, the Ta prepared2O5Nanometer
Grain crystal form is intact, in octahedral build.
The above-mentioned purpose of the present invention is achieved by the following technical solution：A kind of single agents autoreaction prepares octahedral
Body crystal form Ta2O5The method of nano particle, includes the following steps：
(1) it is soluble in water to choose potassium floutaramite powder, obtains potassium floutaramite weak solution, potassium floutaramite weak solution is placed in pre-
In processed noble metal pipe, then by the noble metal seal of tube；
(2) the noble metal pipe of sealing is placed in hydrothermal reaction kettle, then seals hydrothermal reaction kettle, adjust hydro-thermal reaction
Temperature in kettle is 200~500 DEG C, and use in inert gas or deionized water adjusting hydrothermal reaction kettle pressure for 50~
200MPa is hydrolyzed reaction 12~for 24 hours, hydrothermal reaction kettle is cooled to room temperature after reaction；
(3) hydrothermal reaction kettle is opened, take out the noble metal pipe after reaction and is opened, recycles residual solution, sample is collected, washes
Wash, dry after obtain octahedra crystal form Ta2O5Nano particle.
Octahedra crystal form Ta is prepared in above-mentioned single agents autoreaction2O5In the method for nano particle：
Potassium floutaramite (K in step (1)2TaF7) powder Optimization Analysis purity grade, avoid interference of the impurity to experiment.
The concentration of potassium floutaramite weak solution is preferably 0.001~0.005mol/L described in step (1), and volume preferably accounts for
The 40%~60% of noble metal pipe total volume.
Water described in step (1) is preferably deionized water or distilled water.
The pretreatment of noble metal pipe described in step (1) is：Noble metal pipe is chosen, through including truncation, acid boils, washs and quenches
Fire processing, it is ensured that influence to test, and the complete seal of guarantee fund's pipe without other impurities in gold pipe.
The wherein described noble metal includes silver, gold, platinum gold, silver palladium, gold-palladium or platinum-nickel alloys.
When in step (1) by the noble metal seal of tube, potassium floutaramite weak solution is first injected into sealing in noble metal pipe, Ran Houjin
Row weigh simultaneously in 100~120 DEG C of drying boxes dry more than 2h, after weigh again, it is ensured that front and rear quality error be less than 0.001g,
Ensure that it is fully sealed.
Preferably 110 DEG C of drying temperature in step (1).
Further, reaction temperature is preferably 400~500 DEG C in step (1), and pressure is preferably 150~200MPa, reaction
Time is preferably 12~14h.
Inert gas described in step (2) is preferably argon gas or helium.
Fast cooling is carried out to hydrothermal reaction kettle it is preferable to use ice water during cooling in step (2) or constant pressure cools down.
Reaction time in step (2) does not include heating and cools down the consumed time, is anti-under assigned temperature and pressure
Between seasonable.
It needs to carry out the noble metal pipe after reaction clean, drying after reaction in step (3), weigh, so that it is guaranteed that experiment
The validity of progress.
Residual solution described in step (3) includes potassium floutaramite, hydrofluoric acid and potassium fluoride, and the residual solution can recycle
It is recycled after processing as initial soln, while can to a certain degree eliminate hydrofluoric acid pollution.
When sample is collected in step (3), residual solution is first taken out, it will be in noble metal pipe with deionized water and absolute ethyl alcohol
Wall respectively washing 2~3 times, then collect the sample being attached on noble metal inside pipe wall, up to octahedra crystal form Ta after drying2O5It receives
Rice grain.
Drying can be preserved using air-dried or drying basin in step (3).
The octahedra crystal form Ta obtained in step (3)2O5The grain size of nano particle is 20~100nm.
Single agents autoreaction of the present invention prepares octahedra crystal form Ta2O5The core of the method for nano particle is to utilize fluorine
Potassium tantalate single agents generate Ta under the conditions of specific temperature and pressure by the hydrolysis of itself2O5Nano particle, it is used
Unique core reagent for potassium floutaramite solution, under hydrothermal conditions, with water successively following hydrolysis occurs for potassium floutaramite：
K2TaF7+H2O=K2Ta(OH)F6+HF
K2Ta(OH)F6+H2O=K2Ta(OH)2F5+HF
K2Ta(OH)F6+H2O=K2Ta(OH)3F4+HF
K2Ta(OH)F6+H2O=K2Ta(OH)4F3+HF
K2Ta(OH)F6+H2O=Ta (OH)5+2KF+HF
2Ta(OH)5=Nb2O5↓+5H2O
Compared with prior art, the invention has the advantages that：
(1) the method for the present invention passes through single agents autoreaction synthesizing octahedral crystal form Ta2O5Nano particle avoids tradition
The use of a variety of predecessors and pattern controlling agent and complex process steps in technical process, therefore this method is simple for process, easy
Rigorous efficiently in operation and control, advantage of lower cost, and experimentation, the reaction time is short, and reaction temperature is relatively low；
(2) the method for the present invention using potassium floutaramite solution as single agents, by potassium floutaramite under hydrothermal conditions oneself
The octahedra crystal form Ta of hydrolysis generation of body2O5Nano particle generates octahedra crystal form so as to fulfill single agents autoreaction
Ta2O5Nano particle；
(3) the method for the present invention makees housing using noble metal pipe can ensure that reactant with other substance reactions, and can not protected
The leakproofness and validity of reaction process are demonstrate,proved, energy consumption is small, simplifies complicated reaction process；
(4) the incomplete hydrolysis synthesizing octahedral crystal form Ta that the method for the present invention passes through potassium floutaramite itself2O5Nanometer
Grain, recycling solution is mainly comprising potassium floutaramite, hydrofluoric acid and potassium fluoride, and recycling solution is by processing, such as incorporation oxidation thereto
Tantalum powder can continue hydrofluoric acid and potassium fluoride to synthesize potassium floutaramite, and the recycling solution obtained can continue on for the present invention's
Initial feed, on the one hand effectively can recycle and reduce cost, on the other hand can eliminate hydrofluoric acid pollution, maintain process safety, note
Weight environmental protection；
(5) Ta that the method for the present invention synthesizes2O5Nano particle crystal form is intact, and in octahedral build, grain size is 20~100nm,
It suffers from being widely applied prospect in fields such as pigment degradation, sewage disposal and photocatalysis.
Description of the drawings
Fig. 1 is the Ta prepared in 1-5 of the embodiment of the present invention2O5The LR laser raman collection of illustrative plates of nano particle；
Fig. 2 is the Ta prepared in the embodiment of the present invention 12O5The stereoscan photograph of nano particle；
Fig. 3 is the Ta prepared in the embodiment of the present invention 22O5The stereoscan photograph of nano particle；
Fig. 4 is the Ta prepared in the embodiment of the present invention 32O5The stereoscan photograph of nano particle；
Fig. 5 is the Ta prepared in the embodiment of the present invention 42O5The stereoscan photograph of nano particle；
Fig. 6 is the Ta prepared in the embodiment of the present invention 52O5The stereoscan photograph of nano particle.
Specific embodiment
With reference to embodiment and attached drawing, the present invention is further illustrated, but the scope of protection of present invention is for example anti-
Answer device and reaction temperature, the volume of reaction time and reaction liquid is not limited to embodiment and is lifted.
Embodiment 1
Single agents autoreaction provided in this embodiment prepares octahedra crystal form Ta2O5The method of nano particle, including following
Step：
(1) the high-purity gold pipe of a diameter of 3~5mm is truncated into 5cm or so, be placed in equipped with 0.01mol/L dust technologies
Beaker in, then beaker is placed in 80 DEG C of heating plate and carries out acid and boils, make to be washed with deionized later and quenching treatment,
And one end is shifted to an earlier date into sealing, it is ensured that free from admixture and crack in golden pipe；
(2) by the potassium floutaramite (K of 0.098g purity assays2TaF7) powder is dissolved in 250mL deionized waters, fully dissolve
0.001mol/L K are made2TaF7The reaction solution of preparation is taken about 0.2mL to put into golden pipe by solution, and compactedness control is 40%
~60% or so, and sealing is carried out, weighing record is carried out after sealing, the golden pipe equipped with solution example is then put into 110 DEG C of bakings
Dry more than case 2h, after weighed again, it is ensured that it is front and rear weighing quality error be less than 0.001g, illustrate that golden composite pipe tightness is intact；
(3) it will confirm that leakproofness is intact and the golden pipe of solution example is housed and put high temperature and pressure hydro-thermal reaction kettle into, tighten anti-
After answering kettle, the leakproofness of reaction kettle is checked, argon gas is injected extremely into kettle by gas boosting pump and ventilation pipe after confirmation is errorless
Pressure 60MPa as initial pressure, closes shut-off valve and stops gas injection, reaction kettle is heated by heating furnace, setting reaction
Temperature is 200 DEG C；
(4) temperature is risen to after 200 DEG C, shut-off valve in opening steps (3), continues supplement injection argon gas to pressure 100MPa
And keep stablizing and reaction 12h is carried out under Temperature-pressure Conditions, pouring reaction kettle in leaching step (3) using ice water after the completion of reaction carries out quickly
Cooling or constant pressure are cooled to room temperature；
(5) reaction kettle in step (4) is opened, the golden pipe in reaction kettle is taken out, is clean, dries and weighs, it is ensured that is anti-
The leakproofness and validity of process are answered, golden pipe is broken after confirmation is errorless, recycles its residual solution, washed using deionized water, alcohol
It washs golden inside pipe wall each 2~3 times, makes to be attached to the Ta of gold inside pipe wall2O5Nanoparticle sample is clean, then deposit sample is used certainly
Right wind can obtain Ta after air-drying or drying ware drying2O5Nano particle；
(6) by the Ta of acquisition2O5Nanoparticle sample carries out Raman analysis and morphology analysis, and (a) is LR laser raman in Fig. 1
Analysis shows that the nano particle obtained is Ta2O5Nano particle, the Ta of Fig. 2 stereoscan photographs display synthesis2O5Nanometer
Grain, crystal form is poor, based on its shape-subhedral, a diameter of 20~50nm；
(7) residual solution this be mainly potassium floutaramite, hydrofluoric acid and potassium fluoride, this solution is performed some processing, still may be used
To be re-used as above-mentioned initial reaction solution.
Embodiment 2
Octahedron crystal form Ta provided in this embodiment2O5The preparation method of nano particle, includes the following steps：
(1) pre-treatment of platinum pipe is the same as embodiment 1；
(2) by the potassium floutaramite (K of 0.196g purity assays2TaF7) powder is dissolved in 250mL deionized waters, fully dissolve
0.002mol/L K are made2TaF7The reaction solution of preparation is taken about 0.2mL to put into platinum pipe by solution, and compactedness control is
40%~60% or so, and sealing is carried out, weighing record is carried out after sealing, is then put into the platinum pipe equipped with solution example
110 DEG C of more than drying box 2h, after weighed again, it is ensured that it is front and rear weighing quality error be less than 0.001g, illustrate that platinum pipe is close
Envelope property is intact；
(3) it will confirm that leakproofness is intact and the platinum pipe of solution example is housed and put high-temperature high-pressure reaction kettle into, tighten reaction
After kettle, check the leakproofness of reaction kettle, confirm it is errorless after argon gas is injected into kettle by ventilation pipe to pressure 60MPa, as
Initial pressure closes shut-off valve and stops gas injection, reaction kettle is heated by heating furnace, and setting reaction temperature is 200 DEG C；
(4) temperature is risen to after 200 DEG C, shut-off valve in opening steps (3), continues supplement injection argon gas to pressure 200MPa
And keep stablizing and reaction 12h is carried out under Temperature-pressure Conditions, pouring reaction kettle in leaching step (3) using ice water after the completion of reaction carries out quickly
Cooling or constant pressure are cooled to room temperature；
(5) reaction kettle in step (4) is opened, the platinum pipe in reaction kettle is taken out, is clean, dries and weighs, it is ensured that
The leakproofness and validity of reaction process break platinum pipe after confirmation is errorless, recycle its residual solution, use deionized water, wine
Fine purifiation washs platinum inside pipe wall each 2~3 times, makes to be attached to the Ta of platinum inside pipe wall2O5Nanoparticle sample is clean, then will precipitate sample
Product can obtain Ta after air-drying or drying ware drying with natural wind2O5Nano particle；
(6) by the Ta of acquisition2O5Nanoparticle sample carries out Raman analysis and morphology analysis, and Fig. 1 (b) is LR laser raman point
Analysis shows that obtained nano particle is Ta2O5Nano particle, the Ta of Fig. 3 stereoscan photographs display synthesis2O5Nano particle,
Crystal form is poor, its shape-subhedral, a diameter of 20~80nm；
(7) recycling of residual solution is the same as embodiment 1.
Embodiment 3
Octahedron crystal form Ta provided in this embodiment2O5The preparation method of nano particle, includes the following steps：
(1) pre-treatment of gold-palladium pipe is the same as embodiment 1；
(2) by the potassium floutaramite (K of 0.49g purity assays2TaF7) powder is dissolved in 250mL deionized waters, abundant dissolving system
Obtain 0.005mol/L K2TaF7The reaction solution of preparation is taken about 0.2mL to put into gold-palladium pipe by solution, and compactedness control is 40%
~60% or so, and sealing is carried out, weighing record is carried out after sealing, the gold-palladium pipe equipped with solution example is then put into 110 DEG C
More than drying box 2h, after weighed again, it is ensured that it is front and rear weighing quality error be less than 0.001g, illustrate that gold-palladium composite pipe tightness is complete
It is good；
(3) it will confirm that leakproofness is intact and the gold-palladium pipe of solution example is housed and put high-temperature high-pressure reaction kettle into, and inject and go
Ionized water after tightening reaction kettle, checks the leakproofness of reaction kettle, after confirmation is errorless by liquid booster pump into kettle as medium
Inject deionized water to pressure 50MPa, as initial pressure, close shut-off valve and stop gas injection, by heating furnace to reaction kettle into
Row heating, setting reaction temperature are 300 DEG C；
(4) temperature is risen to after 300 DEG C, shut-off valve in opening steps (3), continues supplement injection deionized water to pressure
100MPa simultaneously keeps stablizing and is reacted under Temperature-pressure Conditions for 24 hours, after the completion of reaction using ice water pour in leaching step (3) reaction kettle into
Row fast cooling or constant pressure are cooled to room temperature；
(5) reaction kettle in step (4) is opened, the gold-palladium pipe in reaction kettle is taken out, is clean, dries and weighs, it is ensured that
The leakproofness and validity of reaction process break gold-palladium pipe after confirmation is errorless, recycle its residual solution, use deionized water, wine
Fine purifiation washs gold-palladium inside pipe wall each 2~3 times, makes to be attached to the Ta of gold-palladium inside pipe wall2O5Nanoparticle sample is clean, then will precipitate sample
Product can obtain Ta after air-drying or drying ware drying with natural wind2O5Nano particle；
(6) by the Ta of acquisition2O5Nanoparticle sample carries out Raman analysis and morphology analysis, and Fig. 1 (c) is LR laser raman point
Analysis shows that obtained nano particle is Ta2O5Nano particle, the Ta of Fig. 4 stereoscan photographs display synthesis2O5Nano particle,
Since initial concentration is higher, a large amount of nano particles is caused closely to be arranged, wherein octahedra crystal form is more complete, a diameter of 20~
100nm；
(7) recycling of residual solution is the same as embodiment 1.
Embodiment 4
Octahedron crystal form Ta provided in this embodiment2O5The preparation method of nano particle, includes the following steps：
(1) pre-treatment of gold tube is the same as embodiment 1；
(2) by the potassium floutaramite (K of 0.098g purity assays2TaF7) powder is dissolved in 250mL deionized waters, fully dissolve
0.001mol/L K are made2TaF7The reaction solution of preparation is taken about 0.2mL to put into golden pipe by solution, and compactedness control is 40%
~60% or so, and sealing is carried out, weighing record is carried out after sealing, the golden pipe equipped with solution example is then put into 100 DEG C of bakings
Dry more than case 2h, after weighed again, it is ensured that it is front and rear weighing quality error be less than 0.001g, illustrate that golden composite pipe tightness is intact；
(3) will confirm that leakproofness is intact and golden pipe equipped with solution example puts high-temperature high-pressure reaction kettle into, and inject go from
Sub- water after tightening reaction kettle, checks the leakproofness of reaction kettle, is noted after confirmation is errorless by liquid booster pump into kettle as medium
Enter deionized water to pressure 60MPa, as initial pressure, close shut-off valve and stop gas injection, reaction kettle is carried out by heating furnace
Heating, setting reaction temperature are 400 DEG C；
(4) temperature is risen to after 400 DEG C, shut-off valve in opening steps (3), continues supplement injection deionized water to pressure
150MPa simultaneously keeps stablizing reaction 12h is carried out under Temperature-pressure Conditions, after the completion of reaction using ice water pour in leaching step (3) reaction kettle into
Row fast cooling or constant pressure are cooled to room temperature；
(5) reaction kettle in step (4) is opened, the golden pipe in reaction kettle is taken out, is clean, dries and weighs, it is ensured that is anti-
The leakproofness and validity of process are answered, golden pipe is broken after confirmation is errorless, recycles its residual solution, washed using deionized water, alcohol
It washs golden inside pipe wall each 2~3 times, makes to be attached to the Ta of gold inside pipe wall2O5Nanoparticle sample is clean, then deposit sample is used certainly
Right wind can obtain Ta after air-drying or drying ware drying2O5Nano particle；
(6) by the Ta of acquisition2O5Nanoparticle sample carries out Raman analysis and morphology analysis, and Fig. 1 (d) is LR laser raman point
Analysis shows that obtained nano particle is Ta2O5Nano particle, the Ta of Fig. 5 stereoscan photographs display synthesis2O5Nano particle,
Octahedra crystal form is more complete, a diameter of 50~100nm；
(7) recycling of residual solution is the same as embodiment 1.
Embodiment 5
Octahedron crystal form Ta provided in this embodiment2O5The preparation method of nano particle, includes the following steps：
(1) pre-treatment of gold tube is the same as embodiment 1；
(2) by the potassium floutaramite (K of 0.098g purity assays2TaF7) powder is dissolved in 250mL deionized waters, fully dissolve
0.001mol/L K are made2TaF7The reaction solution of preparation is taken about 0.2mL to put into golden pipe by solution, and compactedness control is 40%
~60% or so, and sealing is carried out, weighing record is carried out after sealing, the golden pipe equipped with solution example is then put into 110 DEG C of bakings
Dry more than case 2h, after weighed again, it is ensured that it is front and rear weighing quality error be less than 0.001g, illustrate that golden composite pipe tightness is intact；
(3) will confirm that leakproofness is intact and golden pipe equipped with solution example puts high-temperature high-pressure reaction kettle into, and inject go from
Sub- water after tightening reaction kettle, checks the leakproofness of reaction kettle, is noted after confirmation is errorless by liquid booster pump into kettle as medium
Enter deionized water to pressure 60MPa, as initial pressure, close shut-off valve and stop gas injection, reaction kettle is carried out by heating furnace
Heating, setting reaction temperature are 500 DEG C；
(4) temperature is risen to after 500 DEG C, shut-off valve in opening steps (3), continues supplement injection deionized water to pressure
200MPa simultaneously keeps stablizing reaction 12h is carried out under Temperature-pressure Conditions, after the completion of reaction using ice water pour in leaching step (3) reaction kettle into
Row fast cooling or constant pressure are cooled to room temperature；
(5) reaction kettle in step (4) is opened, the golden pipe in reaction kettle is taken out, is clean, dries and weighs, it is ensured that is anti-
The leakproofness and validity of process are answered, golden pipe is broken after confirmation is errorless, recycles its residual solution, washed using deionized water, alcohol
It washs golden inside pipe wall each 2~3 times, makes to be attached to the Ta of gold inside pipe wall2O5Nanoparticle sample is clean, then deposit sample is used certainly
Right wind can obtain Ta after air-drying or drying ware drying2O5Nano particle；
(6) by the Ta of acquisition2O5Nanoparticle sample carries out Raman analysis and morphology analysis, and Fig. 1 (e) is LR laser raman point
Analysis shows that obtained nano particle is Ta2O5Nano particle, the Ta of Fig. 6 stereoscan photographs display synthesis2O5Nano particle,
Octahedra crystal form is more complete, a diameter of 50~100nm；
(7) recycling of residual solution is the same as embodiment 1.
Above-described embodiment is the preferable embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any Spirit Essences without departing from the present invention with made under principle change, modification, replacement, combine, simplification,
Equivalent substitute mode is should be, is included in protection scope of the present invention.
Claims (9)
1. a kind of single agents autoreaction prepares octahedra crystal form Ta2O5The method of nano particle, it is characterized in that including following step
Suddenly：
(1) it is soluble in water to choose potassium floutaramite powder, obtains potassium floutaramite weak solution, potassium floutaramite weak solution is placed in pretreatment
In the noble metal pipe crossed, then by the noble metal seal of tube；
(2) the noble metal pipe of sealing is placed in hydrothermal reaction kettle, then seals hydrothermal reaction kettle, adjusted in hydrothermal reaction kettle
Temperature for 200~500 DEG C, and use in inert gas or deionized water adjusting hydrothermal reaction kettle pressure as 50~200MPa,
Reaction 12~for 24 hours is hydrolyzed, hydrothermal reaction kettle is cooled to room temperature after reaction；
(3) hydrothermal reaction kettle is opened, take out the noble metal pipe after reaction and is opened, recycling residual solution, collection sample, washing,
Octahedra crystal form Ta is obtained after drying2O5Nano particle.
2. single agents autoreaction according to claim 1 prepares octahedra crystal form Ta2O5The method of nano particle, it is special
Sign is：A concentration of 0.001~0.005mol/L of potassium floutaramite weak solution described in step (1), it is total that volume accounts for noble metal pipe
The 40%~60% of volume.
3. single agents autoreaction according to claim 1 prepares octahedra crystal form Ta2O5The method of nano particle, it is special
Sign is：The pretreatment of noble metal pipe described in step (1) is：Noble metal pipe is chosen, through including truncation, acid is boiled, washs and quenched
Processing, wherein the noble metal includes silver, gold, platinum gold, silver palladium, gold-palladium or platinum-nickel alloys.
4. single agents autoreaction according to claim 1 prepares octahedra crystal form Ta2O5The method of nano particle, it is special
Sign is：When in step (1) by the noble metal seal of tube, potassium floutaramite weak solution is first injected into sealing in noble metal pipe, is adjusted after weighing
Temperature is saved as 100~120 DEG C of drying more than 2h, weighs gold tube again, it is ensured that front and rear quality error is less than 0.001g.
5. single agents autoreaction according to claim 1 prepares octahedra crystal form Ta2O5The method of nano particle, it is special
Sign is：Inert gas described in step (2) is argon gas or helium.
6. single agents autoreaction according to claim 1 prepares octahedra crystal form Ta2O5The method of nano particle, it is special
Sign is：Fast cooling is carried out to hydrothermal reaction kettle using ice water during cooling in step (2) or constant pressure cools down.
7. single agents autoreaction according to claim 1 prepares octahedra crystal form Ta2O5The method of nano particle, it is special
Sign is：Residual solution described in step (3) includes potassium floutaramite, hydrofluoric acid and potassium fluoride, and the residual solution can recycle place
It is recycled after reason as initial soln.
8. single agents autoreaction according to claim 1 prepares octahedra crystal form Ta2O5The method of nano particle, it is special
Sign is：When sample is collected in step (3), residual solution is first taken out, with deionized water and absolute ethyl alcohol by the inner wall of noble metal pipe
It is each to wash 2~3 times, the sample being attached on noble metal inside pipe wall is then collected, up to octahedra crystal form Ta after drying2O5Nanometer
Particle.
9. single agents autoreaction according to claim 1 prepares octahedra crystal form Ta2O5The method of nano particle, it is special
Sign is：The octahedra crystal form Ta obtained in step (3)2O5The grain size of nano particle is 20~100nm.
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