CN106904649A - A kind of in-situ control method of nano-cerium oxide form and crystal face - Google Patents
A kind of in-situ control method of nano-cerium oxide form and crystal face Download PDFInfo
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- CN106904649A CN106904649A CN201710133479.XA CN201710133479A CN106904649A CN 106904649 A CN106904649 A CN 106904649A CN 201710133479 A CN201710133479 A CN 201710133479A CN 106904649 A CN106904649 A CN 106904649A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/20—Compounds containing only rare earth metals as the metal element
- C01F17/206—Compounds containing only rare earth metals as the metal element oxide or hydroxide being the only anion
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B1/00—Single-crystal growth directly from the solid state
- C30B1/02—Single-crystal growth directly from the solid state by thermal treatment, e.g. strain annealing
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/16—Oxides
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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
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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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
Abstract
The in-situ control method of a kind of nano-cerium oxide form and crystal face, belongs to rare earth nano material technical field.With organic alcohols as dispersant, nano-form is disperseed and is sheared with reference to cavitation effect.It is cerium source precipitating reagent with alkaline matter, by the viscosity and surface tension that adjust dispersant, control the size and its coherent condition in reaction system of nano-form, make cerium precursor in nano-form adsorption and preferred orientation growth, the speed of growth of final regulation and control cerium oxide each crystal face, realizes the regulation and control to nano-scale range internal oxidition cerium form and crystal face.Preparation process is simple of the present invention, reaction condition is gentle, and reaction raw materials are easy to get, due to not adding any surfactant, and add nano-form is through calcined oxide noresidue and consumes part oxygen, its oxygen vacancy concentration can be increased while obtaining pure cerium oxide, application prospect is extensive.
Description
Technical field
It is specifically a kind of to pass through solvent thermal reaction the present invention relates to a kind of preparation method of rare earth nano material technical field
With reference to nano-form in-situ control nano-cerium oxide form and the method for crystal face.
Background technology
Nanostructured cerium oxide has unique redox active and superior storage put oxygen performance, makes its extensive use
In the associated catalytic technical field such as purifying vehicle exhaust, organic wastewater degraded, polishing material and methane and CO 2 reformation.Receive
The factors such as the redox ability and its microstructure, crystal active face, dispersiveness, purity of rice cerium oxide have close ties.Tool
The cerium oxide for having different geometric shapes generally exposes different crystal active faces（Such as（111）、（110）Or（100））, it is catalyzed it
Performance has significantly different.Therefore the regulation and control to nano-cerium oxide form and crystal face are particularly important.
To existing document retrieve find, prepare the main method of nano-cerium oxide have electrochemical deposition method, chemical precipitation method,
Microemulsion method, sol-gal process and the hot method of hydrothermal/solvent etc..W. Shen etc. exists《Chinese Journal of
Catalysis》（Catalysis journal Chinese edition）The 5th phase page 838 to 850 of volume 34 in 2013 delivers《Tuning the shape
of ceria nanomaterials for catalytic applications》（Cerium oxide nano materials pattern regulation and
Catalytic applications）, review influence and its application field of the regulation and control method of nano-cerium oxide shape size to its active crystal face.T.
Taniguchi etc. exists《Advanced Powder Technology》（Advanced powder technology）The 1st phase 64 of volume 27 in 2016
Delivered to page 71《Facet control of ceria nanocrystals synthesized by an oleate-
modified hydrothermal method》（Oleate regulation hydro-thermal method prepares the controllable cerium oxide nanocrystal of crystal face）.D.
Zhang etc. exists《Materials Letters》（Material journal）The 23rd phase of volume 62 in 2008：Page 3821 to 3823 are delivered
《Solvothermal synthesis of necklace-like carbon nanotube/ceria composites》（Water
Hot method synthesis item chain CNT/cerium oxide compound）, made as template, dimethylformamide and ethanol using CNT
It is secondary solvent, the cerium oxide of the nm of size about 100 is prepared for using hydro-thermal method.This three articles to nano-cerium oxide form with
Relation is studied and summarized between crystal active face and catalysis activity, it is indicated that regulation and control ceria nanoparticles form with
The prefered method for exposing crystal face type is the hot method of hydrothermal/solvent, while by surfactant or the booster action of template.But
Because the form of hydrothermal/solvent method regulation and control nano-cerium oxide often uses poisonous or expensive additive, surfactant, and
Need the treatment of HTHP and long period, it is impossible to meet the green environment friendly current demand for preparing nano material；Separately
On the one hand the new functional group introduced during prepared by the method is difficult to be completely removed, and the performance to nano-cerium oxide is interfered,
Limit the practical application area of nano-cerium oxide.
The content of the invention
The purpose of the present invention is directed to defect described above, there is provided the in-situ control of a kind of nano-cerium oxide form and crystal face
Method, the form and crystal face of nano-cerium oxide are adjusted using the CNT of dispersing shear, Graphene etc. as nano-form.
The purpose of the present invention is achieved by the following technical programs.
The in-situ control method of a kind of nano-cerium oxide form and crystal face, comprises the following steps successively：
Step one, using ultrasonic wave by 1-20 mg nano-forms（CNT or Graphene）Be scattered in 50-150 mL methyl alcohol,
In ethanol or ethylene glycol, the nano-form of dispersing shear is obtained after 8-12 h；Using a small amount of deionized water by cerous nitrate or chlorination
Cerium is completely dissolved, and obtains concentration for 1-10 mol L-1Cerium source solution；
Step 2, the nano-form in step one is added in the solution of cerium source, and to injecting alkaline precipitating agent in the system（Ammonia
Water, NaOH, urea）, regulation system pH value（8-11）；It is placed in ptfe autoclave that to carry out solvent heat anti-afterwards
Should, 120-200 DEG C of reaction temperature, reaction time 5-48 h carries out vacuum freeze drying, drying temperature-40-- 60 afterwards
DEG C, drying time 15-24 h, vacuum pressure 40-55 Pa obtain being deposited on the cerium precursor on nano-form；
Step 3, by the cerium precursor in step 2 be placed in air or oxygen atmosphere be heat-treated, programming rate be 10 DEG C/
Min, 400-600 DEG C of heat treatment temperature, heat treatment time 1-3 h are cooled to normal temperature, obtain final product form and controllable pure of crystal face
Nano-cerium oxide.
The present invention with organic alcohols as dispersant, using cavitation effect to nano-form（CNT or Graphene）Carry out
Dispersion is with shearing and as form and crystal face conditioning agent.It is cerium source precipitating reagent with alkaline matter, by the viscosity for adjusting dispersant
And surface tension, the size and its coherent condition in reaction system of nano-form are controlled, make cerium precursor in nano-form
Adsorption and preferred orientation growth, the speed of growth of final regulation and control cerium oxide each crystal face, realize in nano-scale range
The regulation and control of cerium oxide form and crystal face.In solid liquid interface（The interface of nano-form and system solution）Place is conducive to cerium precursor
Forming core, and because nano-form has reduced size and large specific surface area, be conducive to supporting cerium precursor.Ethylene glycol viscosity compared with
It is big and specific surface energy is relatively low, CNT can be made to restrain fluffy dispersion, can effectively adsorb cerium precursor, to its crystal it is each to
Anisotropic growth plays a decisive role.Additionally, methyl alcohol, ethanol and ethylene glycol are all because having hydrophily containing hydroxyl, can be with water
It is miscible, so oil/water microreactor can be constituted with a small amount of water, also there is the regulation cerium precursor direction of growth in reaction system
Effect.The boiling point of methyl alcohol and ethanol is below water, can effectively alleviate the hard aggregation degree of powder, the form of product is controlled
System.
The present invention, as morphology modifying agent, can realize that regulation preparation in situ has difference using nano-form using solvent heat
The nano-cerium oxide of form and crystal face.At present, the method main method that regulation and control prepare nano-cerium oxide form and crystal face be hydro-thermal/
Solvent-thermal method, and the method introduces new functional group mainly using surfactant as adjuvant, have impact on cerium oxide performance
Give full play to.Boiling point of the one aspect of the present invention by using methyl alcohol, ethanol or ethylene glycol during solvent heat, viscosity and Bi Biao
The characteristics such as face energy, the nucleation and growth speed to cerium precursor crystal face is intervened；On the other hand by using nano-form pair
Cerium precursor provide nuclearing centre, to cerium precursor nano-form surface or around anisotropic growth carry out microcosmic tune
Control, afterwards, be passed through oxidizing atmosphere in high temperature reaction zone carries out oxidation removal to nano-form, has obtained form（It is tetragonal body, vertical
Cube, hexagon etc.）With oikocryst face（（111）、（100））Controllable nano-cerium oxide, because the removal of nano-form is consumed
Part oxygen, increased the oxygen vacancy concentration of cerium oxide, be conducive to improving its storage/release oxygen ability.
The present invention has the advantages that：The present invention is controlled by adjusting nano-form distribution in organic alcohols
The anisotropic growth direction of cerium precursor processed, reaches the purpose of regulation nano-cerium oxide form and crystal face.It is pure in order to obtain
Nano-cerium oxide and improve its oxygen vacancy concentration, oxidizing atmosphere can be passed through nano-form is aoxidized.Present invention process
Simple and easy to apply, raw materials used to be easy to get, reaction is gentle, and preparation technology is succinct, can be as desired by regulation nano-form, dispersant
With the factor such as alkaline precipitating agent, regulation and control prepare different shape（Tetragonal body, cube, hexagon etc.）With oikocryst face（（111）With
（100））Nano-cerium oxide.
Brief description of the drawings
Fig. 1 be figure in (a) embodiment 1, figure (b) embodiment 2, figure (c) embodiment 3 and figure (d) embodiment 4 make
Standby different shape and the transmission electron microscope photo of crystal face nano-cerium oxide.
Specific embodiment
The present embodiment be premised on inventive technique scheme under implemented, give detailed implementation method and process,
But protection scope of the present invention is not limited to following embodiments.
Embodiment 1.
5 mg CNTs are scattered in 100 mL ethylene glycol using ultrasonic wave, the carbon that dispersing shear is obtained after 15 h is received
Mitron；Other compound concentration is the cerium solution of 0. 5 mol/L；The CNT of dispersing shear is added to cerium solution
In, while it is 9 that alkaline precipitating agent regulation system pH value is added dropwise；Above-mentioned mixed solution immigration ptfe autoclave is carried out molten
Agent thermal response, 160 DEG C of reaction temperature, the h of reaction time 12 carries out vacuum freeze drying after cooling, -45 DEG C of drying temperature is done
The h of dry time 15, the Pa of vacuum pressure 40, obtain CNT/cerium precursor compound；CNT/cerium precursor is combined
Thing is placed in magnetic boat, is pushed into corundum reaction tube center in horizontal pipe stove, is passed through oxygen and is heat-treated therewith, and heat up speed
It is 5 DEG C/min to spend, 600 DEG C of heat treatment temperature, and the h of heat treatment time 0.5 is cooled to normal temperature, obtains form in square and master
Crystal face is（100）Pure nano-cerium oxide.
Embodiment 2.
10 mg CNTs are scattered in 150 mL ethanol using ultrasonic wave, the carbon that dispersing shear is obtained after 15 h is received
Mitron；Other compound concentration is the cerium solution of 0.1 mol/L；The CNT of dispersing shear is added in cerium solution,
The pH value that alkaline precipitating agent regulation system is added dropwise simultaneously is 9.5；Above-mentioned mixed solution immigration ptfe autoclave is carried out
Solvent thermal reaction, 160 DEG C of reaction temperature, the h of reaction time 24 carries out vacuum freeze drying after cooling, -50 DEG C of drying temperature,
The h of drying time 20, the Pa of vacuum pressure 45, obtain CNT/cerium precursor compound；CNT/cerium precursor is multiple
Compound is placed in magnetic boat, is pushed into corundum reaction tube center in horizontal pipe stove, is passed through oxygen and is heat-treated therewith, is heated up
Speed is 5 DEG C/min, and 600 DEG C of heat treatment temperature, the h of heat treatment time 1 is cooled to normal temperature, obtains form in cube and master
Crystal face is（100）Pure nano-cerium oxide.
Embodiment 3.
Using ultrasonic wave by 5 mg graphene dispersions in 100 mL ethylene glycol, finely dispersed Graphene is obtained after 12 h
Glycolic suspension；Other compound concentration is the cerium solution of 0.5 mol/L；Graphene glycolic suspension is added to cerium
In salting liquid, while the pH value that alkaline precipitating agent regulation system is added dropwise is 10；Above-mentioned mixed solution is moved into polytetrafluoroethylene (PTFE) anti-
Answering kettle carries out solvent thermal reaction, and 180 DEG C of reaction temperature, the h of reaction time 24 carries out vacuum freeze drying, dries temperature after cooling
- 55 DEG C of degree, the h of drying time 25, the Pa of vacuum pressure 50 obtain Graphene/cerium precursor compound；Before CNT/cerium
Drive nanocrystal composition to be placed in magnetic boat, be pushed into corundum reaction tube center in horizontal pipe stove, be passed through air and carry out hot place therewith
Reason, programming rate is 10 DEG C/min, and 600 DEG C of heat treatment temperature, the h of heat treatment time 0.5 is cooled to normal temperature, and obtaining form is in
Hexahedron and oikocryst face are（111）Pure nano-cerium oxide.
Embodiment 4.
Using ultrasonic wave by 15 mg graphene dispersions in 150 mL ethanol, finely dispersed Graphene is obtained after 12 h
Alcohol suspension；Other compound concentration is the cerium solution of 0.5 mol/L；Graphene alcohol suspension is added to cerium salt molten
In liquid, while the pH value that alkaline precipitating agent regulation system is added dropwise is 11；Above-mentioned mixed solution is moved into ptfe autoclave
Solvent thermal reaction is carried out, 180 DEG C of reaction temperature, the h of reaction time 12 carries out vacuum freeze drying, drying temperature -55 after cooling
DEG C, the h of drying time 20, the Pa of vacuum pressure 55 obtain Graphene/cerium precursor compound；CNT/cerium precursor is multiple
Compound is placed in magnetic boat, is pushed into corundum reaction tube center in horizontal pipe stove, is passed through air and is heat-treated therewith, is heated up
Speed is 10 DEG C/min, and 600 DEG C of heat treatment temperature, the h of heat treatment time 2 is cooled to normal temperature, obtain form in hexahedron and
Oikocryst face is（111）Pure nano-cerium oxide.
Claims (4)
1. the in-situ control method of a kind of nano-cerium oxide form and crystal face, it is characterised in that：Comprise the following steps successively：
, be scattered in 1-20 mg nano-forms in 50-150 mL methyl alcohol, ethanol or ethylene glycol using ultrasonic wave, 8-12 by step one
The nano-form of dispersing shear is obtained after h；Cerous nitrate or cerium chloride are completely dissolved using a small amount of deionized water, obtaining concentration is
1-10 mol L-1Cerium source solution；
Step 2, the nano-form in step one is added in the solution of cerium source, and to alkaline precipitating agent is injected in the system, is adjusted
Section system pH（8-11）；Being placed in afterwards carries out solvent thermal reaction in ptfe autoclave, 120-200 DEG C of reaction temperature,
Reaction time 5-48 h, carries out vacuum freeze drying, drying temperature-40-- 60 DEG C, drying time 15-24 h, vacuum afterwards
Pressure 40-55 Pa, obtain being deposited on the cerium precursor on nano-form；
Step 3, by the cerium precursor in step 2 be placed in air or oxygen atmosphere be heat-treated, programming rate be 10 DEG C/
Min, 400-600 DEG C of heat treatment temperature, heat treatment time 1-3 h are cooled to normal temperature, obtain final product form and controllable pure of crystal face
Nano-cerium oxide.
2. the in-situ control method of a kind of nano-cerium oxide form according to claim 1 and crystal face, it is characterised in that：Step
Nano-form described in rapid one is CNT or Graphene.
3. the in-situ control method of a kind of nano-cerium oxide form according to claim 1 and crystal face, it is characterised in that：Step
Alkaline precipitating agent described in rapid two is the one kind in ammoniacal liquor, NaOH or urea.
4. the in-situ control method of a kind of nano-cerium oxide form according to claim 1 and crystal face, it is characterised in that：Step
Regulation system pH value described in rapid two is 8-11.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108767280A (en) * | 2018-06-22 | 2018-11-06 | 西安交通大学 | A kind of Pt nano particles/hydroxyl carbon cerium mine nano-cluster/graphene composite material and preparation method thereof |
| CN108786786A (en) * | 2018-07-17 | 2018-11-13 | 河南科技大学 | A kind of photocatalytic degradation nanometer MoO3The preparation method of powder |
| CN109082329A (en) * | 2018-07-23 | 2018-12-25 | 江苏大学 | A kind of ternary nano self-lubricating composite and preparation method thereof |
| CN109589956A (en) * | 2018-12-26 | 2019-04-09 | 江苏大学 | A kind of preparation method and its usage rich in defect metal oxide |
| CN112939052A (en) * | 2021-03-22 | 2021-06-11 | 北方稀土生一伦高科技有限公司 | Preparation method of small-particle-size cerium oxide |
| CN113104880A (en) * | 2021-05-07 | 2021-07-13 | 江西理工大学 | Yttrium oxide microsphere composed of nano rod-shaped structure and preparation method thereof |
| CN114477264A (en) * | 2022-03-03 | 2022-05-13 | 赣州湛海新材料科技有限公司 | Method for preparing nano cerium oxide by sol-gel method |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108767280A (en) * | 2018-06-22 | 2018-11-06 | 西安交通大学 | A kind of Pt nano particles/hydroxyl carbon cerium mine nano-cluster/graphene composite material and preparation method thereof |
| CN108767280B (en) * | 2018-06-22 | 2020-10-27 | 西安交通大学 | Pt nanoparticle/hydroxyl cerite nanocluster/graphene composite material and preparation method thereof |
| CN108786786A (en) * | 2018-07-17 | 2018-11-13 | 河南科技大学 | A kind of photocatalytic degradation nanometer MoO3The preparation method of powder |
| CN108786786B (en) * | 2018-07-17 | 2021-01-01 | 河南科技大学 | Nano MoO for photocatalytic degradation3Method for preparing powder |
| CN109082329A (en) * | 2018-07-23 | 2018-12-25 | 江苏大学 | A kind of ternary nano self-lubricating composite and preparation method thereof |
| CN109082329B (en) * | 2018-07-23 | 2021-04-20 | 江苏大学 | Ternary nano self-lubricating composite material and preparation method thereof |
| CN109589956A (en) * | 2018-12-26 | 2019-04-09 | 江苏大学 | A kind of preparation method and its usage rich in defect metal oxide |
| CN112939052A (en) * | 2021-03-22 | 2021-06-11 | 北方稀土生一伦高科技有限公司 | Preparation method of small-particle-size cerium oxide |
| CN113104880A (en) * | 2021-05-07 | 2021-07-13 | 江西理工大学 | Yttrium oxide microsphere composed of nano rod-shaped structure and preparation method thereof |
| CN114477264A (en) * | 2022-03-03 | 2022-05-13 | 赣州湛海新材料科技有限公司 | Method for preparing nano cerium oxide by sol-gel method |
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