CN107827141B - Nano ceric oxide and preparation method thereof - Google Patents
Nano ceric oxide and preparation method thereof Download PDFInfo
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- CN107827141B CN107827141B CN201711070720.5A CN201711070720A CN107827141B CN 107827141 B CN107827141 B CN 107827141B CN 201711070720 A CN201711070720 A CN 201711070720A CN 107827141 B CN107827141 B CN 107827141B
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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
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
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- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
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- 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 present invention provides a kind of nano ceric oxide and preparation method thereof, and the preparation method at least includes the following steps: the first silane coupler solution being added in cerous nitrate, solution A is obtained；The second silane coupling agent is added into cerous nitrate solution, obtains the solution B with precipitating；Solution A and solution B are mixed, reaction obtains product under enclosed system.Method of the present invention is simple, one-step synthesis, without annealing.
Description
Technical field
The present invention relates to a kind of nano ceric oxides and preparation method thereof.
Background technique
The performance of nano material improves a lot with its massive phase ratio, and the nano material of ultra-small grain size often has many
New physics and chemical property, therefore, the nano material for preparing ultra-small grain size have become the research hotspot of nm regime in recent years
One of.Wherein, nano ceric oxide is because possessing more Lacking oxygen and higher specific surface area, in auto-emission control, sewage
The fields such as processing, electrode material and chemically mechanical polishing are all widely used.
Currently, hydro-thermal method is to prepare one of main method of nano ceric oxide.It is compared with other methods, hydro-thermal method preparation
Nano particle have good crystallinity, pattern is uniform, the manageable advantage of partial size.It can be prepared by the condition for changing different
The nano ceric oxide of different-grain diameter.Patent CN 201610260014.6 discloses a kind of preparation method of spherical ceria,
Hydro-thermal reaction is carried out by raw material of cerium salt, polyvinylpyrrolidone and short chain organic acid, it is 50- that average grain diameter is obtained after calcining
The cerium oxide particles of 300nm；Patent CN 201610536090.5 discloses a kind of system of small particle ceria nano-crystalline
Preparation Method, using cerous nitrate as source substance, polyethylene glycol 200 is solvent and dispersing agent, and zinc hydroxide is the second progress hydro-thermal reaction,
The cerium oxide particles that average grain diameter is 5-8nm are obtained after calcining.Patent CN201510183012.7 discloses a kind of nanometer two
Cerium oxide catalyst preparation method, using cerous nitrate as source substance, cetyl trimethylammonium bromide is surface first, ammonium hydroxide the
Two carry out hydro-thermal reaction, and the ceria catalyst that average grain diameter is 20-30nm is obtained after calcining.
But the above-mentioned technical method for preparing ceria is two-step synthesis method, i.e., the first step reaction preparation powder need through
Pure cerium oxide nanoparticles can just be obtained by spending high-temperature calcination 2-5 hours.This makes the preparation process period long, and energy consumption is high, institute
Product it is easy to reunite, particle size is far longer than 10nm, it is difficult to meet materials science field to the need of ultra-small grain size nano material
It asks.
Summary of the invention
In view of the foregoing deficiencies of prior art, the purpose of the present invention is to provide a kind of nano ceric oxide and its systems
Preparation Method, for solving the problems, such as that preparation method of nanometer cerium dioxide is complex in the prior art.
In order to achieve the above objects and other related objects, the present invention provides a kind of preparation method of nano ceric oxide, institute
Preparation method is stated at least include the following steps:
(1) the first silane coupler solution is added in cerous nitrate, obtains solution A；Second is added into cerous nitrate solution
Silane coupling agent obtains the solution B with precipitating；
(2) solution A and solution B are mixed, reaction obtains product under enclosed system.
Silane coupling agent be it is a kind of contain simultaneously in the molecule there are two types of different chemical property groups organo-silicon compound,
Classical product can use general formula YSiX3It indicates.In formula, Y is non-hydrolytic group, including alkenyl (predominantly vinyl), Yi Jimo
End has Cl, NH2, SH, epoxy, N3, (methyl) acryloxy, the functional groups such as isocyanate group alkyl, i.e. carbon functional group；X
For hydrolyzable groups, including Cl, OMe, OEt, OC2H4OCH3,OSiMe3, and OAc etc..
Preferably, silane coupling agent is gamma-aminopropyl-triethoxy-silane in the step (1).That is KH550, molecular formula
For (C2H5O)3Si(CH2)3NH2。
Preferably, first silane coupling agent and the second silane coupling agent use identical substance.
Preferably, the quality of the silane coupling agent in the first silane coupler solution in the step (1) and cerous nitrate
Than are as follows: 0.2~2:1；The mass ratio of cerous nitrate in second silane coupling agent and cerous nitrate solution are as follows: 0.2~2:1.
Preferably, the quality of the silane coupling agent in the first silane coupler solution in the step (1) and cerous nitrate
Than are as follows: 0.5:1；The mass ratio of cerous nitrate in second silane coupling agent and cerous nitrate solution are as follows: 0.5:1.
Preferably, silane coupling agent concentration is 0.022~0.22mol/L in first silane coupler solution；It is more excellent
It is selected as 0.11 mol/L.
Preferably, the reaction kettle is hydrothermal reaction kettle.
Preferably, the reaction kettle is stainless steel hydrothermal reaction kettle.
Preferably, reaction temperature is 100~160 DEG C in the step (2), and the reaction time is 12~48 hours.
Preferably, the preparation method further include: (3) by product washing, dry, grinding.
It is highly preferred that the washing is first washed with water 1~3 time, then with ethanol washing 1~3 time.
It is highly preferred that the drying temperature is 30~60 DEG C, drying time 3~18 hours.
It is highly preferred that described dry using vacuum drying.
Another aspect of the present invention provides the nano ceric oxide of above method preparation.
Further, the nano ceric oxide partial size is 3~10nm.
Further, the nano ceric oxide pattern is spherical shape.
As described above, the preparation method of nano ceric oxide of the invention, has the advantages that
1. in preparation method of the invention, using cerous nitrate as raw material, single step reaction can obtain the nano-silica of ultra-small grain size
Change cerium particle, nanosphere 3~10nm of partial size is cubic fluorite structure.
2. the method for the present invention simple process, without annealing, reunion when avoiding high-temperature calcination between nano particle,
Obtained cerium oxide nanoparticles good dispersion.
3. the present invention can not only be prevented between particle using KH550 (gamma-aminopropyl-triethoxy-silane) as first
Reunion, moreover it is possible to regulate and control pattern, obtained nano ceric oxide be spherical shape.
4. the present invention, as second, slowly releases OH under hydrothermal temperature using KH550—, reaction condition is mild, brilliant
Rate of nucleus growing is certain, and obtained cerium dioxide nano ball size is uniform.
5. cerium dioxide nano ball field involved by it that the present invention obtains has a good application prospect.
Detailed description of the invention
Fig. 1 is the XRD diagram of cerium dioxide nano ball made from the embodiment of the present invention 1.
Fig. 2 is the TEM figure of cerium dioxide nano ball made from the embodiment of the present invention 1.
Fig. 3 is the TEM figure of cerium dioxide nano ball made from the embodiment of the present invention 2.
Fig. 4 is the HR-TEM figure of cerium dioxide nano ball made from the embodiment of the present invention 2.
Fig. 5 is the TEM figure of cerium dioxide nano ball prepared by the embodiment of the present invention 3.
Fig. 6 is the electron diffraction pattern figure of cerium dioxide nano ball prepared by the embodiment of the present invention 3.
Fig. 7 is the TEM figure of cerium dioxide nano ball prepared by the embodiment of the present invention 4.
Fig. 8 is the TEM figure of cerium dioxide nano ball prepared by the embodiment of the present invention 5.
Specific embodiment
Embodiments of the present invention are illustrated by particular specific embodiment below, those skilled in the art can be by this explanation
Content disclosed by book is understood other advantages and efficacy of the present invention easily.
It should be clear that in the following example not specifically dated process equipment or device be all made of conventional equipment in the art or
Device.
In addition, it should also be understood that, one or more method and step mentioned in the present invention does not repel before and after the combination step
It can also be inserted into other methods step there may also be other methods step or between these explicitly mentioned steps, unless separately
It is described；It should also be understood that the combination connection relationship between one or more equipment/device mentioned in the present invention is not repelled
The two equipment/devices specifically mentioned before and after the unit equipment/device there may also be other equipment/device or at these it
Between can also be inserted into other equipment/device, unless otherwise indicated.Moreover, unless otherwise indicated, the number of various method steps is only
Identify the convenient tool of various method steps, rather than for the arrangement order of limitation various method steps or limits the enforceable model of the present invention
It encloses, relativeness is altered or modified, and without material changes in technical content, when being also considered as, the present invention is enforceable
Scope.
Embodiment 1
(1) 2.21g KH550 is dissolved in 45mL distilled water, and 4.34g cerous nitrate is added under agitation until complete
Portion's dissolution, obtains solution A.4.24g cerous nitrate is dissolved in 45ml distilled water again, 2.21g KH550 is added, obtaining has precipitating
Solution B.
(2) above-mentioned solution A and solution B are gone into 60mL capacity with close in the stainless steel hydrothermal reaction kettle of Teflon liner
Envelope, is placed in baking oven, is warming up to 140 DEG C, hydro-thermal reaction 24 hours.
(3) reaction terminates, after being cooled to room temperature, by obtained faint yellow solid precipitating distilled water centrifuge washing three
Secondary, twice, last 45 DEG C are dried in vacuo 8 hours ethanol washing, and grinding obtains the ball shaped nano ceria of ultra-small grain size
Grain.
Fig. 1 is the XRD spectra for the cerium oxide nanoparticles that the implementation case is prepared, the corresponding crystal face of diffraction maximum
For (111), (200), (220), (311), (222), (400), (331) and (420) are typical cubic fluorite structure.
Fig. 2 is the TEM figure for the cerium oxide nanoparticles that the implementation case is prepared, it can be seen from the figure that this is received
Rice grain favorable dispersibility, pattern are spherical shape, 3~10nm of partial size.
As a result, Electronic Speculum observation, nanosphere 3~10nm of partial size is cubic fluorite structure such as Fig. 1 and 2.
Embodiment 2
(1) 1.10g KH550 is dissolved in 45mL distilled water, and 2.17g cerous nitrate is added under agitation until complete
Portion's dissolution.4.24g cerous nitrate is dissolved in 45ml distilled water again, 2.21g KH550 is added, obtains the solution B with precipitating.
(2) above-mentioned solution A and solution B are gone into 60mL capacity with close in the stainless steel hydrothermal reaction kettle of Teflon liner
Envelope, is placed in baking oven, is warming up to 100 DEG C, hydro-thermal reaction 48 hours.
(3) reaction terminates, after being cooled to room temperature, by obtained faint yellow solid precipitating distilled water centrifuge washing three
Secondary, twice, last 30 DEG C are dried in vacuo 18 hours ethanol washing, and grinding obtains the ball shaped nano ceria of ultra-small grain size
Grain.
Fig. 3 is the TEM figure for the cerium oxide nanoparticles that the implementation case is prepared, 3~10nm of nanosphere partial size.
Fig. 4 is the HR-TEM figure for the cerium oxide nanoparticles that the implementation case is prepared, it can be seen that prepared
Cerium dioxide nano ball lattice constant be 0.27nm, it is corresponding with (200) face of cubic fluorite structure ceria.
It as a result is cubic fluorite structure such as Fig. 3 and 4, nanosphere 3~10nm of partial size.
Embodiment 3
(1) 1.10g KH550 is dissolved in 45mL distilled water, and 4.34g cerous nitrate is added under agitation until complete
Portion's dissolution.4.24g cerous nitrate is dissolved in 45ml distilled water again, 2.21g KH550 is added, obtains the solution B with precipitating.
(2) above-mentioned solution A and solution B are gone into 60mL capacity with close in the stainless steel hydrothermal reaction kettle of Teflon liner
Envelope, is placed in baking oven, is warming up to 140 DEG C, hydro-thermal reaction 12 hours.
(3) reaction terminates, after being cooled to room temperature, by obtained faint yellow solid precipitating distilled water centrifuge washing three
Secondary, twice, last 50 DEG C are dried in vacuo 5 hours ethanol washing, and grinding obtains the ball shaped nano ceria of ultra-small grain size
Grain.
Fig. 5 is the TEM figure for the cerium oxide nanoparticles that the implementation case is prepared, and nanosphere 3~10nm of partial size is
Cubic fluorite structure.
Fig. 6 is the electron diffraction pattern figure of cerium oxide nanoparticles that the implementation case is prepared, can be with from figure
Find out, prepared cerium oxide nanoparticles are monocrystalline.
As a result such as Figures 5 and 6, nanosphere 3~10nm of partial size is cubic fluorite structure.
Embodiment 4
(1) 0.22g KH550 is dissolved in 45mL distilled water, and 1.10g cerous nitrate is added under agitation until complete
Portion's dissolution.4.24g cerous nitrate is dissolved in 45ml distilled water again, 2.21g KH550 is added, obtains the solution B with precipitating.
(2) above-mentioned solution A and solution B are gone into 60mL capacity with close in the stainless steel hydrothermal reaction kettle of Teflon liner
Envelope, is placed in baking oven, is warming up to 120 DEG C, hydro-thermal reaction 12 hours.
(3) reaction terminates, after being cooled to room temperature, by obtained faint yellow solid precipitating distilled water centrifuge washing three
Secondary, twice, last 50 DEG C are dried in vacuo 5 hours ethanol washing, and grinding obtains the ball shaped nano ceria of ultra-small grain size
Grain.
Fig. 7 is the TEM figure for the cerium oxide nanoparticles that the implementation case is prepared, and nanosphere 3~10nm of partial size is
Cubic fluorite structure.
Embodiment 5
(1) 2.21g KH550 is dissolved in 45mL distilled water, and 1.10g cerous nitrate is added under agitation until complete
Portion's dissolution.4.24g cerous nitrate is dissolved in 45ml distilled water again, 2.21g KH550 is added, obtains the solution B with precipitating.
(2) above-mentioned solution A and solution B are gone into 60mL capacity with close in the stainless steel hydrothermal reaction kettle of Teflon liner
Envelope, is placed in baking oven, is warming up to 160 DEG C, hydro-thermal reaction 12 hours.
(3) reaction terminates, after being cooled to room temperature, by obtained faint yellow solid precipitating distilled water centrifuge washing three
Secondary, twice, last 60 DEG C are dried in vacuo 3 hours ethanol washing, and grinding obtains the ball shaped nano ceria of ultra-small grain size
Grain.
Fig. 8 is the TEM figure for the cerium oxide nanoparticles that the implementation case is prepared, and nanosphere 3~10nm of partial size is
Cubic fluorite structure.
So the present invention effectively overcomes various shortcoming in the prior art and has high industrial utilization value.
The above-described embodiments merely illustrate the principles and effects of the present invention, and is not intended to limit the present invention.It is any ripe
The personage for knowing this technology all without departing from the spirit and scope of the present invention, carries out modifications and changes to above-described embodiment.Cause
This, institute is complete without departing from the spirit and technical ideas disclosed in the present invention by those of ordinary skill in the art such as
At all equivalent modifications or change, should be covered by the claims of the present invention.
Claims (6)
1. a kind of preparation method of nano ceric oxide, which is characterized in that the preparation method includes at least:
(1) the first silane coupler solution is mixed with cerous nitrate, obtains solution A；Cerous nitrate solution is silane coupled with second
Agent obtains the solution B with precipitating；
(2) solution A and solution B are mixed, reaction obtains product under enclosed system；
First silane coupling agent and the second silane coupling agent use identical substance, silane coupling agent in the step (1)
For gamma-aminopropyl-triethoxy-silane；
The mass ratio of the silane coupling agent and cerous nitrate in the first silane coupler solution in the step (1) are as follows: 0.2~2:
1；
The mass ratio of cerous nitrate in second silane coupling agent and cerous nitrate solution are as follows: 0.2~2:1；
Reaction temperature is 100~160 DEG C in the step (2), and the reaction time is 12~48 hours.
2. the preparation method of nano ceric oxide according to claim 1, it is characterised in that: in the step (1)
The mass ratio of silane coupling agent and cerous nitrate in one silane coupler solution are as follows: 0.5:1；Second silane coupling agent and nitre
The mass ratio of cerous nitrate in sour cerium solution are as follows: 0.5:1.
3. the preparation method of nano ceric oxide according to claim 1, it is characterised in that: first silane coupling agent
Silane coupling agent concentration is 0.022~0.22mol/L in solution.
4. the preparation method of nano ceric oxide according to claim 3, it is characterised in that: first silane coupling agent
Silane coupling agent concentration is 0.11mol/L in solution.
5. the preparation method of nano ceric oxide according to claim 1, it is characterised in that: the preparation method is also wrapped
It includes:
(3) by product washing, dry, grinding.
6. the preparation method of nano ceric oxide according to claim 1, it is characterised in that: the drying temperature be 30~
60 DEG C, drying time 3~18 hours.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101659850A (en) * | 2009-09-22 | 2010-03-03 | 中国科学院上海微系统与信息技术研究所 | Modified nanometer cerium oxide and preparation and application thereof |
| CN101734706A (en) * | 2009-12-25 | 2010-06-16 | 中国科学院上海微系统与信息技术研究所 | Method for preparing diamond platy cerium oxide |
| CN103896321A (en) * | 2012-12-28 | 2014-07-02 | 上海新安纳电子科技有限公司 | Cerium oxide composite particles, as well as preparation method and application thereof |
| CN106277020A (en) * | 2015-06-12 | 2017-01-04 | 常州卓煜新材料科技有限公司 | A kind of bigger serface micron cerium oxide preparation method |
| CN107827141A (en) * | 2017-11-03 | 2018-03-23 | 上海映智研磨材料有限公司 | Nano ceric oxide and preparation method thereof |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101659850A (en) * | 2009-09-22 | 2010-03-03 | 中国科学院上海微系统与信息技术研究所 | Modified nanometer cerium oxide and preparation and application thereof |
| CN101734706A (en) * | 2009-12-25 | 2010-06-16 | 中国科学院上海微系统与信息技术研究所 | Method for preparing diamond platy cerium oxide |
| CN103896321A (en) * | 2012-12-28 | 2014-07-02 | 上海新安纳电子科技有限公司 | Cerium oxide composite particles, as well as preparation method and application thereof |
| CN106277020A (en) * | 2015-06-12 | 2017-01-04 | 常州卓煜新材料科技有限公司 | A kind of bigger serface micron cerium oxide preparation method |
| CN107827141A (en) * | 2017-11-03 | 2018-03-23 | 上海映智研磨材料有限公司 | Nano ceric oxide and preparation method thereof |
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