CN110203969A - A kind of high dispersive cubic phase nano zirconium oxide and preparation method thereof - Google Patents
A kind of high dispersive cubic phase nano zirconium oxide and preparation method thereof Download PDFInfo
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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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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
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- 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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- C01P2004/30—Particle morphology extending in three dimensions
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- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
The invention discloses a kind of high dispersive cubic phase nano zirconium oxides and preparation method thereof, comprising: zirconates and yttrium salt are dissolved in deionized water, prepare certain density solution, composite dispersing agent is added, obtains mixed solution；Ammonium hydroxide is added dropwise into the mixed solution being stirred continuously at room temperature, until solution PH is 9, is stirred continuously until to obtain the uniform precursor solution of chemical constituent；Presoma is washed, is filtered, until filtrate can't detect Cl‑Until ion；The presoma washed is added in triethanolamine solution, after mixing evenly, is transferred in reaction kettle, microwave hydrothermal reacts 10-90min at 160-260 DEG C；The powder generated after reaction is washed, is dried, prepares particle diameter distribution in 20-40nm, the nanometer ZrO of good dispersion2Powder.The present invention substantially reduces ZrO by microwave hydrothermal technology and addition mineralizer triethanolamine2Powder generated time solves the problems, such as that nano-powder is reunited by adding composite dispersing agent.
Description
Technical field
The invention belongs to technical field of nanometer material preparation, and in particular to a kind of high dispersive cubic phase nano zirconium oxide and its
Preparation method.
Background technique
Zirconium oxide has very excellent physical and chemical properties, such as high-melting-point (2700 DEG C) and higher boiling, thermal coefficient
Well, wearability is good, corrosion resistance is excellent etc., preparation structure and functional material is therefore widely used in, especially as high property
The source of energy ceramic material.There are three types of crystalline structures under normal pressure for pure zirconia: monoclinic system (Monoclinic zirconia,
m-ZrO2), tetragonal crystal system (Tetragonal zirconia, t-ZrO2) and cubic system (Cubic zirconia, c-ZrO2),
These three crystal forms are present in different temperature ranges, and can mutually convert.With the reduction of Zirconium oxide powder partial size, many property
Can be more superior, therefore the emphasis that the preparation of nano zirconium oxide powder is always studied both at home and abroad.
The preparation method of common nano zircite has, high-temperature calcination, sol-gal process, the precipitation method and hydro-thermal method etc..
Compared with other preparation methods, the powder of hydro-thermal method preparation is due to good dispersion, and ingredient is uniform, crystal form, morphology controllable, dispersibility
The features such as good and production cost is low, is concerned in recent years.Microwave-hydrothermal method is a kind of special liquid-phase synthesis process, its handle
Traditional hydrothermal synthesis method combines with microwave field, carries out energy transmission to the dielectric effect of water using microwave, and heat
Process can generate the temperature gradient opposite with conventional heat transfer process since inside substance.Microwave-hydrothermal method synthesis powder compared with
Conventional hydrothermal method and chemically synthesized powder have particle diameter distribution narrow, good dispersion, reunite few, and crystal grain is complete and good crystallinity,
The advantages that not needing high-temperature calcination, synthesis rate and efficiency are more much higher than traditional hydro-thermal method.
Chinese patent 201410423869.7 provides the preparation method of a kind of nanometer of oxide-stabilizing zirconia powder, this method step
Suddenly include: that polybasic carboxylic acid complexing agent and polyol crosslink agent are added in the aqueous solution containing zirconates and stabilizer, pass through esterification
Reaction makes solution be converted into colloid, and slurry is made in colloid and dispersant, decomposes and makes through high-temp combustion after atomization drying
Obtain nanoscale oxide-stabilizing zirconia powder.The powder roasting process of this method preparation be easy to cause environmental pollution, and the powder after roasting
End be easy to cause reunion, and the dispersibility of powder is poor.
Chinese patent 201610882966.1 provides a kind of preparation method of nano zircite and its nano oxygen of preparation
Change zirconium, this method step includes: to be precipitated zirconium salt solution to form sediment presoma with aqueous slkali, is carried out in aqueous slkali
Reflux is washed finally to precipitating crystal form filtering, and dry, roasting obtains nano zircite specific surface area greater than 100cm2/g.It should
The shortcomings that method is that the reflux course time of aqueous slkali is longer, and working environment is poor, and production efficiency is lower, is unfavorable for industry
Metaplasia produces.
Chinese patent 201610323777.0 provides a kind of preparation method of Zirconium dioxide nano powder, this method step
Include: the certain density zirconyl chloride solution of configuration and be heated to 40~96 DEG C, 1~5h of holding, then the solution is flowed into and is spread
The feed liquid side compartment of dialysis film device, the hydrogen chloride in aqueous solution enter diffusion liquid side compartment, hydrogen-oxygen through anion-exchange membrane
Change zirconium and then stays in feed liquid side compartment formation soliquid, meanwhile, there is pure water to flow into diffusion liquid side compartment, zirconium hydroxide colloidal suspension
Supernatant liquid is zirconium hydroxide slurry by filter filtering, distillation device concentration, which is made titanium dioxide after being dehydrated, being dried
Up to 99.9% or more, partial size is 5~30nm and is evenly distributed zirconium nano-powder purity.It needs to use in this method production process
Special appliance arrangement, production capacity is small, and production cost is higher, is unfavorable for industrialization promotion.
Chinese patent 201710889175.6 provides a kind of nanometer of yttrium stable zirconium oxide raw powder's production technology, this method
Step includes: to mix zirconium oxychloride, yttrium oxide, deionized water according to certain mass ratio, is heated to 90~110 DEG C, heat preservation 1
~3h；Natural plant gum is added, then adds at least one of ethylenediamine tetra-acetic acid or citric acid, stirs 3-5h, generates glue
Liquid solution；Ammonia spirit is added to stir simultaneously, stirs 8-10h, until PH=10.0-11.0, generates white depositions, be then allowed to stand
Ageing 24~48 hours；Sediment is washed, is filtered, then spray-dried, air-flow crushing obtains presoma powder；450
5~7 hours are calcined at~600 DEG C to get nanometer yttrium stable zirconium oxide powder is arrived.The Zirconium powder of this method preparation, sintering
Shrinking percentage is high, and sintered density is high, intensity is good, and performance is good, and partial size is small, narrowly distributing.This method disadvantage technical process is complex,
It is extremely easy to produce reunion in subsequent drying and calcination treatment process, is unfavorable for industrialized production.
Above-mentioned patent elaborates various method production Zirconium dioxide nano powders, and production process is unavoidably required to lead to
High temperature calcine technology is crossed, technique is more complex, and subsequent process easily generates reunion.Therefore it is controllable to explore simple process, and subsequent place
The nano-powder preparation method that reason is not likely to produce reunion has very important significance.
Summary of the invention
The purpose of the present invention is to provide a kind of high dispersive cubic phase nano zirconium oxides and preparation method thereof, overcome current biography
System hydro-thermal method prepares deficiency present in nano zircite technique, to obtain the big nanometer of crystallinity height, good dispersion, specific surface
Zirconium powder.
The specific technical solution of the present invention is as follows: a kind of high dispersive cubic phase nano zirconium oxide and preparation method thereof.
(1) by zirconium oxychloride ZrOCl2·8H2Certain density zirconium ion (Zr is made in O dissolution in deionized water4+) solution is simultaneously
Stabilizer YCl is added3·6H2O and composite dispersing agent；
(2) ammonium hydroxide is added dropwise in zirconyl chloride solution, control solution ph 9-10 or so continues to stir, until obtaining
The uniform precursor liquid of chemical constituent；
(3) presoma is washed repeatedly with deionized water, until being free of Cl in filtrate-Ion；
(4) presoma of certain mass is taken to be scattered in deionized water, mineralizer triethanolamine is added will expect after mixing
It is fitted into microwave hydrothermal reaction kettle, carries out microwave hydrothermal reaction；
(5) after will be above-mentioned should after obtained powder deionized water and dehydrated alcohol clean and filter repeatedly after dry, obtain two
Nm-class powder of zirconium oxide.
In a kind of above-mentioned high dispersive cubic phase nano zirconium oxide and preparation method thereof, preferably, the addition is steady
Determine agent YCl3·6H2The amount of O is 2-8mol% (with ZrOCl2·8H2O molar amount), the amount that composite dispersing agent is added is 1.0-
5.0wt.% is (with ZrOCl2·8H2O and YCl3·6H2O mass meter).
In a kind of above-mentioned high dispersive cubic phase nano zirconium oxide and preparation method thereof, preferably, the dispersing agent
For one of polymethylacrylic acid, polyacrylic acid, polyethyleneimine, polyethylene glycol 400~4000 or a variety of.
In a kind of above-mentioned high dispersive cubic phase nano zirconium oxide and preparation method thereof, preferably, the ammonium hydroxide
Concentration is 0.5-1mol/L, rate of addition 0.5-1mL/min, mixing time 60-120min.
In a kind of above-mentioned high dispersive cubic phase nano zirconium oxide and preparation method thereof, preferably, the mineralizer
Concentration is 0.1-0.5mol/L, and microwave hydrothermal temperature is 160-260 DEG C, reaction pressure 0.4-4.0MPa, microwave hydrothermal time 10-
90min；
In a kind of above-mentioned high dispersive cubic phase nano zirconium oxide and preparation method thereof, preferably, the drying side
Formula is freeze-drying, and drying condition is -57 DEG C, 10-15h, 20-35Pa.
The Zirconium dioxide nano powder is tetragonal phase zirconium oxide, and pattern is spherical in shape, and crystallinity is high, grain diameter 20~
40nm, and particle diameter distribution is narrow, good dispersion
Compared with prior art, the present invention having a kind of following major advantage: 1. high dispersive cubic phase nanos of the invention
Zirconium oxide and preparation method thereof, using composite dispersing agent it is possible to prevente effectively from conventional hydrothermal method and chemical synthesis prepare nano oxygen
The reunion of powder during change zirconium, obtains the big nano zircite product of crystallinity height, good dispersion, specific surface；Using microwave
It is simple that hydro-thermal method prepares nano zirconium oxide powder its production procedure, and process effectively prevents subsequent high temperature calcination process, cost with
Low energy consumption, environmental-friendly, scaleable, easy to industrialized production.2. a kind of high dispersive cubic phase nano zirconium oxide of the invention
And preparation method thereof, by adding mineralizer triethanolamine during microwave hydrothermal, substantially reduce ZrO2When powder synthesizes
Between, improve the crystal property of powder.3. a kind of high dispersive cubic phase nano zirconium oxide of the invention and preparation method thereof uses
The mode of freeze-drying, obtained diameter of particle narrowly distributing and uniformly are reunited few, good dispersion.
A kind of high dispersive cubic phase nano zirconium oxide of the invention and preparation method thereof, the cubic phase nano oxidation prepared
Zirconium powder body, pattern is spherical in shape, and crystallinity is high, and grain diameter is in 20-40nm, and particle diameter distribution is narrow, good dispersion.
Detailed description of the invention
Fig. 1 is the XRD diagram of gained nano zirconium oxide powder in the embodiment of the present invention 1
Fig. 2 is the TEM figure of gained nano zirconium oxide powder in the embodiment of the present invention 1
Fig. 3 is the XRD diagram of gained nano zirconium oxide powder in the embodiment of the present invention 2
Fig. 4 is the TEM figure of gained nano zirconium oxide powder in the embodiment of the present invention 2
Fig. 5 is the XRD diagram of gained nano zirconium oxide powder in the embodiment of the present invention 3
Fig. 6 is the TEM figure of gained nano zirconium oxide powder in the embodiment of the present invention 3
Specific embodiment
After now specific embodiments of the present invention are described in.
Embodiment 1
By ZrOCl2·8H2O dissolves the zirconium solution for being configured to that concentration is 0.1mol/L in deionized water, and stabilizer is added
YCl3·6H2O and dispersing agent Macrogol 4000；The ammonium hydroxide of 0.5mol/L is added dropwise in zirconyl chloride solution (drop speed
0.5mL/min), control solution ph is 9 or so, continues to stir, until obtaining the uniform precursor liquid of chemical constituent；Use deionization
Water washs presoma repeatedly, until being free of Cl- ion in filtrate；It takes the presoma of certain mass to be scattered in deionized water, adds
Entering concentration is 0.3mol/L triethanolamine as mineralizer, and after mixing, slurries are fitted into microwave hydrothermal reaction kettle,
200 DEG C, microwave hydrothermal reacts 30min under pressure 1.628MPa in kettle；Finally, by the powder deionized water obtained after reaction and
Dehydrated alcohol is cleaned and is filtered repeatedly, is freeze-dried 10h under -57 DEG C, 20Pa, obtains nano zirconium oxide powder 1.By nano oxygen
Change zirconium powder body 1 to be analyzed using X-ray diffraction analysis (see Fig. 1) and transmission electron microscope (see Fig. 2), it is known that nano zirconium oxide powder
1 is square zirconium oxide, and shape is spherical shape, and particle is uniform, has and slightly reunites, and the average grain diameter of nano zirconium oxide powder 1 is 25
~35nm.
Embodiment 2
By ZrOCl2·8H2O dissolves the zirconium solution for being configured to that concentration is 0.1mol/L in deionized water, and stabilizer is added
YCl3·6H2O and dispersing agent Macrogol 4000；The ammonium hydroxide of 0.5mol/L is added dropwise in zirconyl chloride solution (drop speed
0.5mL/min), control solution ph is 9 or so, continues to stir, until obtaining the uniform precursor liquid of chemical constituent；Use deionization
Water washs presoma repeatedly, until being free of Cl- ion in filtrate；It takes the presoma of certain mass to be scattered in deionized water, adds
Entering concentration is 0.3mol/L triethanolamine as mineralizer, and after mixing, slurries are fitted into microwave hydrothermal reaction kettle,
240 DEG C, microwave hydrothermal reacts 30min under pressure 3.885MPa in kettle；Finally, by the powder deionized water obtained after reaction and
Dehydrated alcohol is cleaned and is filtered repeatedly, is freeze-dried 10h under -57 DEG C, 20Pa, obtains nano zirconium oxide powder 2.By nano oxygen
Change zirconium powder body 2 and use X-ray diffraction analysis (see Fig. 3) and transmission electron microscope analysis (see Fig. 4), it is known that nano zirconium oxide powder 2 is
Square zirconium oxide, shape are that spheric granules is uniform, favorable dispersibility, the average grain diameter of nano zirconium oxide powder 2 is 30~
40nm。
Embodiment 3
By ZrOCl2·8H2O dissolves the zirconium solution for being configured to that concentration is 0.1mol/L in deionized water, and stabilizer is added
YCl3·6H2O and dispersing agent Macrogol 4000；The ammonium hydroxide of 0.5mol/L is added dropwise in zirconyl chloride solution (drop speed
0.5mL/min), solution ph 9 or so is controlled, continues to stir, until obtaining the uniform precursor liquid of chemical constituent；Use deionized water
Presoma is washed repeatedly, until being free of Cl- ion in filtrate；It takes the presoma of certain mass to be scattered in deionized water, is added
Concentration is 0.5mol/L triethanolamine as mineralizer, after mixing, slurries is fitted into microwave hydrothermal reaction kettle, 200
DEG C, microwave hydrothermal reacts 30min under pressure 1.628MPa in kettle；Finally, the powder deionized water and nothing that will be obtained after reaction
Water-ethanol is cleaned and is filtered repeatedly, is freeze-dried 15h under -57 DEG C, 25Pa, obtains nano zirconium oxide powder 3.It will be nano oxidized
Zirconium powder body 3 is analyzed using X-ray diffraction analysis (see Fig. 5) and transmission electron microscope (see Fig. 6), it is known that nano zirconium oxide powder 3
For square zirconium oxide, shape is spherical shape, and particle is uniform, has and slightly reunites, the average grain diameter of nano zirconium oxide powder 3 is 20~
30nm。
Sample manufactured in the present embodiment obtains the Zirconium powder that primary particle size mean value is 20~40nm or so, uses microwave
The nano zirconium oxide powder form of hydro-thermal method preparation is more regular, and spherical in shape, crystal property is good, good dispersion property, and prepares
Diameter of particle it is smaller, and it can thus be appreciated that embodiment 2 be optimum embodiment of the present invention.
Although the present invention has already been described in detail in the embodiment, itself is simultaneously not considered as to limit of the invention
System.The invention is not limited to above embodiment, using same as the previously described embodiments or similar raw material and preparation method or
All changes, equivalents and the improved preparation method within the context described in it are chased after, should be included in of the invention
Within protection scope.
Claims (9)
1. a kind of high dispersive cubic phase nano zirconium oxide and preparation method thereof, with ZrOCl2·8H2O is raw material, is added into raw material
Stabilizer, dispersing agent and mineralizer, mainly comprise the steps that
(1) by zirconium oxychloride ZrOCl2·8H2O dissolves in deionized water, is configured to 0.1-0.5mol/L zirconyl chloride solution simultaneously
Stabilizer YCl is added3·6H2O and dispersing agent, obtain solution A；
(2) ammonium hydroxide is added dropwise in solution A, controls solution ph 9 or so, continues to stir, until it is equal to obtain chemical constituent
Even precursor liquid；
(3) presoma is washed repeatedly with deionized water, until being free of Cl in filtrate-Ion；
(4) it disperses presoma obtained above in deionized water, mineralizer triethanolamine is added will expect after mixing
It is fitted into microwave hydrothermal reaction kettle, carries out microwave hydrothermal reaction；
(5) after will be above-mentioned should after obtained powder deionized water and dehydrated alcohol clean and filter repeatedly after dry, obtain two
Nm-class powder of zirconium oxide.
2. a kind of high dispersive cubic phase nano zirconium oxide powder according to claim 1 and preparation method thereof, feature exists
In in step (1), the concentration of zirconyl chloride solution is 0.1-0.5mol/L.
3. a kind of high dispersive cubic phase nano zirconium oxide powder according to claim 1 and preparation method thereof, feature exists
In, in step (1), addition stabilizer YCl3·6H2The amount of O is 2-8mol% (with ZrOCl2·8H2O molar amount), it is added multiple
The amount for closing dispersing agent is 1.0-5.0wt.% (with ZrOCl2·8H2O and YCl3·6H2O mass meter).
4. a kind of high dispersive cubic phase nano zirconium oxide powder according to claim 1 and preparation method thereof, feature exists
In in step (1), dispersing agent is polymethylacrylic acid, polyacrylic acid, polyethyleneimine, one in polyethylene glycol 400~4000
Kind is a variety of.
5. a kind of high dispersive cubic phase nano zirconium oxide powder according to claim 1 and preparation method thereof, feature exists
In in step (2), the concentration of ammonium hydroxide is 0.5-1mol/L, rate of addition 0.5mL/min, mixing time 60-120min.
6. a kind of high dispersive cubic phase nano zirconium oxide powder according to claim 1 and preparation method thereof, feature exists
In in step (3), using the Cl in centrifugal process or the method for suction filtration removal filtrate-Ion, with the AgNO of 0.1mol/L3Solution inspection
Survey the Cl- ion in filtrate.
7. a kind of high dispersive cubic phase nano zirconium oxide powder according to claim 1 and preparation method thereof, feature exists
In in step (4), mineralizer triethanolamine concentrations are 0.1-0.5mol/L, and microwave hydrothermal temperature is 160-260 DEG C, reaction pressure
Power 0.4-4.0MPa, microwave hydrothermal time 10-90min.
8. a kind of high dispersive cubic phase nano zirconium oxide powder according to claim 1 and preparation method thereof, feature exists
In in step (5), drying mode is freeze-drying, and drying condition is -57 DEG C of temperature, time 10-15h, pressure 20-35Pa.
9. a kind of high dispersive cubic phase nano zirconium oxide powder according to claim 1 and preparation method thereof, feature exists
Be tetragonal phase zirconium oxide in, the Zirconium dioxide nano powder, pattern is spherical in shape, and crystallinity is high, grain diameter in 20~40nm,
And particle diameter distribution is narrow, good dispersion.
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| CN112125663A (en) * | 2020-08-14 | 2020-12-25 | 广东省科学院稀有金属研究所 | Preparation method of monodisperse yttria-stabilized zirconia nano powder |
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Application publication date: 20190906 |