CN108083334A - A kind of preparation method of monodisperse spherical nano zirconium dioxide powder body material - Google Patents
A kind of preparation method of monodisperse spherical nano zirconium dioxide powder body material Download PDFInfo
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- C01P2004/52—Particles with a specific particle size distribution highly monodisperse size distribution
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Abstract
The invention discloses a kind of preparation methods of monodisperse spherical nano zirconium dioxide powder body material, comprise the following steps：(1) it is 1~10 according to volume ratio by organic zirconium source, electrolyte solution and alcoholic solution:0.5~1.4:50~100 stocks, are divided into 2 parts by alcoholic solution；In inert gas environment, organic zirconium source and electrolyte solution are separately added into 2 parts of alcoholic solutions, obtain A mixed liquors and B mixed liquors after mixing；(2) B mixed liquors are instilled with the speed of 6~14d/s in A mixed liquors, after mixing, 7~9h is aged at 62~78 DEG C, after the completion of reaction, product is through centrifuging, washing, being dried in vacuo up to zirconium dioxide precursor powder；(3) by zirconium dioxide precursor powder in 450~750 DEG C of temperature lower calcinations, calcined after postcooling to room temperature to get Nanosized Zirconia Powders material.Zirconium dioxide prepared by the present invention is spherical in shape, centralized particle diameter, good dispersion.
Description
Technical field
The invention belongs to inorganic non-metallic oxide material preparing technical fields, and in particular to a kind of monodisperse spherical nano
The preparation method of zirconium dioxide powder body material.
Background technology
Zirconium dioxide (ZrO2) there is unique physics and chemical property, such as good both thermally and chemically stability, height
Intensity and fracture toughness, low heat conductivity and good wear resistance and corrosion resistance etc., thus except being used for tradition
Outside refractory material, the function ceramics such as piezo component, ceramic capacitor field and advanced structural ceramic, work(are also widely used in
The fields such as energy coating, lambda sensor and catalyst carrier, and in the application of the departments such as metallurgy, chemical industry, cosmetics, space flight and medicine
Also it is continuously increased, has broad application prospects.
At present, the preparation method of nano zirconium dioxide mainly has hydro-thermal method, sol-gel method, microemulsion method, coprecipitation
Deng.Hydro-thermal method is inconvenient for operation, the particle purity of preparation is relatively low and easy reunion, granularity are difficult to control, and grain diameter is larger, product
Lose more, low output.It is more that sol-gel method prepares the advantages of zirconium dioxide powder body material, such as reaction temperature is relatively low, dioxy
Change zirconium powder body even particle size distribution and size tunable, but due to adding in chelating agent in reaction process or surfactant to give birth to
Production cost greatly improves, and is unfavorable for large-scale industrial production, particle can be made quickly to reunite when being heat-treated at high temperature, is formed
Micelle and gel filtration, washing process are difficult to control.Microemulsion method is complicated there are production process, and of high cost and low yield etc. is no
Foot part.Coprecipitation process is simple, but easily introduces plurality of impurity ions and cause purity bad, and drying is precipitated in zirconium dioxide
Easily reunite the pattern for causing zirconium dioxide powder granule during calcining and dispersiveness is barely satisfactory.Therefore, find
A kind of simple controllable method, prepares the Nanosized Zircomea Particles powder that good dispersion, regular shape, and size distribution are concentrated
Material has great significance.
The content of the invention
It is an object of the invention to overcome above-mentioned technical deficiency, a kind of monodisperse spherical nano zirconium dioxide powder material is proposed
The preparation method of material solves nano zirconium dioxide bad dispersibility, skill in irregular shape and wide particle diameter distribution in the prior art
Art problem.
To reach above-mentioned technical purpose, technical scheme provides a kind of monodisperse spherical nano zirconium dioxide powder
The preparation method of material, comprises the following steps：
S1. it is 1~10 according to volume ratio by organic zirconium source, electrolyte solution and alcoholic solution：0.5~1.4：50~100 is standby
Material, is divided into 2 parts by alcoholic solution；In inert gas environment, organic zirconium source and electrolyte solution are separately added into 2 parts of alcoholic solutions
In, A mixed liquors and B mixed liquors are obtained after mixing；
S2. in inert gas environment, B mixed liquors is instilled with the speed of 6~14d/s in A mixed liquors, are uniformly mixed
Afterwards, 7~9h is aged at 62~78 DEG C, after the completion of reaction, product is through centrifuging, washing, being dried in vacuo up to zirconium dioxide forerunner
Body powder；
S3. under inert gas shielding, by zirconium dioxide precursor powder in 450~750 DEG C of temperature lower calcinations, calcined
To get Nanosized Zirconia Powders material after postcooling to room temperature.
Compared with prior art, beneficial effects of the present invention include：The technical program is by controlling organic zirconium source, electrolyte
The volume ratio of solution and alcoholic solution is aged reaction temperature, digestion time and addition rate, before effectively inhibiting zirconium dioxide
Drive zirconium dioxide particle agglomeration in body powder preparing processes；By controlling calcining heat, spherical and grain size can be directly obtained
Uniform nanometer materials, without using additional chelating agent or surfactant.The technical program is using hydrolysis zirconium
Source and temperature control calcine united method and prepare Nanosized Zirconia Powders material, and the zirconium dioxide powder body material prepared is in ball
Shape, centralized particle diameter, good dispersion and monodispersity excellent effect, the preparation process of the technical program is simple and practicable, is suitble to
Mass produce spherical nanometer zirconium dioxide powder body material.
Description of the drawings
Fig. 1 is the SEM figures of zirconium dioxide prepared by embodiment 1；
Fig. 2 is the XRD spectra of zirconium dioxide prepared by embodiment 1；
Fig. 3 is the grain size distribution of zirconium dioxide prepared by embodiment 1.
Specific embodiment
A kind of preparation method of monodisperse spherical nano zirconium dioxide powder body material is present embodiments provided, including following step
Suddenly：
(1) it is 1~10 according to volume ratio by organic zirconium source, electrolyte solution and alcoholic solution：0.5~1.4：50~100 is standby
Material, and alcoholic solution is divided into 2 parts；In inert gas environment, inert gas is preferably nitrogen, and organic zirconium source and electrolyte is molten
Liquid is separately added into 2 parts of alcoholic solutions, is uniformly mixed when temperature is 20~80 DEG C, is 50 DEG C as preferred mixing temperature,
Obtain A mixed liquors (mixed liquor of organic zirconium source -ol solution) and B mixed liquors (mixed liquor of electrolyte solution -ol solution)；
Organic zirconium source includes tetraethoxy zirconium, zirconium-n-propylate, zirconium iso-propoxide, zirconium tetraisopropoxide, zirconium-n-butylate, the tert-butyl alcohol
Zirconium, 2- [(2- amino-ethyls) amino] ethyl alcohol zirconium complex, 2- methyl-1s-propyl alcohol zirconates, double (diethyl citric acid) two propyl alcohol
At least one of zirconium.
Electrolyte solution can be at least one of metal salt solution, highly basic, weak acid and weak base, preferably, electrolysis
Matter solution is NaCl solution, NaOH solution, KOH solution, KCl solution, CH3COOH solution, NH4At least one of OH solution；Electricity
Electrolyte solution is concentrated solution, and concentration is 0.01~2.0mol/L, is preferably 0.3mol/L.
Alcohol in alcoholic solution is included in methanol, ethyl alcohol, normal propyl alcohol, isopropanol, n-butanol, isobutanol, sec-butyl alcohol, the tert-butyl alcohol
At least one.
(2) in inert gas environment, inert gas is nitrogen, by the B mixed liquors in step (1) with the speed of 6~14d/s
Degree is instilled in A mixed liquors, is then uniformly mixed mixed solution and is carried out ageing reaction, and reaction temperature is 62~78 DEG C,
Reaction time is 7~9h, and after the completion of reaction, product is through centrifuging, washing, being dried in vacuo up to zirconium dioxide precursor powder；
(3) the zirconium dioxide precursor powder in step (2) is placed in temperature control in inert atmosphere stove and calcines 2~10h, inertia
Atmosphere furnace is nitrogen atmosphere stove, and calcining heat is 450~750 DEG C, is cooled to the furnace after having calcined after room temperature to get nano-silica
Change zirconium powder body material.
Below in conjunction with specific embodiment to the system of monodisperse spherical nano zirconium dioxide powder body material provided by the invention
Preparation Method is further described.The embodiments described below is exemplary, be only used for explain the present invention, and it is not intended that
Limitation of the present invention.
Since the effect of organic zirconium source, electrolyte solution and alcoholic solution in the present invention is roughly the same, can mutually replace
It changes, the organic zirconium source in following embodiments selects zirconium-n-butylate (IV) to be illustrated, and electrolyte solution selects KCl molten
Liquid is illustrated, and alcoholic solution selects butanol solution to be illustrated.
Embodiment 1：
A kind of preparation method of monodisperse spherical nano zirconium dioxide powder body material is present embodiments provided, including following step
Suddenly：
(1) KCl is made into the KCl solution of 0.3mol/L, according to zirconium-n-butylate (IV), KCl solution and butanol solution
Volume ratio is 2：1：80 stocks, and alcoholic solution is divided into 2 parts；Under nitrogen atmosphere protection, zirconium-n-butylate and KCl solution are distinguished
It adds in 2 parts of butanol solutions, 30min is persistently stirred at 50 DEG C and obtains uniformly mixed A mixed liquors and B mixed liquors；
(2) the B mixed liquors in step (1) are instilled according to the speed of 10d/s in A mixed liquors, and is persistently stirred liquid
It is warming up to 70 DEG C after 1h to start to be aged, is persistently aged 8h, after the completion of reaction, products therefrom is through centrifuging, washing, being dried in vacuo to obtain the final product
Zirconium dioxide precursor powder；
(3) the zirconium dioxide precursor powder in step (2) is placed in nitrogen atmosphere stove and calcined, in 600 DEG C of perseverances
Temperature calcining 5h, cools to room temperature with the furnace to get Nanosized Zirconia Powders material after having calcined.
By detecting and analyzing, the Nanosized Zirconia Powders material that the present embodiment obtains is put down in homodisperse spherical shape
Equal grain size is 130nm.
Method according to embodiment 1 prepares the product of embodiment 2~10 and comparative example 1~4, and raw material and method are the same as real
Example 1 is applied, the volume ratio difference lies in the raw material added in, step (1) is different, specific experiment condition and the results are shown in Table 1.
Influence of the volume ratio of 1 raw material of table to product
(note：" -- " represents not measuring or unmeasured in form)
From Examples 1 to 10 and comparative example 1~4, work as zirconium-n-butylate, any raw material in KCl solution and n-butanol
Amount when adding in excessive or very few, zirconium dioxide obtained is in irregular shape or spherical, and zirconium dioxide powder can part
Reunion or serious agglomeration, only when V (zirconium-n-butylate)：V (KCl solution)：V (n-butanol) is 1~10：0.5~1.4：50~100
It adds in, zirconium dioxide powder body material ability obtained spherical in shape, centralized particle diameter and good dispersion；By Examples 1 to 4 and reality
It applies example 5~10 to understand, when V (zirconium-n-butylate)：V (KCl solution)：V (n-butanol) is 2：0.5~1.4：When 80, and using other
Zirconium dioxide prepared by volume ratio raw material is compared, zirconium dioxide average grain diameter smaller obtained, and effect is more preferable；By Examples 1 to 4
It understands, when V (zirconium-n-butylate)：V (KCl solution)：V (n-butanol) is 2：1：When 80, zirconium dioxide average grain diameter obtained is most
Small, performance is best.
The product of embodiment 11~12 and comparative example 5~7 is prepared according to the method for embodiment 1, raw material and method are same
Embodiment 1, difference lies in instill B mixed liquors, specific experiment condition into A mixed liquors in step (2) according to different speed
With the results are shown in Table 2.
Table 2 instills influence of the speed to product
(note：" -- " represents not measuring or unmeasured in form)
From embodiment 1,11 and 12 and comparative example 5~7, when B mixed liquors addition A mixed liquor medium velocities are too fast or mistake
Slowly, final product quality obtained, only when it is 6~14d/s to add in speed, zirconium dioxide powder material obtained can be influenced
Material just spherical in shape, centralized particle diameter and good dispersion, and when it is 10d/s to add in speed, zirconium dioxide obtained is averaged grain
Footpath is minimum, and performance is best.
The product of embodiment 13~14 and comparative example 8~10 is prepared according to the method for embodiment 1, raw material and method are same
Embodiment 1, difference lies in, Aging Temperature is different in step (2), after mixed liquor is uniformly mixed, rises to 62 DEG C respectively, and 78
DEG C, 50 DEG C, 60 DEG C, 80 DEG C start to be aged, digestion time 8h, specific experiment condition and the results are shown in Table 3.
Influence of 3 Aging Temperature of table to product
(note：" -- " represents not measuring or unmeasured in form)
It is understood by embodiment 1,13 and 14 and comparative example 8~10, when Aging Temperature is too high or too low, can influenced final
Product quality obtained, only when Aging Temperature is 62~78 DEG C, spherical in shape, the grain size of zirconium dioxide powder body material ability obtained
Distribution is concentrated and good dispersion, and when Aging Temperature is 70 DEG C, zirconium dioxide average grain diameter obtained is minimum, and performance is best.
The product of embodiment 15~16 and comparative example 11~13 is prepared according to the method for embodiment 1, raw material and method are equal
With embodiment 1, difference lies in digestion time is different in step (2), after mixed liquor is uniformly mixed, is warming up to 70 DEG C and opens
Begin ageing, it is respectively 7h, 9h, 4h, 6h, 10h to continue digestion time, specific experiment condition and the results are shown in Table 4.
Influence of 4 digestion time of table to product
(note：" -- " represents not measuring or unmeasured in form)
It is understood by embodiment 1,15 and 16 and comparative example 11~13, when digestion time is long or too short, can influenced
Final product quality obtained, only when digestion time is 7~9h, spherical in shape, the grain of zirconium dioxide powder body material ability obtained
Footpath distribution is concentrated and good dispersion, and when digestion time is 8h, zirconium dioxide average grain diameter obtained is minimum, and performance is best.
The product of embodiment 17~18 and comparative example 14~16 is prepared according to the method for embodiment 1, raw material and method are equal
With embodiment 1, difference lies in the calcining heat of zirconium dioxide precursor powder is different in step (3), by zirconium dioxide presoma
Powder is placed in nitrogen atmosphere stove and is calcined, respectively the calcining at constant temperature at 400 DEG C, 450 DEG C, 750 DEG C, 800 DEG C, 1000 DEG C
5h, specific experiment condition and the results are shown in Table 5.
Influence of 5 calcining heat of table to product
(note：" -- " represents not measuring or unmeasured in form)
Understood by embodiment 1,17 and 18 and comparative example 14~16, when zirconium dioxide precursor powder calcining heat too
When high or too low, final product quality obtained, only when calcining heat is 450~750 DEG C, dioxy obtained can be influenced
Change zirconium powder body material just spherical in shape, centralized particle diameter and good dispersion, and when calcining heat is 600 DEG C, dioxy obtained
It is minimum to change zirconium average grain diameter, performance is best.
From above example and comparative example, when preparing zirconium dioxide using the technical program, when the volume ratio of raw material
For V (zirconium-n-butylate)：V (KCl solution)：V (n-butanol)=2：1：The mixed liquor addition zirconium-n-butylate of 80, KCl- n-butanols-just
The mixed liquor medium velocity of butanol is 10d/s, and ageing reaction temperature is 70 DEG C, reaction time 8h, and zirconium dioxide precursor
When the calcining heat at end is 600 DEG C, zirconium dioxide obtained is not only spherical in shape, centralized particle diameter, good dispersion, and average grain
Footpath is minimum, and performance is best.
The specific embodiment of present invention described above, is not intended to limit the scope of the present invention..Any basis
The various other corresponding changes and deformation that the technical concept of the present invention is made, should be included in the guarantor of the claims in the present invention
In the range of shield.
Claims (10)
1. a kind of preparation method of monodisperse spherical nano zirconium dioxide powder body material, which is characterized in that comprise the following steps：
S1. it is 1~10 according to volume ratio by organic zirconium source, electrolyte solution and alcoholic solution：0.5~1.4：50~100 stocks, will
Alcoholic solution is divided into 2 parts；In inert gas environment, organic zirconium source and electrolyte solution are separately added into 2 parts of alcoholic solutions, mixed
A mixed liquors and B mixed liquors are obtained after uniformly；
S2. in inert gas environment, B mixed liquors are instilled with the speed of 6~14d/s in A mixed liquors, after mixing,
7~9h is aged at 62~78 DEG C, after the completion of reaction, product is through centrifuging, washing, being dried in vacuo up to zirconium dioxide precursor
End；
S3. it is cold after having calcined by zirconium dioxide precursor powder in 450~750 DEG C of temperature lower calcinations under inert gas shielding
But to after room temperature to get Nanosized Zirconia Powders material.
2. the preparation method of monodisperse spherical nano zirconium dioxide powder body material according to claim 1, which is characterized in that
The volume ratio in organic zirconium source, electrolyte solution and alcoholic solution is 2 in the step S1：0.5~1.4：80.
3. the preparation method of monodisperse spherical nano zirconium dioxide powder body material according to claim 1, which is characterized in that
The volume ratio in organic zirconium source, electrolyte solution and alcoholic solution is 2 in the step S1：1：80.
4. the preparation method of monodisperse spherical nano zirconium dioxide powder body material according to claim 1, which is characterized in that
Organic zirconium source in the step S1 include tetraethoxy zirconium, zirconium-n-propylate, zirconium iso-propoxide, zirconium tetraisopropoxide, zirconium-n-butylate,
Zirconium tert-butoxide, 2- [(2- amino-ethyls) amino] ethyl alcohol zirconium complex, 2- methyl-1s-propyl alcohol zirconates, double (diethyl citric acids)
At least one of dipropyl alcohol zirconium.
5. the preparation method of monodisperse spherical nano zirconium dioxide powder body material according to claim 1, which is characterized in that
The alcohol in alcoholic solution in the step S1 includes methanol, ethyl alcohol, normal propyl alcohol, isopropanol, n-butanol, isobutanol, sec-butyl alcohol, uncle
At least one of butanol.
6. the preparation method of monodisperse spherical nano zirconium dioxide powder body material according to claim 1, which is characterized in that
The concentration of electrolyte solution is 0.01~2.0mol/L in the step S1.
7. the preparation method of monodisperse spherical nano zirconium dioxide powder body material according to claim 1, which is characterized in that
The mixing temperature that A mixed liquors and B mixed liquors are mixed in the step S1 is 20~80 DEG C.
8. the preparation method of monodisperse spherical nano zirconium dioxide powder body material according to claim 1, which is characterized in that
Instillation speed in the step S2 is 10d/s.
9. the preparation method of monodisperse spherical nano zirconium dioxide powder body material according to claim 1, which is characterized in that
Aging Temperature in the step S2 is 70 DEG C, digestion time 8h.
10. the preparation method of monodisperse spherical nano zirconium dioxide powder body material according to claim 1, feature exist
In the calcining heat in the step S3 is 600 DEG C, and calcination time is 2~10h.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109110809A (en) * | 2018-08-03 | 2019-01-01 | 长江大学 | A kind of composite cathode material for lithium ion cell ZrO2And preparation method thereof |
| CN110217818A (en) * | 2019-06-13 | 2019-09-10 | 中国科学院广州地球化学研究所 | Uniform particle size zirconium dioxide nanosphere and its film and preparation method |
| CN115954511A (en) * | 2023-03-14 | 2023-04-11 | 潮州三环（集团）股份有限公司 | Electrolyte powder and preparation method and application thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109110809A (en) * | 2018-08-03 | 2019-01-01 | 长江大学 | A kind of composite cathode material for lithium ion cell ZrO2And preparation method thereof |
| CN110217818A (en) * | 2019-06-13 | 2019-09-10 | 中国科学院广州地球化学研究所 | Uniform particle size zirconium dioxide nanosphere and its film and preparation method |
| CN115954511A (en) * | 2023-03-14 | 2023-04-11 | 潮州三环（集团）股份有限公司 | Electrolyte powder and preparation method and application thereof |
| CN115954511B (en) * | 2023-03-14 | 2023-06-16 | 潮州三环（集团）股份有限公司 | Electrolyte powder and preparation method and application thereof |
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