CN108675348A - A method of preparing superfine zirconia powder - Google Patents
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- CN108675348A CN108675348A CN201810726033.2A CN201810726033A CN108675348A CN 108675348 A CN108675348 A CN 108675348A CN 201810726033 A CN201810726033 A CN 201810726033A CN 108675348 A CN108675348 A CN 108675348A
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Abstract
The invention belongs to technical fields prepared by nano-powder, are related to a kind of method preparing superfine zirconia powder.The present invention precipitation method prepare ultra-fine ZrO2Powder, in precipitate phase, replace deionized water as reaction carriers using absolute ethyl alcohol, it is precipitating and is introducing the processing modes such as ultrasonic disperse and activated carbon adsorption respectively in ageing process, and stringent control is carried out to zirconium ion solution concentration, supersonic frequency, reaction temperature, activated carbon dosage, calcination temperature and soaking time etc., to the nanometer ZrO to preparation2The dispersibility and particle size uniformity of powder are strictly controlled.
Description
Technical field
The invention belongs to the technical fields of nano-powder, are related to a kind of method preparing superfine zirconia powder.
Background technology
Zirconium oxide is a kind of important semiconductor material with wide forbidden band.It has good chemical stability, mechanical strength and
Low-thermal conductivity, and make it important high temperature resistant with properties, these properties such as high-melting-point, high resistivity, high refractive indexes
Material, ceramic insulating material and ceramic opacifier, are also the primary raw materials manually bored.Therefore, ultra-fine ZrO is prepared2Powder has
Wide application prospect is one of the hot spot of material science research.
Preparing ultra-fine ZrO2In the method for powder, the precipitation method are widely adopted.It includes preparing instead that the precipitation method, which prepare powder,
Answer solution, precipitation, washing, drying, calcining, sieving.The precipitation method are anti-by the way that zirconium ion in solution and precipitating reagent occurs
Presoma should be obtained, then presoma is filtered and washed, dried and calcining and decomposing, to obtain required ZrO2It receives
Rice flour body.The ZrO that the precipitation method are prepared2Powder has many advantages, such as that granule-morphology is good, grain size is small.
But there is also many problems, such as the grain size of powder and dispersibility cannot obtain stabilization during the precipitation method
Control.Reason is primarily due to the precipitation method and prepares ZrO2During nano-powder, due to preparation nano-powder grain size very
It is small, often it is 100nm or so, so the specific surface energy of powder is very big, precipitation, ageing, calcination stage are all easy to reunite
And grain size phenomena such as becoming larger.Traditional dispersing mode is that ammonium sulfate is added into solution as dispersant, is sent out in precipitate phase
The electrostatic repulsion for waving sulfate radical acts on to improve the dispersibility of granular precursor.But the high decomposition temperature of sulfate radical (>1000
DEG C) to lead to it be difficult to be completely removed in calcination stage, remaining sulfate radical will become the impurity in powder.In addition, traditional
Precipitation reaction solvent be generally aqueous solution, and in the drying process, due to the removal of water, powerful capillary between powder granule
Guan Li also results in the serious agglomeration of powder.Therefore, take a rational deposition condition and dispersing method to controllably making
Standby ZrO2Nano-powder has great significance.
Invention content
Ultra-fine ZrO is prepared effectively to solve the precipitation method2Since dispersibility is not effectively controlled and causes in powder process
Size tunable it is poor, dispersibility it is bad the problems such as, the invention discloses a kind of methods preparing superfine zirconia powder.This side
The reaction dissolvent of method is absolute ethyl alcohol, and is taken respectively at ultrasonic disperse and activated carbon adsorption in the precipitation of reaction, ageing stage
Reason can effectively solve the precipitation method and prepare nanometer ZrO2The problems such as size tunable is poor in powder process, dispersibility is bad, greatly
The powder characteristic in reaction process is improved, and this method, to the of less demanding of equipment, final experimental result is more controllable, grasps
Make simple, high yield rate.
The present invention is realized by following technical solution：
The present invention provides a kind of method preparing superfine zirconia powder, it is characterised in for preparing nanometer using the precipitation method
ZrO2Powder replaces deionized water as reaction dissolvent, is precipitating and in ageing process points in precipitate phase using absolute ethyl alcohol
Not Yin Ru the processing modes such as ultrasonic disperse and activated carbon adsorption, and to zirconium ion solution concentration, supersonic frequency, reaction temperature, work
Property charcoal dosage, calcination temperature and soaking time etc. carry out stringent control, to the nanometer ZrO to preparation2Powder dispersibility and
Particle size uniformity is strictly controlled, and is included the following steps：
(1) reaction solution is prepared：ZrOCl is poured into container2·8H2O crystal adds absolute ethyl alcohol to dissolve to obtain ZrOCl2
Solution, using magnetic stirring apparatus to ZrOCl2Solution carries out continuing stirring, until fully dissolving；
(2) heating water bath：Uniformly mixed zirconium ion solution is placed in water bath with thermostatic control and is heated, after being raised to certain temperature,
Ammonia spirit is slowly dropped into and fills ZrOCl2In solution, until reaction solution pH reaches 4.8~5.2；It is right in this process
Reaction solution carries out continuing stirring, along with the discontinuity ultrasonic disperse of certain frequency in whipping process；
(3) it is aged：Magnetic stirring apparatus, ultrasonic disperse device and heating device are closed, activity is added into reaction solution
Charcoal particle then takes out to be placed in air and is aged as absorption carrier；
(4) it washs：The precipitation for preparing gained is filtered, is washed with absolute ethyl alcohol, until can not with silver nitrate solution
Detect Cl-；The precipitated filter cakes for washing and being obtained by filtration are collected into evaporating dish, drying box drying is placed in；
(5) it calcines：Presoma after drying is subjected to sieving processing, to the precursor powder after sieving be placed in Muffle furnace into
Row calcination processing obtains ZrO2Powder；
(6) it is sieved：Powder after calcining is subjected to sieving processing, by the ZrO after sieving2Powder is collected, and is obtained subsphaeroidal
Nanometer ZrO2Powder.
In step (1), a concentration of 0.1~0.3mol/L of the zirconium ion solution, the rotary speed of magnetic stirring apparatus is
150~300r/min.
In step (2), bath temperature is 25~30 DEG C, and heating rate is 0.5~1.5 DEG C/min, and ammonia spirit is a concentration of
2.0~3.0mol/L, dropwise addition ammonium hydroxide rate be 2~6mL/min, ultrasonic disperse frequency be 20~60KHz, ultrasonic time be 3~
6min, ultrasonic break time are 3~6min.
In step (3), activated carbon and ZrOCl2·8H2O crystal quality ratios are 2:1~4:1, digestion time is 8~16h.
In step (4), drying temperature is 40~55 DEG C, and drying time is 24~36h.
In step (5), sieving selects the specification of nylon test sieve for 100~300 mesh, and sieving number is 2~4 times, calcining
Temperature is 800~1000 DEG C, and soaking time is 2~5h.
In step (6), sieving selects the specification of nylon test sieve for 200~300 mesh, and sieving number is 2~5 times.
Beneficial effects of the present invention
(1) in precipitation reaction, using absolute ethyl alcohol as reaction dissolvent, zirconium hydroxide presoma is in absolute ethyl alcohol
Solubility be significantly smaller than its solubility in deionized water, this will make the outburst of presoma nucleation stage be nucleated, and make to obtain
The quantity of the presoma obtained is increased sharply, and the grain size of each granular precursor greatly reduces.And due to absolute ethyl alcohol surface tension
The only one third of the surface tension of water, therefore drying stage pass through the capillary between the powder granule of ethanol system preparation
Guan Li is also significantly smaller than the capillary force between the powder granule prepared using aqueous systems, therefore can be with point of significant increase powder
Dissipate property.
(2) ultrasonic disperse, the cavitation that ultrasound is brought is used to will produce microcosmic part in precipitate phase due to this method
High temperature and pressure, and generate huge impact force and microjet, under its effect, surface energy is weakened nano-powder, to real
Now to the peptizaiton of nano-powder.
(3) activated carbon is added as absorption carrier in the ageing stage due to this method, granular precursor will be by uniform adsorption
Agglomeration on active carbon particle, therefore between presoma will be weakened severely；And in calcination process, activated carbon
Grain will decompose, the CO of generation2Gas will to generate space steric effect between particle, to improve the dispersion of powder
Property.
Description of the drawings
Fig. 1 is Zirconium powder XRD diagram prepared by embodiment 1.
Fig. 2 is Zirconium powder SEM figures prepared by embodiment 1.
Specific implementation mode
With reference to specific example and Figure of description, the present invention is described further, but should not limit this hair with this
Bright protection domain.
Embodiment 1
ZrOCl is poured into container2·8H2O crystal, adds absolute ethyl alcohol to be diluted to ZrOCl2Solution, zirconium ion solution concentration
For 0.1mol/L, mixed solution is carried out using magnetic stirring apparatus to continue stirring, until solution is uniformly mixed, magnetic stirring apparatus
Rotary speed is 150r/min.Uniformly mixed solution is placed in water bath with thermostatic control and is heated, bath temperature is 25 DEG C, heating rate
For 0.5 DEG C/min, magnetic stirring apparatus is used in combination to be stirred, after solution temperature reaches 25 DEG C, ammonium hydroxide is slowly dropped into and is filled
ZrOCl2In the beaker of solution, ammonia spirit a concentration of 2.0mol/L, drop rate 2mL/min keep magnetic in the process
Power blender persistently stirs, and along with the discontinuity ultrasonic disperse of certain frequency, ultrasonic disperse frequency in whipping process
For 20KHz, each ultrasonic time is 3min, and ultrasonic break time is also 3min.
After reaction solution pH reaches 4.8, magnetic stirring apparatus, ultrasonic disperse device and heating device are closed, to solution
Middle addition active carbon particle as absorption carrier, then take out beaker be placed in it is still aging in air.Wherein activated carbon with
ZrOCl2·8H2O crystal quality ratios are 2：1, digestion time 8h.Then the precipitation for preparing gained is filtered, with anhydrous second
Alcohol washs, until can not detect Cl with silver nitrate solution-。
The precipitated filter cakes for washing and being obtained by filtration are collected into evaporating dish, drying box drying is placed in, drying temperature is
40 DEG C, drying time is for 24 hours；
Presoma after drying is subjected to sieving processing, sieving selects the specification of nylon test sieve for 100 mesh, and be sieved number
It is 4 times；Precursor powder after sieving is placed in Muffle furnace and carries out calcination processing, obtains subsphaeroidal nanometer ZrO2Particle is forged
It is 800 DEG C to burn temperature, soaking time 5h；
Powder after calcining is subjected to sieving processing, by the ZrO after sieving2Powder is collected, and subsphaeroidal nanometer ZrO is obtained2Powder
Body, wherein sieving selects the specification of nylon test sieve for 200 mesh, sieving number is 5 times.
Fig. 1 is Zirconium powder SEM figures prepared by embodiment 1, as shown, the Zirconium powder prepared using this method
Grain size is 100nm or so, and particle diameter distribution is more uniform, and dispersibility is preferably.
Fig. 1 is Zirconium powder XRD diagram prepared by embodiment 1, as shown in Figure 1, using powder prepared by this method for list
Oblique zirconium oxide phase, without other dephasigns, powder purity is higher.
Embodiment 2
ZrOCl is poured into container2·8H2O crystal, adds absolute ethyl alcohol to be diluted to ZrOCl2Solution, zirconium ion solution concentration
For 0.2mol/L, mixed solution is carried out using magnetic stirring apparatus to continue stirring, until solution is uniformly mixed, magnetic stirring apparatus
Rotary speed is 250r/min.Uniformly mixed solution is placed in water bath with thermostatic control and is heated, bath temperature is 28 DEG C, heating rate
For 1.0 DEG C/min, magnetic stirring apparatus is used in combination to be stirred, after solution temperature reaches 28 DEG C, ammonium hydroxide is slowly dropped into and is filled
ZrOCl2In the beaker of solution, ammonia spirit a concentration of 2.5mol/L, drop rate 4mL/min keep magnetic in the process
Power blender persistently stirs, and along with the discontinuity ultrasonic disperse of certain frequency, ultrasonic disperse frequency in whipping process
For 40KHz, each ultrasonic time is 5min, and ultrasonic break time is also 5min.
After reaction solution pH reaches 5.0, magnetic stirring apparatus, ultrasonic disperse device and heating device are closed, to solution
Middle addition active carbon particle as absorption carrier, then take out beaker be placed in it is still aging in air.Wherein activated carbon with
ZrOCl2·8H2O crystal quality ratios are 3：1, digestion time 12h.Then the precipitation for preparing gained is filtered, use is anhydrous
Ethyl alcohol washs, until can not detect Cl with silver nitrate solution-。
The precipitated filter cakes for washing and being obtained by filtration are collected into evaporating dish, drying box drying is placed in, drying temperature is
50 DEG C, drying time 30h；
Presoma after drying is subjected to sieving processing, sieving selects the specification of nylon test sieve for 200 mesh, and be sieved number
It is 3 times；Precursor powder after sieving is placed in Muffle furnace and carries out calcination processing, obtains subsphaeroidal nanometer ZrO2Particle is forged
It is 900 DEG C to burn temperature, soaking time 4h；
Powder after calcining is subjected to sieving processing, by the ZrO after sieving2Powder is collected, and subsphaeroidal nanometer ZrO is obtained2Powder
Body, wherein sieving selects the specification of nylon test sieve for 250 mesh, sieving number is 4 times.
Embodiment 3
ZrOCl is poured into container2·8H2O crystal, adds absolute ethyl alcohol to be diluted to ZrOCl2Solution, zirconium ion solution concentration
For 0.3mol/L, mixed solution is carried out using magnetic stirring apparatus to continue stirring, until solution is uniformly mixed, magnetic stirring apparatus
Rotary speed is 300r/min.Uniformly mixed solution is placed in water bath with thermostatic control and is heated, bath temperature is 30 DEG C, heating rate
For 1.5 DEG C/min, magnetic stirring apparatus is used in combination to be stirred, after solution temperature reaches 30 DEG C, ammonium hydroxide is slowly dropped into and is filled
ZrOCl2In the beaker of solution, ammonia spirit a concentration of 3.0mol/L, drop rate 6mL/min keep magnetic in the process
Power blender persistently stirs, and along with the discontinuity ultrasonic disperse of certain frequency, ultrasonic disperse frequency in whipping process
For 60KHz, each ultrasonic time is 6min, and ultrasonic break time is also 6min.
After reaction solution pH reaches 5.2, magnetic stirring apparatus, ultrasonic disperse device and heating device are closed, to solution
Middle addition active carbon particle as absorption carrier, then take out beaker be placed in it is still aging in air.Wherein activated carbon with
ZrOCl2·8H2O crystal quality ratios are 4：1, digestion time 16h.Then the precipitation for preparing gained is filtered, use is anhydrous
Ethyl alcohol washs, until can not detect Cl with silver nitrate solution-。
The precipitated filter cakes for washing and being obtained by filtration are collected into evaporating dish, drying box drying is placed in, drying temperature is
55 DEG C, drying time 36h；
Presoma after drying is subjected to sieving processing, sieving selects the specification of nylon test sieve for 300 mesh, and be sieved number
It is 2 times；Precursor powder after sieving is placed in Muffle furnace and carries out calcination processing, obtains subsphaeroidal nanometer ZrO2Particle is forged
It is 1000 DEG C to burn temperature, soaking time 2h；
Powder after calcining is subjected to sieving processing, by the ZrO after sieving2Powder is collected, and subsphaeroidal nanometer ZrO is obtained2
Powder, wherein sieving selects the specification of nylon test sieve for 300 mesh, sieving number is 2 times.
Claims (8)
1. a kind of method preparing superfine zirconia powder, which is characterized in that include the following steps：
(1) reaction solution is prepared：ZrOCl is poured into container2·8H2O crystal adds absolute ethyl alcohol to dissolve to obtain ZrOCl2Solution,
Using magnetic stirring apparatus to ZrOCl2Solution carries out continuing stirring, until fully dissolving；
(2) heating water bath：Uniformly mixed zirconium ion solution is placed in water bath with thermostatic control and is heated, after being raised to certain temperature, by ammonia
Aqueous solution, which is slowly dropped into, fills ZrOCl2In solution, until reaction solution pH reaches 4.8~5.2；In this process to reaction
Liquid carries out continuing stirring, along with the discontinuity ultrasonic disperse of certain frequency in whipping process；
(3) it is aged：Magnetic stirring apparatus, ultrasonic disperse device and heating device are closed, activated carbon is added into reaction solution
Grain is used as absorption carrier, then takes out to be placed in air and is aged；
(4) it washs：The precipitation for preparing gained is filtered, is washed with absolute ethyl alcohol, until can not be detected with silver nitrate solution
To Cl-；The precipitated filter cakes for washing and being obtained by filtration are collected into evaporating dish, drying box drying is placed in；
(5) it calcines：Presoma after drying is subjected to sieving processing, the precursor powder after sieving is placed in Muffle furnace and is forged
Burning processing, obtains ZrO2Powder；
(6) it is sieved：Powder after calcining is subjected to sieving processing, by the ZrO after sieving2Powder is collected, and subsphaeroidal nanometer is obtained
ZrO2Powder.
2. a kind of method preparing superfine zirconia powder as described in claim 1, which is characterized in that described in step (1)
The rotary speed of a concentration of 0.1~0.3mol/L of zirconium ion solution, magnetic stirring apparatus are 150~300r/min.
3. a kind of method preparing superfine zirconia powder as described in claim 1, which is characterized in that in step (2), water-bath
Temperature be 25~30 DEG C, heating rate be 0.5~1.5 DEG C/min, ultrasonic disperse frequency be 20~60KHz, ultrasonic time be 3~
6min, ultrasonic break time are 3~6min.
4. a kind of method preparing superfine zirconia powder as described in claim 1, which is characterized in that in step (2), ammonium hydroxide
Solution concentration is 2.0~3.0mol/L, and dropwise addition ammonium hydroxide rate is 2~6mL/min.
5. a kind of method preparing superfine zirconia powder as described in claim 1, which is characterized in that in step (3), activity
Charcoal and ZrOCl2·8H2O crystal quality ratios are 2:1~4:1, digestion time is 8~16h.
6. a kind of method preparing superfine zirconia powder as described in claim 1, which is characterized in that dry in step (4)
Temperature is 40~55 DEG C, and drying time is 24~36h.
7. a kind of method preparing superfine zirconia powder as described in claim 1, which is characterized in that in step (5), sieving
Select the specification of nylon test sieve for 100~300 mesh, sieving number is 2~4 times, and calcination temperature is 800~1000 DEG C, heat preservation
Time is 2~5h.
8. a kind of method preparing superfine zirconia powder as described in claim 1, which is characterized in that in step (6), sieving
Select the specification of nylon test sieve for 200~300 mesh, sieving number is 2~5 times.
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| CN112194184A (en) * | 2020-10-10 | 2021-01-08 | 贵州梅岭电源有限公司 | Preparation method of nano silver chromate |
| CN112871148A (en) * | 2021-01-20 | 2021-06-01 | 陕西瑞科新材料股份有限公司 | Preparation method of zirconium dioxide carrier for noble metal catalyst |
| CN113135593A (en) * | 2021-05-25 | 2021-07-20 | 西南科技大学 | Method for preparing high-purity nano zirconium dioxide by hydrothermal-assisted sol-gel method |
| CN113681007A (en) * | 2021-09-14 | 2021-11-23 | 山东金钻石金属材料有限公司 | Copper-gold powder collecting and storing method |
| CN116282144A (en) * | 2023-02-15 | 2023-06-23 | 吕梁学院 | Preparation method of zirconium dioxide |
| CN117185346A (en) * | 2023-09-11 | 2023-12-08 | 苏州市伊贝高温技术材料有限公司 | Intelligent zirconia powder processing device, method and system and storage medium |
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|---|---|---|---|---|
| CN112194184A (en) * | 2020-10-10 | 2021-01-08 | 贵州梅岭电源有限公司 | Preparation method of nano silver chromate |
| CN112871148A (en) * | 2021-01-20 | 2021-06-01 | 陕西瑞科新材料股份有限公司 | Preparation method of zirconium dioxide carrier for noble metal catalyst |
| CN113135593A (en) * | 2021-05-25 | 2021-07-20 | 西南科技大学 | Method for preparing high-purity nano zirconium dioxide by hydrothermal-assisted sol-gel method |
| CN113135593B (en) * | 2021-05-25 | 2022-01-28 | 西南科技大学 | Method for preparing high-purity nano zirconium dioxide by hydrothermal-assisted sol-gel method |
| CN113681007A (en) * | 2021-09-14 | 2021-11-23 | 山东金钻石金属材料有限公司 | Copper-gold powder collecting and storing method |
| CN116282144A (en) * | 2023-02-15 | 2023-06-23 | 吕梁学院 | Preparation method of zirconium dioxide |
| CN116282144B (en) * | 2023-02-15 | 2024-04-12 | 吕梁学院 | Preparation method of zirconium dioxide |
| CN117185346A (en) * | 2023-09-11 | 2023-12-08 | 苏州市伊贝高温技术材料有限公司 | Intelligent zirconia powder processing device, method and system and storage medium |
| CN117185346B (en) * | 2023-09-11 | 2024-07-02 | 苏州市伊贝高温技术材料有限公司 | Intelligent zirconia powder processing device, method and system and storage medium |
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Application publication date: 20181019 |