CN104606061B - A kind of preparation method of dental Zirconium oxide powder - Google Patents
A kind of preparation method of dental Zirconium oxide powder Download PDFInfo
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- CN104606061B CN104606061B CN201510045489.9A CN201510045489A CN104606061B CN 104606061 B CN104606061 B CN 104606061B CN 201510045489 A CN201510045489 A CN 201510045489A CN 104606061 B CN104606061 B CN 104606061B
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- zirconium oxide
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Abstract
The invention discloses a kind of preparation method of dental Zirconium oxide powder.Including:Add organic solvent after zirconium oxide and yittrium oxide mixing to be dispersed with stirring, be tuned into the slurry that solid content is 20 30%, be dispersed with stirring, be then sanded, dried, crush after obtained Zirconium oxide powder.With 1000 parts of calculating of gross mass, wherein zirconium oxide is 800 950 parts, and yittrium oxide is 50 200 parts.Preparation process simple and convenient of the present invention, cost is relatively low, and the cycle is short, reproducible, and powder granularity is uniform, is nanoscale, is adapted to batch production.
Description
Technical field
The present invention relates to dental material field, further say, be to be related to a kind of preparation of dental Zirconium oxide powder
Method.
Background technology
The method for preparing dental Zirconium powder at present mainly has three kinds：Coprecipitation, sol-gel process, tradition are solid
Mechanical kilowatt mixing method.When preparing powder using coprecipitation, sediment is easily reunited when washing, filter, drying so that
Powder granularity is bigger than normal, bad dispersibility.The cycle that sol-gel process prepares powder is longer, and cost is higher, same easily to reunite, no
It is adapted to batch production.Conventional solid mechanical mixing is generally adopted by ball grinding technique, the particle diameter of its abrasive body zirconia ball compared with
Greatly so that synthetic powder particle is thicker, and can not be well mixed the Ball-milling Time, it is necessary to longer.Therefore there is an urgent need to seek one
Novel powder preparation technology is planted to solve problem above, the process that sand milling technology prepares powder is simple and convenient, and the cycle is short, repeatability
It is good, and the powder granularity prepared is uniform, is nanoscale, is adapted to batch production.
The content of the invention
To solve produced problem in the prior art, the invention provides a kind of preparation side of dental Zirconium oxide powder
Method.Preparation process simple and convenient, cost is relatively low, and the cycle is short, reproducible, and powder granularity is uniform, is nanoscale, is adapted to criticize
Amount production.
It is an object of the invention to provide a kind of preparation method of dental Zirconium oxide powder.
Including：
Organic solvent is added after zirconium oxide and yittrium oxide mixing, the slurry that solid content is 20-30% is tuned into, is dispersed with stirring,
Then be sanded, dried, crush after be made Zirconium oxide powder.The yittrium oxide of addition plays the work of tetragonal phase of zirconia stabilizer
With.
The organic solvent is ethanol, methanol, acetone or carbon tetrachloride, preferably ethanol.
Wherein, preferably：
Using zirconium oxide and yittrium oxide gross mass as 1000 parts of calculating, wherein zirconium oxide is 800-950 parts, yittrium oxide 50-
200 parts.
It is 20-120 minutes to be dispersed with stirring the time.The sand milling time is 2-6 hours, and abrasive body is particle diameter 0.01-0.9mm oxygen
Change zirconium ball, it is that 2000-4000 turns/min that rotating speed, which is sanded,.
Drying temperature is 20-100 DEG C, and drying time is 2-20 hours.
It is calcined respectively before zirconium oxide and yittrium oxide mixing, removes moisture removal, roasting time is 2~6 hours.
Specifically include following steps：
(1) baking material：A certain amount of zirconium oxide, yittrium oxide are weighed roughly, is placed in different oxidation zirconium crucibles, and are put into electricity
Hinder in stove, 2-6 hours are calcined at 400-800 DEG C, remove the moisture in raw material；
(2) dispensing：Each oxide raw material is accurately weighed according to stoichiometric proportion, with 1000 parts of calculating of gross mass, wherein oxygen
Change zirconium is 800-950 parts, and yittrium oxide is 50-200 parts；
(3) disperse：Each oxide raw material is placed in magazine, it is 20- to add appropriate organic solvent and be tuned into solid content
30% slurry, is sufficiently stirred, and disperses 20-120 minutes；
(4) it is sanded：Scattered slurry is imported in sand mill, 2-6 hours are sanded under 2000-4000 turns/min, grind
Mill body is particle size 0.01-0.9mm zirconia ball；
(5) dry：Slurry after sand milling is placed in drying box, 2-20 hours are dried at 20-100 DEG C；
(6) crush：By dried block powder crushing grinding, sieving, that is, obtain final powder, average grain diameter is less than etc.
In 80nm.
The present invention has the advantages that：
The reunion that the present invention uses organic solvent to be solved for abrasive media encountered in traditional powder preparation technology is asked
Topic, its preparation process simple and convenient, cost is relatively low, and the cycle is short, reproducible, and powder granularity is uniformly (shown in Fig. 1), to receive
Meter level, it is adapted to batch production.The powder diameter scope prepared by sand milling is within 80nm (shown in Fig. 2).
Brief description of the drawings
Taken into consideration outside powder prepared by Fig. 1 present invention；
Nano-powder transmission electron microscope photo prepared by Fig. 2 embodiments 4, average grain diameter are less than 40nm；
The XRD of nano-powder synthesis in solid state result prepared by Fig. 3 embodiments 1.
Embodiment
With reference to embodiment, the present invention is further illustrated.
Embodiment 1
(1) baking material：A certain amount of zirconium oxide, yittrium oxide are weighed roughly, is placed in different oxidation zirconium crucibles, and are put into electricity
Hinder in stove, be calcined 6 hours at 400 DEG C, remove the moisture in raw material；
(2) dispensing：Each oxide raw material is accurately weighed according to stoichiometric proportion, with 1000 parts of calculating of gross mass, wherein oxygen
It is 800 parts to change zirconium, and yittrium oxide is 200 parts；
(3) disperse：Each oxide raw material is placed in magazine, adds organic solvent ethanol, being tuned into solid content is
20% slurry, is sufficiently stirred, and disperses 120 minutes；
(4) it is sanded：Scattered slurry is imported in sand mill, is sanded 6 hours under 2000 turns/min, abrasive body is grain
Footpath size 0.01-0.06mm zirconia ball；
(5) dry：Slurry after sand milling is placed in drying box, dried 20 hours at 20 DEG C；
(6) crush：By dried block powder crushing grinding, sieving, that is, final powder is obtained, particle diameter is less than or equal to
80nm, transmission electron microscope results are as shown in Figure 2.
Embodiment 2
(1) baking material：A certain amount of zirconium oxide is weighed roughly, yittrium oxide is placed in different oxidation zirconium crucibles, and is put into electricity
Hinder in stove, be calcined 4 hours at 500 DEG C, remove the moisture in raw material；
(2) dispensing：Each oxide raw material is accurately weighed according to stoichiometric proportion, with 1000 parts of calculating of gross mass, wherein oxygen
It is 900 parts to change zirconium, and yittrium oxide is 100 parts；
(3) disperse：Each oxide raw material is placed in magazine, adds organic solvent methanol, being tuned into solid content is
25% slurry, is sufficiently stirred, and disperses 90 minutes；
(4) it is sanded：Scattered slurry is imported in sand mill, respectively each sand under 2300 turns/min and 2500 turn/min
Mill 4 hours, abrasive body are particle size 0.04-0.06mm zirconia ball；
(5) dry：Slurry after sand milling is placed in drying box, dried 12 hours at 35 DEG C；
(6) crush：By dried block powder crushing grinding, sieving, that is, final powder is obtained, particle diameter is less than or equal to
70nm。
Embodiment 3
(1) baking material：A certain amount of zirconium oxide is weighed roughly, yittrium oxide is placed in different oxidation zirconium crucibles, and is put into electricity
Hinder in stove, be calcined 5 hours at 600 DEG C, remove the moisture in raw material；
(2) dispensing：Each oxide raw material is accurately weighed according to stoichiometric proportion, with 1000 parts of calculating of quality, wherein aoxidizing
Zirconium is 920 parts, and yittrium oxide is 80 parts；
(3) disperse：Each oxide raw material is placed in magazine, adds organic solvent-acetone, being tuned into solid content is
30% slurry, is sufficiently stirred, and disperses 90 minutes；
(4) it is sanded：Scattered slurry is imported in sand mill, respectively each sand under 2200 turns/min and 2600 turn/min
Mill 3 hours, abrasive body are particle size 0.05-0.07mm zirconia ball；
(5) dry：Slurry after sand milling is placed in drying box, dried 8 hours at 55 DEG C；
(6) crush：By dried block powder crushing grinding, sieving, that is, obtain final powder, average grain diameter is less than etc.
In 70nm.
Embodiment 4
(1) baking material：A certain amount of zirconium oxide is weighed roughly, yittrium oxide is placed in different oxidation zirconium crucibles, and is put into electricity
Hinder in stove, be calcined 2 hours at 800 DEG C, remove the moisture in raw material；
(2) dispensing：Each oxide raw material is accurately weighed according to stoichiometric proportion, with 1000 parts of calculating of gross mass, wherein oxygen
It is 950 parts to change zirconium, and yittrium oxide is 50 parts；
(3) disperse：Each oxide raw material is placed in magazine, organic solvent carbon tetrachloride, being tuned into solid content is
30% slurry, is sufficiently stirred, and disperses 20 minutes；
(4) it is sanded：Scattered slurry is imported in sand mill, respectively each sand under 2400 turns/min and 4000 turn/min
Mill 2 hours, abrasive body are particle size 0.04-0.9mm zirconia ball；
(5) dry：Slurry after sand milling is placed in drying box, dried 2 hours at 100 DEG C；
(6) crush：By dried block powder crushing grinding, sieving, that is, obtain final powder, average grain diameter is less than etc.
In 40nm.
Claims (6)
1. a kind of preparation method of dental Zirconium oxide powder, it is characterised in that methods described comprises the steps of:
Organic solvent is added after zirconium oxide and yittrium oxide mixing, the slurry that solid content is 20-30% is tuned into, is dispersed with stirring, then
Be sanded, dried, crush after be made Zirconium oxide powder；
The organic solvent is ethanol, methanol, acetone or carbon tetrachloride；
Wherein, using zirconium oxide and yittrium oxide gross mass as 1000 parts of calculating, wherein zirconium oxide is 800-950 parts, yittrium oxide 50-
200 parts.
2. the preparation method of dental Zirconium oxide powder as claimed in claim 1, it is characterised in that：
The organic solvent is ethanol.
3. the preparation method of dental Zirconium oxide powder as claimed in claim 1, it is characterised in that：
It is 20-120 minutes to be dispersed with stirring the time.
4. the preparation method of dental Zirconium oxide powder as claimed in claim 1, it is characterised in that：
The sand milling time is 2-6 hours, and abrasive body is particle diameter 0.01-0.9mm zirconia ball, be sanded rotating speed be 2000-4000 turn/
min。
5. the preparation method of dental Zirconium oxide powder as claimed in claim 1, it is characterised in that：
Drying temperature is 20-100 DEG C, and drying time is 2-20 hours.
6. the preparation method of the dental Zirconium oxide powder as described in one of Claims 1 to 5, it is characterised in that：
It is calcined respectively before zirconium oxide and yittrium oxide mixing, removes moisture removal, roasting time is 2~6 hours.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1986424A (en) * | 2006-12-28 | 2007-06-27 | 昆明贵金属研究所 | Alcohol-water co-precipiting and low temperature treating process for preparing superfine zirconia powder |
| CN102260078A (en) * | 2010-05-31 | 2011-11-30 | 比亚迪股份有限公司 | Zirconia ceramic and preparation method thereof |
| CN103204542A (en) * | 2013-05-07 | 2013-07-17 | 景德镇陶瓷学院 | Method for preparing stable zirconium oxide ultrafine powder by non-aqueous precipitation method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103550069B (en) * | 2013-10-30 | 2015-04-22 | 西安博科新材料科技有限责任公司 | Zirconia ceramic material applied to dental restoration and preparation method of zirconia ceramic material |
| CN103936416B (en) * | 2014-04-03 | 2016-04-13 | 南昌大学 | A kind of dental prosthetic yttria-stabilized zirconia pottery and preparation method thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1986424A (en) * | 2006-12-28 | 2007-06-27 | 昆明贵金属研究所 | Alcohol-water co-precipiting and low temperature treating process for preparing superfine zirconia powder |
| CN102260078A (en) * | 2010-05-31 | 2011-11-30 | 比亚迪股份有限公司 | Zirconia ceramic and preparation method thereof |
| CN103204542A (en) * | 2013-05-07 | 2013-07-17 | 景德镇陶瓷学院 | Method for preparing stable zirconium oxide ultrafine powder by non-aqueous precipitation method |
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Inventor after: Bao Jinxiao Inventor after: Song Xiwen Inventor after: Tian Wei Inventor after: Xie Min Inventor after: Zhou Fen Inventor after: Gao Jianquan Inventor before: Song Xiwen Inventor before: Bao Jinxiao Inventor before: Xie Min Inventor before: Zhou Fen Inventor before: Gao Jianquan |
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Effective date of registration: 20180108 Address after: 014016 the Inner Mongolia Autonomous Region Baotou Kunqu Arden Street No. 7 Co-patentee after: Baotou Jin Gerui new ceramics limited liability company Patentee after: University of Science and Technology of Inner Mongolia Address before: 014010 the Inner Mongolia Autonomous Region Baotou City, rare-earth high tech Zone headquarters economic Park, No. 9 building 310-1 Patentee before: Baotou Jin Gerui new ceramics limited liability company |
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