CN108046775A - Complex phase powder and preparation method thereof - Google Patents
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- CN108046775A CN108046775A CN201711335172.4A CN201711335172A CN108046775A CN 108046775 A CN108046775 A CN 108046775A CN 201711335172 A CN201711335172 A CN 201711335172A CN 108046775 A CN108046775 A CN 108046775A
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Abstract
The present invention relates to a kind of complex phase powders and preparation method thereof, which comprises the following steps：S1, Ceramic precursor resin and oxide ceramic powder body are provided；S2, Ceramic precursor resin is dissolved in organic solvent, obtains Ceramic precursor resin solution, then oxide ceramic powder body is added in into Ceramic precursor resin solution, be stirred at room temperature, obtain mixed liquor；S3, mixed liquor is obtained into ceramic mixed slurry by grinding technics, then ceramic mixed slurry is dried and is dusted, obtain precursor powder；S4, precursor powder is calcined, obtains complex phase powder.The preparation method is simple for process, low energy consumption, of low cost, non-environmental-pollution, can be suitably used for production and the commercial Application of extensive spherical complex phase submicron powder.Also, obtained complex phase powder dispersity is good, uniform particle diameter, purity are high, ingredient is uniform, crystallinity is high and with spherical clad structure, can achieve the purpose that practical.
Description
Technical field
The present invention relates to a kind of complex phase powders and preparation method thereof.
Background technology
In recent years, nano complex phase ceramic material shows have better high temperature resistant, anticorrosive, high hard compared with single phase ceramic material
The characteristics such as degree and high tenacity.Such as in zirconium oxide-alumina system, by adding 40% (mass fraction) into 3Y-TZP
Aluminium oxide by 1450 DEG C of HIP processing, has been made the diphase ceramic material that intensity is up to 3000MPa, has been expected to as a kind of high
Toughness, the structural ceramic material of high intensity obtain practical, it has also become a hot spot of high performance ceramic material research.It is good
Complex phase powder is basis prepared by diphase ceramic material.It is one of major technique of powder working process that surface, which is modified, to improving
The application performance and application value of powder body material have most important；Powder surface modification technology is with Modern New composite diphase material
Rise and grow up, to organic/inorganic composite diphase material, inorganic/inorganic composite diphase material, coating or coating material, absorption
Or the preparation and application of catalysis material, environmentally conscious materials and superfine powder and nano-powder are of great significance.Prepare complex phase at present
The main method of ceramic powder has coprecipitation, hydro-thermal method, sol-gal process etc., and its preparation method is more complicated, morphology microstructure with
Phase composition is difficult to control, and in the case where not adding any additive, the complex phase powder of coprecipitation and hydro-thermal method preparation gained
The crystal morphology of body is mostly rodlike, block in sub-micron, can not obtain the complex phase powder of submicron order spherical shape.
To solve the process complexity that existing method prepares complex phase powder, powder composition is uneven with object distributed mutually, meanwhile,
Powder dispersity is poor under conditions of active additive is not added with, and can not obtain the complex phase powder that growth morphology is submicron order spherical shape
The technical issues of body, spy propose the present invention.
The content of the invention
It is an object of the invention to provide a kind of complex phase powder and preparation method thereof, by simple technique and it is relatively low into
Instinct efficiently prepares that powder crystallinity is good, purity is high, the uniform submicron order spherical shape complex phase powder of ingredient on a large scale.
In order to achieve the above objectives, the present invention provides following technical solution：A kind of complex phase raw powder's production technology, including following
Step：
S1, Ceramic precursor resin and oxide ceramic powder body are provided；
S2, the Ceramic precursor resin is dissolved in organic solvent, obtains Ceramic precursor resin solution, then to described
The oxide ceramic powder body is added in Ceramic precursor resin solution, is stirred at room temperature, obtains mixed liquor；
S3, mixed liquor described in step S2 is obtained into ceramic mixed slurry by ground and mixed, then the ceramics is mixed
Slurry, which is dried, to dust, and obtains precursor powder；
S4, precursor powder described in step S3 is calcined, obtains the complex phase powder.
Further, in step S1, the Ceramic precursor resin includes aluminium oxide ceramics presoma resin, zirconium oxide is made pottery
Any one in porcelain presoma resin, silicon oxide ceramics presoma resin or titanium oxide ceramics presoma resin.
Further, in step S1, the oxide ceramic powder body includes alumina ceramic powder, zirconia ceramics powder
Any one in body, silicon oxide ceramics powder or titanium oxide ceramics powder.
Further, in step S2, the organic solvent is included in ethylene glycol ethyl ether, absolute ethyl alcohol, normal propyl alcohol or toluene
Any one.
Further, in the Ceramic precursor resin solution ratio of Ceramic precursor resin be preferably 0.1~
75wt%.
Further, the specific steps of S3 include：
Mixed liquor described in step S2 is ground and mixed by extra-fine grinding technique, obtains ceramic mixed slurry, by institute
It states ceramic mixed slurry and is put into be dried in spray drying device and dust, obtain precursor powder.
Further, in step S4, in the calcination process, temperature is preferably 350 to 1300 DEG C, calcination time is preferred
For 1 to 14h.
In order to achieve the above objectives, the present invention also provides a kind of as answering obtained by the complex phase raw powder's production technology
Phase powder.
Compared with prior art, the beneficial effects of the present invention are：The complex phase raw powder's production technology of the present invention is by making
Mixed liquor is mixed and made into Ceramic precursor resin and nano-oxide ceramic powder, using extra-fine grinding technique, is prepared
Controllable submicron order spherical shape complex phase powder is formed, the preparation method is simple for process, low energy consumption, of low cost, non-environmental-pollution,
It can be suitably used for production and the commercial Application of extensive spherical complex phase submicron powder.
Also, obtained complex phase powder dispersity is good, uniform particle diameter, purity are high, ingredient is uniform, crystallinity is high and has
Spherical clad structure can achieve the purpose that practical.
Above description is only the general introduction of technical solution of the present invention, in order to better understand the technological means of the present invention,
And can be practiced according to the content of specification, below with presently preferred embodiments of the present invention and coordinate attached drawing be described in detail as after.
Description of the drawings
Fig. 1 is the process step figure of the complex phase raw powder's production technology shown in the present invention；
Fig. 2 is the TEM figures of the ceramic mixed slurry shown in the embodiment of the present invention one；
Fig. 3 is the line scanning figure of the ceramic mixed slurry shown in the embodiment of the present invention one；
Fig. 4 is the grain size distribution of the complex phase powder shown in the embodiment of the present invention one；
Fig. 5 is the TEM figures of the ceramic mixed slurry shown in the embodiment of the present invention two；
Fig. 6 is macroscopical TEM figures of the complex phase powder shown in the embodiment of the present invention two；
Fig. 7 is the microcosmic TEM figures of the complex phase powder shown in the embodiment of the present invention two；
Fig. 8 is the grain size distribution of the complex phase powder shown in the embodiment of the present invention two.
Specific embodiment
With reference to the accompanying drawings and examples, the specific embodiment of the present invention is described in further detail.Implement below
Example is not limited to the scope of the present invention for illustrating the present invention.
Fig. 1 is referred to, the complex phase raw powder's production technology shown in the present invention comprises the following steps：
S1, Ceramic precursor resin and oxide ceramic powder body are provided, the Ceramic precursor resin is made pottery including aluminium oxide
Porcelain presoma resin, zirconia ceramics presoma resin, silicon oxide ceramics presoma resin or titanium oxide ceramics presoma resin
In any one；The oxide ceramic powder body includes alumina ceramic powder, zirconia ceramics powder, silicon oxide ceramics powder
Any one in body or titanium oxide ceramics powder；
S2, the Ceramic precursor resin is dissolved in organic solvent, the organic solvent includes ethylene glycol ethyl ether, anhydrous
Any one in ethyl alcohol, normal propyl alcohol or toluene, be configured to mass ratio be preferably 0.1~75wt% Ceramic precursor resin it is molten
Liquid, then the oxide ceramic powder body is added in into the Ceramic precursor resin solution, it is stirred at room temperature, obtains mixed liquor；
S3, mixed liquor described in step S2 is added in into sand mill and grinds and mixes by extra-fine grinding technique, obtained
The ceramic mixed slurry is put into be dried in spray drying device and be dusted, obtains precursor powder by ceramic mixed slurry；
S4, precursor powder described in step S3 is forged under conditions of temperature preferably 350 to 1300 DEG C
It burns, calcination time is preferably 1 to 14h, obtains the complex phase powder with spherical core-shell structure.
Below in conjunction with specific embodiments come to the present invention illustrated in further detail.
Embodiment one
The titanium oxide ceramics presoma resin for weighing 39.58g is dissolved in normal propyl alcohol, and it is 15wt%'s to be configured to mass ratio
Titanium oxide ceramics forerunner's precursor resin solution, then the alumina ceramic powder of 39.58g is weighed, it is slowly added to titanium oxide ceramics
It drives in precursor resin solution, it is stirring while adding at ambient temperature, obtain mixed liquor.Mixed liquor is uniform by stick pin-type sand mill
It mixes and grinds, obtain ceramic mixed slurry after the completion of grinding, then ceramic mixed slurry is put into spray drying device and is carried out
Drying is dusted, and obtains precursor powder.Obtained precursor powder is finally calcined to 2h under the conditions of 350 DEG C of temperature to get to shell core
Structure and the titanium dioxide-aluminum oxide complex phase submicron powder for adulterating multielement, refer to Fig. 2 to Fig. 4, as seen from the figure, titanium oxide
Ceramic precursor resin is evenly coated at the surface of alumina ceramic powder, forms spherical core-shell structure.Also, ceramics mixing
The D50 of slurry is 161 nanometers, and particle diameter distribution is in relatively narrow bimodal distribution.
Embodiment two
The aluminium oxide ceramics presoma resin for weighing 38.03g is dissolved in absolute ethyl alcohol, is configured to mass ratio as 7wt%
Aluminium oxide ceramics forerunner's precursor resin solution, then weigh the zirconia ceramics powder of 150.53g, be slowly added to aluminium oxide ceramics
It is stirring while adding at ambient temperature in forerunner's precursor resin solution, obtain mixed liquor.Mixed liquor is equal by stick pin-type sand mill
Even mixing is simultaneously ground, and ceramic mixed slurry is obtained after the completion of grinding, then by ceramic mixed slurry be put into spray drying device into
Row drying is dusted, and obtains precursor powder.Finally obtained precursor powder is calcined under the conditions of 1000 DEG C of temperature 10h to get to
Core-shell structure and the aluminium oxide-zirconium oxide complex phase submicron powder for adulterating multielement, refer to Fig. 5 to Fig. 8, as seen from the figure, oxygen
Change the surface that aluminium Ceramic precursor resin is evenly coated at zirconia ceramics powder, form spherical core-shell structure.Also, complex phase
Powder D50 is 212 nanometers, and a very narrow distribution is presented in particle diameter distribution.
Embodiment three
The aluminium oxide ceramics presoma resin for weighing 52.07g is dissolved in ethylene glycol ethyl ether, and being configured to mass ratio is
The Ceramic precursor resin solution of 38wt%, then the silicon oxide ceramics powder of 121.49g is weighed, it is slowly added to ceramic forerunner
It is stirring while adding at ambient temperature in resin solution, obtain mixed liquor.Mixed liquor is uniformly mixed by stick pin-type sand mill
And grind, ceramic mixed slurry is obtained after the completion of grinding, then ceramic mixed slurry is put into spray drying device and is dried
It dusts, obtains precursor powder.Obtained precursor powder is finally calcined to 14h under the conditions of 1100 DEG C of temperature to get to shell core knot
Structure and the aluminium oxide-silicon oxide complex phase submicron powder for adulterating multielement.
Example IV
The silicon oxide ceramics presoma resin for weighing 15.09g is dissolved in toluene, is configured to the pottery that mass ratio is 75wt%
Porcelain forerunner's precursor resin solution, then the zirconia ceramics powder of 286.71g is weighed, it is slowly added to Ceramic precursor resin solution
In, it is stirring while adding at ambient temperature, obtain mixed liquor.Mixed liquor is uniformly mixed and ground by stick pin-type sand mill,
Ceramic mixed slurry is obtained after the completion of grinding, then ceramic mixed slurry is put into be dried in spray drying device and is dusted, is obtained
To precursor powder.Obtained precursor powder is finally calcined to 8h under the conditions of 573 DEG C of temperature to get to core-shell structure and adulterating more
The silica-zirconia complex phase submicron powder of element.
In summary：The complex phase raw powder's production technology of the present invention is by using Ceramic precursor resin and nano-oxide
Ceramic powder is mixed and made into mixed liquor, using extra-fine grinding technique, is prepared and forms controllable submicron order spherical shape complex phase powder
Body, the preparation method is simple for process, low energy consumption, of low cost, non-environmental-pollution, can be suitably used for extensive spherical complex phase sub-micron
The production of powder and commercial Application.
Also, the preparation method of the present invention can be such that the introducing of element more holds during final complex phase powder is formed
Easily effectively, and there are following characteristics：1st, element species are adjustable；2nd, element ratio is adjustable；3rd, the functional group in contained molecular composition
It is adjustable；4th, microstructure is nanostructured to Ceramic precursor resin under the high temperature conditions.
Meanwhile complex phase powder dispersity obtained by preparation in accordance with the present invention is good, uniform particle diameter, purity are high, into
Divide uniform, crystallinity height and with spherical clad structure, can achieve the purpose that practical.
Each technical characteristic of embodiment described above can be combined arbitrarily, to make description succinct, not to above-mentioned reality
It applies all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited
In contradiction, the scope that this specification is recorded all is considered to be.
Embodiment described above only expresses the several embodiments of the present invention, and description is more specific and detailed, but simultaneously
It cannot therefore be construed as limiting the scope of the patent.It should be pointed out that come for those of ordinary skill in the art
It says, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to the protection of the present invention
Scope.Therefore, the protection domain of patent of the present invention should be determined by the appended claims.
Claims (8)
1. a kind of complex phase raw powder's production technology, which is characterized in that comprise the following steps：
S1, Ceramic precursor resin and oxide ceramic powder body are provided；
S2, the Ceramic precursor resin is dissolved in organic solvent, obtains Ceramic precursor resin solution, then to the ceramics
The oxide ceramic powder body is added in forerunner's precursor resin solution, is stirred at room temperature, obtains mixed liquor；
S3, mixed liquor described in step S2 is obtained into ceramic mixed slurry by grinding technics, then by the ceramic mixed slurry
It is dried and dusts, obtain precursor powder；
S4, precursor powder described in step S3 is calcined, obtains the complex phase powder.
2. complex phase raw powder's production technology as described in claim 1, which is characterized in that in step S1, the ceramic forerunner
Resin includes aluminium oxide ceramics presoma resin, zirconia ceramics presoma resin, silicon oxide ceramics presoma resin or oxidation
Any one in titanium Ceramic precursor resin.
3. complex phase raw powder's production technology as described in claim 1, which is characterized in that in step S1, the oxide ceramics
Powder includes arbitrary in alumina ceramic powder, zirconia ceramics powder, silicon oxide ceramics powder or titanium oxide ceramics powder
It is a kind of.
4. complex phase raw powder's production technology as described in claim 1, which is characterized in that in step S2, the organic solvent bag
Include any one in ethylene glycol ethyl ether, absolute ethyl alcohol, normal propyl alcohol or toluene.
5. complex phase raw powder's production technology as described in claim 1, which is characterized in that in the Ceramic precursor resin solution
The ratio of Ceramic precursor resin is preferably 0.1~75wt%.
6. complex phase raw powder's production technology as described in claim 1, which is characterized in that the specific steps of S3 include：
Mixed liquor described in step S2 is ground and mixed by extra-fine grinding technique, obtains ceramic mixed slurry, by the pottery
Porcelain mixed slurry, which is put into be dried in spray drying device, to dust, and obtains precursor powder.
7. complex phase raw powder's production technology as described in claim 1, which is characterized in that in step S4, in the calcination process
In, temperature is preferably 350 to 1300 DEG C, calcination time is preferably 1 to 14h.
8. a kind of complex phase powder as obtained by the complex phase raw powder's production technology any one of claim 1 to 7.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102432294A (en) * | 2011-09-08 | 2012-05-02 | 浙江晟翔电子科技有限公司 | Preparation method of complex phase ceramic powder |
| CN102964114A (en) * | 2012-11-09 | 2013-03-13 | 航天材料及工艺研究所 | Method for preparing composite ceramic material through utilizing ceramic and precursor |
| CN104261851A (en) * | 2014-09-19 | 2015-01-07 | 航天材料及工艺研究所 | High-temperature resistant low-ablation coating and preparation method thereof |
| CN105254320A (en) * | 2015-11-13 | 2016-01-20 | 中航复合材料有限责任公司 | Preparation method of continuous oxide fiber reinforced oxide ceramic based composite |
| WO2017124065A1 (en) * | 2016-01-15 | 2017-07-20 | Hrl Laboratories, Llc | Resin formulations for polymer-derived ceramic materials |
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- 2017-12-14 CN CN201711335172.4A patent/CN108046775A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102432294A (en) * | 2011-09-08 | 2012-05-02 | 浙江晟翔电子科技有限公司 | Preparation method of complex phase ceramic powder |
| CN102964114A (en) * | 2012-11-09 | 2013-03-13 | 航天材料及工艺研究所 | Method for preparing composite ceramic material through utilizing ceramic and precursor |
| CN104261851A (en) * | 2014-09-19 | 2015-01-07 | 航天材料及工艺研究所 | High-temperature resistant low-ablation coating and preparation method thereof |
| CN105254320A (en) * | 2015-11-13 | 2016-01-20 | 中航复合材料有限责任公司 | Preparation method of continuous oxide fiber reinforced oxide ceramic based composite |
| WO2017124065A1 (en) * | 2016-01-15 | 2017-07-20 | Hrl Laboratories, Llc | Resin formulations for polymer-derived ceramic materials |
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Application publication date: 20180518 |