CN115650723A - Preparation method of zirconia ceramic rod - Google Patents
Preparation method of zirconia ceramic rod Download PDFInfo
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- CN115650723A CN115650723A CN202211397440.6A CN202211397440A CN115650723A CN 115650723 A CN115650723 A CN 115650723A CN 202211397440 A CN202211397440 A CN 202211397440A CN 115650723 A CN115650723 A CN 115650723A
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Abstract
The invention discloses a preparation method of a zirconia ceramic rod, belonging to the technical field of ceramic rods; the preparation method comprises the following steps: s1, modifying zirconia by adopting silicate ester to prepare silicate ester modified zirconia; modifying yttrium oxide by adopting titanate to prepare titanate modified yttrium oxide; s2, mixing the silicate modified zirconia, the titanate modified yttria and an adhesive to prepare pug; s3, extruding the pug to prepare a blank; and calcining the blank. According to the invention, the yttrium oxide and the zirconium oxide are subjected to modification treatment, so that the zirconium oxide and the yttrium oxide are fully fused, the density of the ceramic rod is improved, and the wear resistance of the ceramic rod is further improved.
Description
Technical Field
The invention belongs to the technical field of ceramic rods, and particularly relates to a preparation method of a zirconia ceramic rod.
Background
The zirconia ceramic rod is a ceramic rod made of zirconia materials, has the characteristics of high strength, high density, wear resistance, corrosion resistance, high temperature resistance and the like, and can be widely applied to the fields of electronic paste, semiconductors, new energy sources, new nano materials, medical instruments, refractory materials and the like.
CN102765943A discloses a preparation method of a zirconia ceramic rod for flame spraying, and the ceramic rodThe porcelain rod comprises the following main raw materials in percentage by weight: al (Al) 2 O 3 2％～3％、SiO 2 3％～4％、Fe 2 O 3 0.02％～0.03％、TiO 2 0.75 to 0.85 percent of CaO, 3.90 to 3.95 percent of CaO and the balance of ZrO 2 (ii) a The raw materials for preparing the zirconia ceramic rod have poor fusibility, and the formed material has low density, so that the finally prepared zirconia ceramic rod has poor wear resistance.
Therefore, the invention provides a preparation method of the zirconia ceramic rod, and the zirconia ceramic rod prepared by the method has good wear resistance.
Disclosure of Invention
An object of the present invention is to provide a method for preparing a zirconia ceramic rod to solve at least one aspect of the problems and disadvantages set forth in the background art described above.
Specifically, the invention provides a preparation method of a zirconia ceramic rod, which comprises the following steps:
s1, adding zirconium oxide into an ethanol water solution (the volume fraction of ethanol is 99%) and modifying with silicate to prepare silicate modified zirconium oxide;
modifying yttrium oxide by adopting titanate to prepare titanate modified yttrium oxide;
s2, mixing the silicate modified zirconia, the titanate modified yttria and an adhesive to prepare pug;
s3, extruding the pug to prepare a blank;
and calcining the blank.
According to one technical scheme of the preparation method provided by the invention, the preparation method at least has the following beneficial effects:
according to the invention, the zirconium oxide is subjected to silicate ester modification treatment, so that a silicon-containing group is grafted on the surface of the zirconium oxide, and the introduction of the silicon-containing group is beneficial to the full mixing of the zirconium oxide and the adhesive and the full dispersion of the zirconium oxide in the adhesive; and the silicon-containing group is converted into silicon dioxide, so that the full fusion of the zirconium oxide and the silicon dioxide is realized.
According to the invention, the yttrium oxide is subjected to titanate modification treatment, so that a titanium-containing group is grafted on the surface of the yttrium oxide, and the introduction of the titanium-containing group is beneficial to realizing the full mixing of the yttrium oxide and the adhesive and the full dispersion of the yttrium oxide and the zirconium oxide in the adhesive; and the titanium-containing group can be converted into titanium dioxide, so that the zirconium oxide, the yttrium oxide, the silicon dioxide and the titanium dioxide are fully fused, the density of the ceramic rod is improved, and the wear resistance of the ceramic rod is further improved.
According to some embodiments of the invention, the zirconia ceramic rod comprises the following preparation raw materials in parts by weight:
100 parts of zirconium oxide, 0.2-0.4 part of silicate ester, 10-20 parts of yttrium oxide, 0.1-0.2 part of titanate and 12-15 parts of adhesive.
According to some embodiments of the invention, the silicate is n-butyl silicate.
According to some embodiments of the invention, the method of preparing silicate-modified zirconia comprises the steps of:
adding zirconium oxide into an ethanol water solution to prepare a mixed system; and adding the silicate into the mixed system for reaction.
According to some embodiments of the invention, the reaction time during the preparation of the silicate-modified zirconia is between 2h and 3h.
According to some embodiments of the invention, the temperature of the reaction during the preparation of the silicate-modified zirconia is between 35 ℃ and 45 ℃.
According to some embodiments of the invention, the mass to volume ratio of the zirconia and the aqueous ethanol solution is 1g:50mL to 100mL.
According to some embodiments of the invention, the titanate is tetrabutyl titanate.
According to some embodiments of the invention, the method of preparing titanate-modified yttrium oxide comprises the steps of:
adding yttrium oxide into an ethanol water solution to prepare a mixed system; and adding the titanate into the mixed system for reaction.
According to some embodiments of the invention, the mass to volume ratio of the yttrium oxide to the aqueous ethanol solution is 1g:50mL to 100mL.
According to some embodiments of the invention, the volume fraction of the aqueous ethanol solution is between 95% and 99%.
According to some embodiments of the invention, the titanate modified yttrium oxide is prepared by a reaction time of 2-3 h.
According to some embodiments of the invention, the temperature of the reaction during the preparation of the titanate-modified yttrium oxide is between 35 ℃ and 45 ℃.
According to some embodiments of the invention, the adhesive comprises the following preparation raw materials in parts by weight:
10 parts of hydroxypropyl methyl cellulose, 1-2 parts of polyethylene glycol and 3-5 parts of water.
According to some embodiments of the invention, the polyethylene glycol is PEG1000.
According to some embodiments of the invention, the mixing is by ball milling.
According to some embodiments of the invention, the rotational speed of the ball mill is 300r/min to 500r/min.
According to some embodiments of the invention, the ball milling time is 1.5h to 2.5h.
According to some embodiments of the invention, the temperature of the calcination is from 1000 ℃ to 1500 ℃.
According to some embodiments of the invention, the calcination is for a time period of 8h to 12h.
According to some embodiments of the invention, the procedure of the calcination is as follows:
first temperature rise, first heat preservation, second temperature rise and second heat preservation.
According to some embodiments of the invention, the final temperature of the first temperature increase is 950 ℃ to 1050 ℃.
According to some embodiments of the invention, the temperature of the first incubation is between 950 ℃ and 1050 ℃.
According to some embodiments of the invention, the first incubation time is between 1.5h and 2.5h.
According to some embodiments of the invention, the final temperature of the second ramp is 1350 ℃ to 1450 ℃.
According to some embodiments of the invention, the holding temperature of the second holding is 1350 ℃ to 1450 ℃.
According to some embodiments of the invention, the holding time of the second holding is 5.5h to 6.5h.
According to some embodiments of the invention, the zirconia has a particle size of 500nm to 1000nm.
According to some embodiments of the invention, the yttria has a particle size of 100nm to 200nm.
By controlling the grain diameters of the zirconia and the yttria, the good grading of the yttria and the zirconia is realized, so that the density between the yttria and the zirconia is further improved, and the wear resistance and the density of the final ceramic rod are further improved.
According to some embodiments of the invention, the post-extrusion drying is at a temperature of 140 ℃ to 150 ℃.
According to some embodiments of the invention, the drying time is between 3h and 5h.
Detailed Description
The concept and technical effects of the present invention will be clearly and completely described below in conjunction with the embodiments to fully understand the objects, features and effects of the present invention. It is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments, and those skilled in the art can obtain other embodiments without inventive effort based on the embodiments of the present invention, and all embodiments are within the protection scope of the present invention.
In the description of the present invention, reference to the description of the terms "one embodiment," "some embodiments," "an illustrative embodiment," "an example," "a specific example," or "some examples," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
In the embodiment of the invention, the zirconium oxide is purchased from Ningbo Begal New materials Co., ltd, and the product number is B-ZrO 2 -200N(200nm)、B-ZrO 2 -500N(500nm)、B-ZrO 2 1W (1 μm) and B-ZrO 2 -5W(5μm)。
The yttrium oxide in the embodiment of the invention is purchased from Beijing, kyoko technology and technology Limited, and has the grain diameters of 50nm, 100nm, 200nm and 500nm.
Example 1
The embodiment is a preparation method of a zirconia ceramic rod, which comprises the following steps:
s1, raw material modification:
preparation of silicate-modified zirconia:
adding zirconium oxide into an ethanol water solution (the volume fraction is 99%, and the mass-volume ratio of the zirconium oxide to the ethanol water solution is 1g; after the reaction is finished, carrying out solid-liquid separation, and collecting a solid phase to prepare silicate ester modified zirconia;
modifying yttrium oxide by adopting titanate to prepare titanate modified yttrium oxide;
adding yttrium oxide into an ethanol water solution (the volume fraction is 99%, and the mass-volume ratio of yttrium oxide to the ethanol water solution is 1g; after the reaction is finished, carrying out solid-liquid separation, and collecting a solid phase to prepare titanate modified yttrium oxide;
s2, mixing materials:
mixing silicate modified zirconia, titanate modified yttria and adhesive, and ball milling to obtain pug;
in the embodiment, the ball milling time is 2 hours, and the rotating speed in the ball milling process is 400r/min.
S3, calcining:
extruding the pug in a vacuum extruder to prepare a blank;
drying the blank at 145 ℃ for 4h to obtain a dried blank;
then calcining the dried blank; the calcination was carried out in a horizontal sintering furnace, with the following calcination procedure:
firstly heating to 1000 ℃ (the heating time is 1 h), and preserving the heat for 2h at 1000 ℃;
heating to 1400 deg.C again (the heating rate is 20 deg.C/min), and keeping at 1400 deg.C for 6h.
The preparation method comprises the following raw materials in parts by mass:
100 parts of zirconia, 0.3 part of silicate ester (n-butyl silicate), 10 parts of yttrium oxide, 0.1 part of titanate and 15 parts of adhesive.
The adhesive in the embodiment is prepared from the following raw materials in parts by mass:
10 parts of hydroxypropylmethylcellulose, 2 parts of polyethylene glycol (PEG 1000) and 5 parts of water.
Example 2
This example is a method for preparing a zirconia ceramic rod, and is different from example 1 in that:
in this example, B-ZrO was selected as the zirconia 2 -1W(1μm)。
Example 3
This example is a method for preparing a zirconia ceramic rod, and is different from example 1 in that:
in this example, B-ZrO was selected as the zirconia 2 -5W(5μm)。
Example 4
This example is a method for preparing a zirconia ceramic rod, and is different from example 1 in that:
zirconium oxide in the present exampleBy using B-ZrO 2 -200N(200nm)。
Example 5
This example is a method for preparing a zirconia ceramic rod, and is different from example 1 in that:
the particle size of the yttrium oxide in this example was 200nm.
Example 6
This example is a method for preparing a zirconia ceramic rod, and is different from example 1 in that:
the particle size of the yttrium oxide in this example was 500nm.
Example 7
This example is a method for preparing a zirconia ceramic rod, and is different from example 1 in that:
the particle size of the yttrium oxide in this example was 50nm.
Comparative example 1
This comparative example is a method for preparing a zirconia ceramic rod, and is different from example 1 in that:
in this comparative example, the zirconia was not subjected to silicate modification treatment.
Comparative example 2
This comparative example is a method for preparing a zirconia ceramic rod, and is different from example 1 in that:
in this comparative example, no titanate modification treatment was performed on the yttrium oxide.
Comparative example 3
This comparative example is a method for preparing a zirconia ceramic rod, and is different from example 1 in that:
in this comparative example, the zirconium oxide was not subjected to silicate modification treatment and the yttrium oxide was not subjected to titanate modification treatment.
The performance test of the zirconia ceramic rods prepared in examples 1 to 7 of the present invention and comparative examples 1 to 3 was conducted according to the following method:
compressive strength: JIS R1601-2008.
The results of the performance test of the zirconia ceramic rods obtained in examples 1 to 7 of the present invention and comparative examples 1 to 3 are shown in table 1.
TABLE 1 results of property tests of zirconia ceramic rods obtained in inventive examples 1 to 7 and comparative examples 1 to 3
In conclusion, the silicon-containing groups are grafted on the surface of the zirconia by performing silicate modification treatment on the zirconia, and the introduction of the silicon-containing groups is favorable for fully mixing the zirconia and the binder and fully dispersing the zirconia in the binder; and the silicon-containing groups can be converted into silicon dioxide in the calcining process, so that the zirconium oxide and the silicon dioxide are fully fused. According to the invention, the yttrium oxide is subjected to titanate modification treatment, so that a titanium-containing group is grafted on the surface of the yttrium oxide, and the introduction of the titanium-containing group is beneficial to realizing the full mixing of the yttrium oxide and the adhesive and the full dispersion of the yttrium oxide and the zirconium oxide in the adhesive; and the titanium-containing group can be converted into titanium dioxide in the calcining process, so that the zirconium oxide, the yttrium oxide, the silicon dioxide and the titanium dioxide are fully fused, the density of the ceramic rod is improved, and the wear resistance of the ceramic rod is further improved.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and various modifications and changes may be made to the embodiment of the present invention by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are only exemplary embodiments of the present invention, and are not intended to limit the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The preparation method of the zirconia ceramic rod is characterized by comprising the following steps:
s1, modifying zirconia by using silicate ester to prepare silicate ester modified zirconia;
modifying yttrium oxide by adopting titanate to prepare titanate modified yttrium oxide;
s2, mixing the silicate modified zirconia, the titanate modified yttria and an adhesive to prepare pug;
s3, extruding the pug to prepare a blank;
and calcining the blank.
2. The method for preparing the zirconia ceramic rod according to claim 1, wherein the zirconia ceramic rod comprises the following raw materials in parts by weight:
100 parts of zirconium oxide, 0.2-0.4 part of silicate ester, 10-20 parts of yttrium oxide, 0.1-0.2 part of titanate and 12-15 parts of adhesive.
3. The method for preparing zirconia ceramic rods according to claim 1 where the silicate is butyl orthosilicate.
4. The method for producing a zirconia ceramic rod according to claim 1, wherein the titanate is tetrabutyl titanate.
5. The method for preparing zirconia ceramic rods according to any one of claims 1 to 4, wherein the binder comprises the following raw materials in parts by weight:
10 parts of hydroxypropyl methyl cellulose, 1-2 parts of polyethylene glycol and 3-5 parts of water.
6. The method for producing zirconia ceramic rods according to any one of claims 1 to 4, characterized in that the temperature of the calcination is 1000 ℃ to 1500 ℃.
7. The method for producing zirconia ceramic rods according to any one of claims 1 to 4, characterized in that the calcination time is 8 to 12 hours.
8. The method for producing a zirconia ceramic rod according to any one of claims 1 to 4, wherein the zirconia has a particle size of 500nm to 1000nm.
9. The method of manufacturing zirconia ceramic rods according to any of claims 1 to 4 where the yttria has a particle size of 100nm to 200nm.
10. The method for preparing zirconia ceramic rods according to any one of claims 1 to 4, wherein the post-extrusion drying is carried out at a temperature of 140 ℃ to 150 ℃.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004115343A (en) * | 2002-09-27 | 2004-04-15 | Nitsukatoo:Kk | Method of producing partially stabilized zirconia sintered compact |
| US20090215609A1 (en) * | 2005-04-15 | 2009-08-27 | Saint Gobain Centre De Recherches Et D'etudes Europeen | Zirconium-Base Sintered Product |
| CN102173800A (en) * | 2010-12-31 | 2011-09-07 | 中国科学院上海硅酸盐研究所 | Method for preparing yttrium aluminum garnet-based transparent ceramic by modifying of surface active agent |
| CN112552041A (en) * | 2019-09-10 | 2021-03-26 | 比亚迪股份有限公司 | Composition for preparing zirconia ceramic, zirconia ceramic and preparation method and application thereof |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004115343A (en) * | 2002-09-27 | 2004-04-15 | Nitsukatoo:Kk | Method of producing partially stabilized zirconia sintered compact |
| US20090215609A1 (en) * | 2005-04-15 | 2009-08-27 | Saint Gobain Centre De Recherches Et D'etudes Europeen | Zirconium-Base Sintered Product |
| CN102173800A (en) * | 2010-12-31 | 2011-09-07 | 中国科学院上海硅酸盐研究所 | Method for preparing yttrium aluminum garnet-based transparent ceramic by modifying of surface active agent |
| CN112552041A (en) * | 2019-09-10 | 2021-03-26 | 比亚迪股份有限公司 | Composition for preparing zirconia ceramic, zirconia ceramic and preparation method and application thereof |
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