CN115650723B - Preparation method of zirconia ceramic rod - Google Patents
Preparation method of zirconia ceramic rod Download PDFInfo
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- CN115650723B CN115650723B CN202211397440.6A CN202211397440A CN115650723B CN 115650723 B CN115650723 B CN 115650723B CN 202211397440 A CN202211397440 A CN 202211397440A CN 115650723 B CN115650723 B CN 115650723B
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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 zirconium oxide by silicate to obtain silicate modified zirconium oxide; modifying yttrium oxide by titanate to obtain titanate modified yttrium oxide; s2, mixing the silicate modified zirconia, the titanate modified yttrium oxide and an adhesive to prepare pugs; s3, extruding the pug to obtain a blank; and calcining the blank. According to the invention, the yttrium oxide and the zirconium oxide are modified, 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 processed by zirconia materials, has the characteristics of high strength, high density, wear resistance, corrosion resistance, high temperature resistance and the like, and is widely applied to the fields of electronic slurry, 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, the ceramic 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, 3.90 to 3.95 percent of CaO and the balance of ZrO 2 The method comprises the steps of carrying out a first treatment on the surface of the The fusion property of the raw materials for preparation is poor, and the density of the formed material is low, 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
The present invention is directed to a method for preparing a zirconia ceramic rod, which solves at least one of the problems and disadvantages set forth in the background art.
The invention provides a preparation method of a zirconia ceramic rod, which comprises the following steps:
s1, adding zirconia into an ethanol water solution (the volume fraction of ethanol is 99%) and modifying by silicate to prepare silicate modified zirconia;
modifying yttrium oxide by titanate to obtain titanate modified yttrium oxide;
s2, mixing the silicate modified zirconia, the titanate modified yttrium oxide and an adhesive to prepare pugs;
s3, extruding the pug to obtain a blank;
and calcining the blank.
According to one of the technical schemes of the preparation method, the preparation method at least has the following beneficial effects:
according to the invention, the zirconium oxide is subjected to silicate modification treatment, so that the silicon-containing groups are grafted on the surface of the zirconium oxide, the introduction of the silicon-containing groups is beneficial to the full mixing of the zirconium oxide and the adhesive, and meanwhile, the zirconium oxide is beneficial to the full dispersion in the adhesive; and the silicon-containing groups are converted into silicon dioxide, thereby realizing the full fusion of the zirconium oxide and the silicon dioxide.
According to the invention, the yttrium oxide is modified, so that the titanium-containing groups are grafted on the surface of the yttrium oxide, the introduction of the titanium-containing groups is favorable for realizing the sufficient mixing of the yttrium oxide and the adhesive, and meanwhile, the yttrium oxide and the zirconium oxide are also favorable for being sufficiently dispersed in the adhesive; and the titanium-containing groups 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 zirconia, 0.2 to 0.4 part of silicate, 10 to 20 parts of yttrium oxide, 0.1 to 0.2 part of titanate and 12 to 15 parts of adhesive.
According to some embodiments of the invention, the silicate is butyl orthosilicate.
According to some embodiments of the invention, the silicate-modified zirconia is prepared by a process comprising the steps of:
adding zirconia into 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 silicate-modified zirconia is prepared for a reaction time of 2 to 3 hours.
According to some embodiments of the invention, the silicate-modified zirconia is prepared at a reaction temperature of 35 ℃ to 45 ℃.
According to some embodiments of the invention, the mass to volume ratio of the zirconia to the aqueous ethanol solution is 1g:50 mL-100 mL.
According to some embodiments of the invention, the titanate is tetrabutyl titanate.
According to some embodiments of the invention, the method for preparing titanate-modified yttria 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:50 mL-100 mL.
According to some embodiments of the invention, the volume fraction of the aqueous ethanol solution is 95% to 99%.
According to some embodiments of the invention, the titanate-modified yttria is prepared for a reaction time of 2 to 3 hours.
According to some embodiments of the invention, the temperature of the reaction during the preparation of the titanate-modified yttria is from 35 ℃ to 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 to 2 parts of polyethylene glycol and 3 to 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 calcination temperature is 1000 ℃ to 1500 ℃.
According to some embodiments of the invention, the calcination time is 8-12 hours.
According to some embodiments of the invention, the calcination procedure is as follows:
the first temperature rise, the first heat preservation, the second temperature rise and the 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 950 ℃ to 1050 ℃.
According to some embodiments of the invention, the first incubation time is from 1.5h to 2.5h.
According to some embodiments of the invention, the second elevated temperature has a final temperature of 1350 ℃ to 1450 ℃.
According to some embodiments of the invention, the second incubation is at a soak temperature of 1350 ℃ to 1450 ℃.
According to some embodiments of the invention, the second incubation time 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 particle sizes of the zirconia and the yttria, the good grading of the yttria and the zirconia is realized, and the compactness between the zirconia and the zirconia is further improved, so that the wear resistance and the compactness 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 3-5 hours.
Detailed Description
The conception and the technical effects produced by the present invention will be clearly and completely described in conjunction with the embodiments below to fully understand the objects, features and effects of the present invention. It is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments, and that other embodiments obtained by those skilled in the art without inventive effort are within the scope of the present invention based on the embodiments of the present invention.
In the description of the present invention, the descriptions of the terms "one embodiment," "some embodiments," "illustrative embodiments," "examples," "specific examples," or "some examples," etc., mean 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, schematic representations of the above terms do not necessarily refer to the same embodiments or examples. 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 specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
In an embodiment of the invention, the zirconia is purchased from Ningbo Bei Gaer New Material Co., ltd, with the product number 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 Cork Utility sciences Co., ltd, and the particle size is 50nm, 100nm, 200nm and 500nm.
Example 1
The embodiment is a preparation method of a zirconia ceramic rod, which comprises the following steps:
s1, modifying raw materials:
preparation of silicate modified zirconia:
adding zirconium oxide into ethanol water solution (volume fraction is 99%, mass volume ratio of the zirconium oxide to the ethanol water solution is 1g:100 mL) to prepare a mixed system, and adding silicate (butyl orthosilicate) into the mixed system for reaction at 40 ℃ for 2h; after the reaction is completed, solid-liquid separation is carried out, and solid phases are collected to prepare silicate modified zirconia;
modifying yttrium oxide by titanate to obtain titanate modified yttrium oxide;
adding yttrium oxide into an ethanol water solution (the volume fraction is 99%, the mass volume ratio of the yttrium oxide to the ethanol water solution is 1g:100 mL) to prepare a mixed system, and then adding titanate (tetrabutyl titanate) into the mixed system for reaction, wherein the reaction temperature is 35 ℃ and the reaction time is 3h; after the reaction is completed, solid-liquid separation is carried out, and solid phase is collected to prepare titanate modified yttrium oxide;
s2, mixing:
mixing silicate modified zirconia, titanate modified yttria and an 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 obtain a blank;
drying the blank at 145 ℃ for 4 hours to obtain a dried blank;
calcining the dried blank; calcination was performed in a horizontal sintering furnace, and the calcination procedure was as follows:
firstly heating to 1000 ℃ (heating time is 1 h), and preserving heat for 2h at 1000 ℃;
heating to 1400 deg.c (with heating rate of 20 deg.c/min) and maintaining at 1400 deg.c for 6 hr.
The embodiment comprises the following preparation raw materials in parts by mass:
100 parts of zirconia, 0.3 part of silicate (butyl orthosilicate), 10 parts of yttrium oxide, 0.1 part of titanate and 15 parts of adhesive.
The adhesive in the embodiment comprises the following preparation raw materials in parts by weight:
10 parts of hydroxypropyl methylcellulose, 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, which differs from example 1 in that:
in this embodiment, the zirconia is B-ZrO 2 -1W(1μm)。
Example 3
This example is a method for preparing a zirconia ceramic rod, which differs from example 1 in that:
in this embodiment, the zirconia is B-ZrO 2 -5W(5μm)。
Example 4
This example is a method for preparing a zirconia ceramic rod, which differs from example 1 in that:
in this embodiment, the zirconia is B-ZrO 2 -200N(200nm)。
Example 5
This example is a method for preparing a zirconia ceramic rod, which differs 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, which differs from example 1 in that:
the particle size of the yttria in this example was 500nm.
Example 7
This example is a method for preparing a zirconia ceramic rod, which differs from example 1 in that:
the particle size of the yttria in this example was 50nm.
Comparative example 1
This comparative example is a method for producing a zirconia ceramic rod, which differs 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 producing a zirconia ceramic rod, which differs from example 1 in that:
the yttrium oxide in this comparative example was not subjected to titanate modification treatment.
Comparative example 3
This comparative example is a method for producing a zirconia ceramic rod, which differs from example 1 in that:
in this comparative example, zirconium oxide was not subjected to silicate modification treatment and yttrium oxide was not subjected to titanate modification treatment.
The performance test of the zirconia ceramic rods produced in examples 1 to 7 and comparative examples 1 to 3 of the present invention was referred to the following method:
compressive strength: JIS R1601-2008.
The results of the performance test of the zirconia ceramic rods produced in examples 1 to 7 of the present invention and comparative examples 1 to 3 are shown in Table 1.
TABLE 1 results of Performance test of zirconia ceramic bars produced in examples 1 to 7 and comparative examples 1 to 3 of the present invention
In summary, in the invention, the silicon-containing groups are grafted on the surface of the zirconia by carrying out silicate modification treatment on the zirconia, so that the introduction of the silicon-containing groups is beneficial to the full mixing of the zirconia and the adhesive, and meanwhile, the full dispersion of the zirconia in the adhesive is also beneficial to; and the silicon-containing groups are converted into silicon dioxide in the calcining process, so that the sufficient fusion of the zirconium oxide and the silicon dioxide is realized. According to the invention, the yttrium oxide is modified, so that the titanium-containing groups are grafted on the surface of the yttrium oxide, the introduction of the titanium-containing groups is favorable for realizing the sufficient mixing of the yttrium oxide and the adhesive, and meanwhile, the yttrium oxide and the zirconium oxide are also favorable for being sufficiently dispersed in the adhesive; and the titanium-containing groups are converted into titanium dioxide in the calcination 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 of the preferred embodiments of the present invention and is not intended to limit the present invention, and various modifications and variations can be made to the embodiments of the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
While the foregoing is directed to embodiments of the present invention, other and further details of the invention may be had by the present invention, it should be understood that the foregoing description is merely illustrative of the present invention and that no limitations are intended to the scope of the invention, except insofar as modifications, equivalents, improvements or modifications are within the spirit and principles of the invention.
Claims (6)
1. The preparation method of the zirconia ceramic rod is characterized by comprising the following steps:
s1, modifying zirconium oxide by silicate to obtain silicate modified zirconium oxide;
modifying yttrium oxide by titanate to obtain titanate modified yttrium oxide;
s2, mixing the silicate modified zirconia, the titanate modified yttrium oxide and an adhesive to prepare pugs;
s3, extruding the pug to obtain a blank;
calcining the blank;
the zirconia ceramic rod comprises the following preparation raw materials in parts by weight:
100 parts of zirconia, 0.2 to 0.4 part of silicate, 10 to 20 parts of yttrium oxide, 0.1 to 0.2 part of titanate and 12 to 15 parts of adhesive;
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;
the particle size of the zirconia is 500-1000 nm;
the particle size of the yttrium oxide is 100 nm-200 nm.
2. The method for producing a zirconia ceramic rod according to claim 1, wherein the silicate is butyl orthosilicate.
3. The method for preparing a zirconia ceramic rod according to claim 1, wherein the titanate is tetrabutyl titanate.
4. A method for producing a zirconia ceramic rod according to any one of claims 1 to 3, wherein the calcination temperature is 1000 ℃ to 1500 ℃.
5. The method for producing a zirconia ceramic rod according to any one of claims 1 to 3, wherein the calcination time is 8 to 12 hours.
6. A method of preparing a zirconia ceramic rod according to any one of claims 1 to 3 wherein the post extrusion drying is carried out at a temperature of 140 ℃ to 150 ℃.
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| 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 |
| 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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| FR2884510B1 (en) * | 2005-04-15 | 2007-06-22 | Saint Gobain Mat Constr Sas | FRITTE PRODUCT BASED ON ZIRCON |
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| 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 |
| 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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