CN1171827C - Method for making aluminium oxide ceramic products - Google Patents
Method for making aluminium oxide ceramic products Download PDFInfo
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- CN1171827C CN1171827C CNB021121338A CN02112133A CN1171827C CN 1171827 C CN1171827 C CN 1171827C CN B021121338 A CNB021121338 A CN B021121338A CN 02112133 A CN02112133 A CN 02112133A CN 1171827 C CN1171827 C CN 1171827C
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Abstract
The present invention relates to a method for making alumina ceramic products. Alpha-alumina (alpha-Al2O3) is used as base material, and magnesium oxide, cobalt oxide, chromium oxide, etc. are used as auxiliary materials. The materials are treated, molded though compaction, sintered and polished. The method is characterized in that high-temperature chemical polishing and coloring technology is adopted in the polishing procedure, and the technology comprises two steps: firstly, water solution of a mixture of iron trichloride and chromic acid is dripped on sintered alumina ceramic at high temperature in oxidizing atmosphere; secondly, water solution of sodium borate is dripped on the alumina ceramic treated in the first step at high temperature in oxidizing atmosphere. Compared with the prior art, the technical process is simple, and the product has the advantages of beautiful and smooth appearance, uniform and bright color, favorable chemical and physical properties, stable quality and high product qualified rate. The product is suitable for the production of wire guiding rings in fishing tackle industry and yarn guides in textile industry.
Description
Technical Field
The invention relates to a method for manufacturing an alumina ceramic product.
Background
The alumina ceramic has the characteristics of stable chemical property, good mechanical strength, wear resistance and high hardness in high-temperature oxide. The guide wire ring and guide wire pin in the products of fishing gear industry are used as the key parts of the line passing and protecting of fishing rod winder, and the guide wire used in chemical fiber industry is required to have high hardness, high strength, high heat conductivity, high wear resistance, low friction coefficient or smooth surface due to the particularity of the use conditions. Under the traditional process conditions, the alumina porcelain basically meets the required mechanical property requirements, but the subsequent processing of the porcelain, particularly the polishing of the product, is labor and time consuming, and is difficult to meet the requirements on the appearance of the product, low friction coefficient and low wire and line abrasion in the use process. For example, chinese patent No. 00134357.2, which adopts hot press molding, and the product is polished by mechanical polishing and manual polishing. The mechanical polishing is divided into rough polishing and fine polishing because silicon carbide with different specifications is used for polishing in a vibration polishing machine; the manual polishing is finished by sequentially adopting 150-mesh and 320-mesh iron abrasive cloths, and the fine cloth is dipped with the grinding paste for final fine polishing. The processing procedures are very complicated, the product has poor finishing effect, the requirements of surface roughness and appearance cannot be met, the product quality is not easy to be stable, and the individual difference is large.
Disclosure of Invention
The invention aims to provide a method for manufacturing alumina ceramic products with simple process, beautiful and smooth appearance, uniform and bright color and excellent chemical and physical properties aiming at the current situation of the prior art.
The technical scheme adopted by the invention to achieve the aim is as follows:the alumina ceramic product is made with α -alumina (α -Al)2O3) The base material is 85-98% of the raw material, the rest is auxiliary material, and magnesium oxide (MgO), cobalt oxide (CoO), chromium oxide (Cr)2O3) Iridium sesquioxide (Y)2O3) Manganese dioxide (MnO)2) Vanadium pentoxide (V)2O5) At least one of the materials is auxiliary material, the manufacturing process comprises the procedures of raw material treatment, compaction forming, sintering to form porcelain and polishing, and the polishing process is characterized by comprising a high-temperature chemical polishing and coloring process, and the process comprises two steps:
a. dropwise adding ferric trichloride (FeCl) to the sintered alumina ceramic under the oxidizing atmosphere and at the controlled temperature of 800-860 DEG C3) With chromic acid (CrO)3) The mass percentage (%) of the aqueous solution of the mixture is as follows:
ferric chloride (FeCl)3) 15～25
Chromic acid (CrO)3) 5～15
Balance of water
b. Dripping sodium tetraborate (Na) on the alumina ceramic treated by the previous step under the oxidizing atmosphere and at the controlled temperature of 920-2B4O7.10H2O), sodium tetraborate (Na)2B4O7.10H2O) is less than 2 percent by mass.
In the high-temperature chemical polishing and coloring process, the treatment time of the aqueous solution of the mixture of ferric trichloride and chromic acid is 10-20 minutes, and sodium tetraborate (Na) is used2B4O7.10H2O) the time for treating the water solution is 3-5 minutes;
the auxiliary materials are magnesium oxide (MgO), cobalt oxide (CoO) and chromium oxide (Cr)2O3)；
The raw material treatment process adopts a wet-method blind-area-free 3D vibration mill;
the raw material processing procedure is characterized in that the proportion of the grinding material to the ball stone to the alcohol is 1: 2: 0.5;
80% of the powder treated by the raw material treatment process has the granularity of less than 0.5 micron;
the compaction molding process adopts dry compaction molding, and the molding pressure is 1200-1500 Kg/cm2；
The sintering temperature is 1520-1570 ℃, the sintering time is 2.5-3.5 hours, the heating rate is 90-110 ℃/hour, and the cooling rate is 40-60 ℃/hour.
In the invention, the industrial alcohol is used as a medium for the treatment of the raw materials, and the wet-process non-blind-area 3D vibration mill is adopted, so that the refined materials are prevented from agglomerating and coarsening, the particle size distribution of the powder can be controlled, the particle size of 80 percent of the powder can be ensured to be less than 0.5 micron, and the raw materials are uniformly stirred. Mixing the ultrafine crushed powder with a certain proportion of binder by industrial alcohol, uniformly mixing, sieving with a 40-60 mesh sieve, and then selecting particles at 1200-1500 Kg/cm2And (4) dry pressing and forming under pressure. Compared with hot-press molding, the dry-press molding has high production efficiency, low sintering shrinkage rate of products, difficult deformation and favorable control of size and shape precision, and the dry-press process does not need a drying procedure, so that the molded blank has enough strength, the damage of inter-procedure transportation can be reduced, and the qualification rate of finished products is improved; the compact body can also provide guarantee for subsequent processing. In addition, the superfine crushed material has increased specific surface area and activity, and the added supplementary material can make the crystal lattice of the product malformed or defected, and this is favorable to promoting sintering.
The alumina product does not generate liquid phase in the sintering process, and the sintering is completed through the reaction between phases. The melting point of alumina is 2050 ℃, but when other oxides are introduced therein, the temperature at which the liquid phase occurs decreases. The sintering temperature is controlled to be 0.8 times of the liquid phase appearance temperature in the production. The sintering temperature is too high, and crystal grains are easy to grow up to make the crystal grains thicker. By controlling proper sintering temperature, the microcrystal sinter can be obtained, so that the product has excellent mechanical property indexes. The heating rate is too high, the cracking and deformation of the blank are easily caused, and the qualification rate of the finished product is reduced. If the cooling rate is too high and the cooling is too fast, internal stress exists in the product, microcracks are easy to generate, and the strength of the product is damaged. The proper sintering temperature curve can reduce the porosity of the product, obtain a high-density product and ensure that the product has high strength and high hardness.
In the invention, after the sintered ceramic piece is mechanically polished, the high-temperature chemical polishing and coloring process is adopted, and the surface of the ceramic piece forms a layer of metal compound film and presents different color effects due to the following chemical reaction in a high-temperature polishing furnace under the proper atmosphere and temperature conditions.
Iron ion (Fe)3+) The color of pearl is as follows:
chromium ion (Cr)3+) And (3) green color:
cobalt ion (Co)2+) The appearance of a smoky gray color:
further, tin ion (Sn)4+) Antimony ion (Sb)3+) An olive color is presented.
The reaction is carried out at 800-860 ℃ to form Fe2O3·Al2O3、Cr2O3·Al2O3、Co2O3·Al2O3And (3) thin films of the compounds. In order to prevent the formed film from falling off, it is critical to control the reaction temperature and the reaction time. The reaction time is too long, the film is too thick, and the surface hardness and the wear resistance of the product are influenced. The borax is added to adsorb and separate excessive metal oxides on the surface of the product and oxides formed in the reaction furnace, and a small amount of B remains2O3The compound can endow the product with strong metal feeling and increase the texture of the product.
Compared with the prior art, the invention has simple process and high production efficiency; the product has beautiful and smooth appearance and uniform and bright color; the water absorption rate can reach below 0.03%, the surface friction coefficient can reach below 0.02, the quality is stable, and the qualification rate of finished products is high.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
The present invention will be described in further detail with reference to examples.
Example one
The embodiment takes a wire loop in the fishing gear industry as an example, and the specific manufacturing method is as follows:
by calcining α -alumina (α -Al)2O3) As base material, magnesium oxide (MgO), cobalt oxide (CoO), chromium oxide (Cr)2O3) And 5% of auxiliary materials are added into a 3D non-blind area vibration mill, industrial alcohol is used as a medium, the proportion of the grinding materials is 1: 2: 0.5, the superfine vibration mill is used for about 10 hours, the particle size distribution of the powder is controlled, the particle size of 80% of the powder is ensured to be less than 0.5 micron, and the powder is uniformly stirred.
Adding 3-5% of adhesive into the superfine powder for granulation, uniformly mixing, sieving by a 60-mesh sieve, and then sieving at 1500Kg/cm2And (3) dry pressing and forming under pressure.
And (3) placing the dried and pressed blank into a sintering furnace, controlling the atmosphere in the furnace to be a nearly neutral reducing atmosphere, raising the temperature in the furnace to 1550 ℃ at a heating rate of 100 ℃/h, sintering for 3 hours, then reducing the temperature in the furnace to be nearly room temperature at a cooling rate of 50 ℃/h, and taking the sintered ceramic piece out of the furnace for later use.
After the porcelain piece is mechanically finished by a vibration grinding machine, a centrifugal polishing machine and other equipment, the porcelain piece is placed in a high-temperature polishing furnace, the oxidizing atmosphere in the furnace is controlled, the temperature is about 830 ℃, and an aqueous solution of a mixture of ferric trichloride and chromic acid is dripped on the porcelain piece in the furnace, wherein the aqueous solution is prepared from the following components in percentage by weight: ferric chloride (FeCl)3) Chromic acid (CrO)3) 17 percent of water, 7 percent of water and 76 percent of water (mass percentage) and dropping for about 15 minutes; then the temperature in the furnace is raised to 970 DEGDropping borax water solution at about 1.8% concentration for 4 min to obtain the final product.
The finished product is detected by the national cultural and cultural relics standardized quality detection center according to the Q/HB 050.1-2001 standard, and the performance verification test results are shown in the following table 1.
And (3) testing the name of the part: (fishing gear) alumina porcelain ring
Table 1 performance verification test results:
| detecting items | Unit of measurement | Technical requirements | Measured data | Remarks for note |
| Appearance requirements | Standard 4.1.1-4.1.2 | Conform to | ||
| Surface roughness | μm | Rα≤0.4 | ＜0.2 | |
| Coefficient of sliding friction | ≤0.04 | ＜0.02 | ||
| Hardness of | N/mm2 | ≥12000 | ＞12000 | |
| Thermal conductivity | W/m·K | ≥10 | ＞10 | |
| Density of | g/cm3 | ≤4 | ＜3.8 | |
| Bending strength | Mpa | ≥250 | ＞250 | |
| Rate of wear | g/Kg·h | 0.4～0.6 | Conform to | |
| Water absorption rate | ％ | ≤0.35 | ＜0.35 | |
| Resistance to rapid change of temperature | Standard 4.10 strips | Conform to | ||
| Detection and identification conclusion | The product performance reaches the standard through verification and test. | |||
Claims (8)
1. A process for preparing ceramic products of alumina from α -alumina (α -Al)2O3) The base material is 85-98% of the raw material, the rest is auxiliary material, and magnesium oxide (MgO), cobalt oxide (CoO), chromium oxide (Cr)2O3) Iridium sesquioxide (Y)2O3) Manganese dioxide (MnO)2) Vanadium pentoxide (V)2O5) At least one of the materials is auxiliary material, the manufacturing process comprises the procedures of raw material treatment, compaction forming, sintering to form porcelain and polishing, and the polishing process is characterized by comprising a high-temperature chemical polishing and coloring process, and the process comprises two steps:
a. dropwise adding ferric trichloride (FeCl) to the sintered alumina ceramic under the oxidizing atmosphere and at the controlled temperature of 800-860 DEG C3) With chromic acid (CrO)3) The mass percentage (%) of the aqueous solution of the mixture is as follows:
ferric chloride (FeCl)3) 15～25
Chromic acid (CrO)3) 5～15
Balance of water
b. Dripping sodium tetraborate (Na) on the alumina ceramic treated by the previous step under the oxidizing atmosphere and at the controlled temperature of 920-2B4O7.10H2O), sodium tetraborate (Na)2B4O7.10H2O) is less than 2 percent by mass.
2. The method of claim 1, wherein the high temperature chemical polishing coloring process comprises treating with an aqueous solution of a mixture of ferric trichloride and chromic acid for 10-20 min, and treating with sodium tetraborate (Na)2B4O7.10H2O) is treated with the aqueous solution for 3 to 5 minutes.
3. The method of claim 1 or 2, wherein the auxiliary materials are magnesium oxide (MgO), cobalt oxide (CoO) and chromium oxide (Cr)2O3)。
4. The method of manufacturing an alumina ceramic article according to claim 1, wherein the raw materialtreatment process employs a wet non-blind zone 3D vibration mill.
5. The method of claim 1, wherein the raw material processing step comprises the steps of mixing the abrasive material in a ratio of powder, spherulite and alcohol of 1: 2: 0.5.
6. The method of manufacturing an alumina ceramic article according to claim 1, 4 or 5, wherein 80% of the powder treated in the raw material treatment process has a particle size of less than 0.5 μm.
7. The method for manufacturing the alumina ceramic product according to claim 1, wherein the compacting and forming process adopts dry compacting and forming, and the forming pressure is 1200 to 1500Kg/cm2。
8. The method of claim 1, wherein the sintering temperature is 1520 to 1570 ℃, the sintering time is 2.5 to 3.5 hours, the temperature rising rate is 90 to 110 ℃/hour, and the cooling rate is 40 to 60 ℃/hour.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB021121338A CN1171827C (en) | 2002-06-18 | 2002-06-18 | Method for making aluminium oxide ceramic products |
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| CNB021121338A CN1171827C (en) | 2002-06-18 | 2002-06-18 | Method for making aluminium oxide ceramic products |
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| CN1171827C true CN1171827C (en) | 2004-10-20 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101318833B (en) * | 2008-07-18 | 2012-05-30 | 哈尔滨工业大学 | Surface preoxidizing method for boride based ceramic material |
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| CN100335441C (en) * | 2003-06-14 | 2007-09-05 | 宜兴市法兰特工贸有限公司 | Ceramic valve plate for double gate valve |
| CN1326800C (en) * | 2005-07-08 | 2007-07-18 | 清华大学 | Nano Co-Ni-Al2O3 composite ceramic material and its preparation method |
| US8283271B2 (en) * | 2008-10-31 | 2012-10-09 | Saint-Gobain Ceramics & Plastics, Inc. | High strength proppants |
| CN101628806B (en) * | 2009-08-05 | 2012-06-27 | 郑州九环科贸有限公司 | Nanometer composite ceramic lining material and preparation method thereof |
| CN102153335B (en) * | 2011-04-02 | 2013-01-16 | 西南科技大学 | Machinable aluminium oxide ceramics and preparation method of machinable aluminium oxide ceramics |
| CN103478092A (en) * | 2012-06-15 | 2014-01-01 | 苏州市京伦陶瓷有限公司 | Method for machining two-transverse-plane ceramic ring of fishing tool |
| CN108585814A (en) * | 2018-02-26 | 2018-09-28 | 合肥尚强电气科技有限公司 | A kind of piezo-electric ceramic composite material and preparation method thereof |
| CN114988918B (en) * | 2022-06-13 | 2023-04-07 | 湖南省新化县鑫星电子陶瓷有限责任公司 | Surface metallization method of alumina ceramic |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101318833B (en) * | 2008-07-18 | 2012-05-30 | 哈尔滨工业大学 | Surface preoxidizing method for boride based ceramic material |
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