CN105418164B - Surface coats the preparation method of the silicon carbide ceramics kiln furnitures of yttrium stable zirconium oxide coating - Google Patents

Surface coats the preparation method of the silicon carbide ceramics kiln furnitures of yttrium stable zirconium oxide coating Download PDF

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CN105418164B
CN105418164B CN201510762902.3A CN201510762902A CN105418164B CN 105418164 B CN105418164 B CN 105418164B CN 201510762902 A CN201510762902 A CN 201510762902A CN 105418164 B CN105418164 B CN 105418164B
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yttrium
silicon carbide
zirconium oxide
carbide ceramics
alcohol
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CN105418164A (en
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郭兴忠
宋杰
刘大明
徐生富
杨辉
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ANJI KELING MAGNETIC MATERIAL Co Ltd
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ANJI KELING MAGNETIC MATERIAL Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/50Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
    • C04B41/5025Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials with ceramic materials
    • C04B41/5042Zirconium oxides or zirconates; Hafnium oxides or hafnates
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/009After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/80After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
    • C04B41/81Coating or impregnation
    • C04B41/85Coating or impregnation with inorganic materials
    • C04B41/87Ceramics

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Compositions Of Oxide Ceramics (AREA)

Abstract

The invention discloses the preparation methods that a kind of surface coats the silicon carbide ceramics kiln furnitures of yttrium stable zirconium oxide coating, include the following steps:1), yttrium stable zirconium oxide colloidal sol is uniformly coated on to the surface of silicon carbide ceramics kiln furnitures blank by the way of spraying, to form coating;It is 5~7 hours dry in 45~55 DEG C of environment after spontaneously drying 2~3 hours;The yttrium stable zirconium oxide colloidal sol is the zirconia sol of the yttrium containing 3mol%, is prepared using sol-gal process;2) gains of step 1), are fired into 72~96h in 1450~1500 DEG C;Obtain product.Method using the present invention can improve the inoxidizability and high temperature resistance of silicon carbide ceramics kiln furnitures.

Description

Surface coats the preparation method of the silicon carbide ceramics kiln furnitures of yttrium stable zirconium oxide coating
Technical field
The present invention relates to a kind of preparation methods of silicon carbide ceramics kiln furnitures, are a kind of surface coating yttrium stabilizations specifically The preparation method of the oxidation resistant carbon SiClx ceramic kiln furniture of zirconia coating.
Background technology
Silicon carbide ceramics has high bending strength, superior corrosion resistance, high wear-resistant and low friction coefficient, Mechanical behavior under high temperature (intensity, creep resistance etc.), in oil, chemical industry, microelectronics, automobile, space flight, aviation, papermaking, laser, mine The industrial circles such as industry and atomic energy have been widely used.Nearly ten years, silicon carbide ceramics is as a kind of advanced high temperature pottery Porcelain kiln tool is increasingly used in the kiln of each industrial circle, is especially rapidly fired to kiln.As a kind of refractory material, high temperature The quality of kiln furnitures has direct influence to the quality production cost of burnt product, it is desirable that has higher refractoriness, good Good thermal stability and chemical stability, higher room temperature and elevated temperature strength, it is necessary to the load of product and kiln furnitures itself is withstood, Good thermal conductivity, low heat storing and antioxygenic property.Silicon carbide Hightemperature Kiln Furniture with its excellent high-temperature behavior, fire resistance with And thermal shock resistance can apply in high temperature rapid firing stove, and kiln production capacity can be improved, and energy consumption be greatly lowered, and effectively reduce and hold Burned product such as deforms, is scaling-off at the firing defects, it has also become indispensable in the Industrial Stoves and larger kiln furniture material of consumption it One.
However, though silicon carbide kiln furnitures have certain blunt oxidation characteristic, its antioxygenic property under high-temperature low-oxygen It is poor, it is easily aoxidized during high temperature prolonged use, so that kiln furniture material vitrifying and formation christobalite, cause Its volume swells, deforms, and becomes fragile, slag, and causes crackle, even cracks, and thermal shock resistance also decreases, and limits in fact Border service life, and directly affect the performance held and burn ceramic.So the inoxidizability for improving silicon carbide kiln furniture has become this The emphasis and hot spot of kiln furniture material research and development.
In coating material, zirconia coating is a kind of high temperature-resistant coating material, due to ZrO2The Gao Rong of substance itself Point does not aoxidize and other high temperature good characteristics, the inoxidizability, high temperature resistant and durability of component can be significantly improved, using wide It is general.After yttrium stabilizer is added, the Phase Transformation of Zirconia that room temperature can be made unstable is stable or metastable state zirconium oxide.
But currently, there has been no using yttrium stable zirconium oxide colloidal sol as coating material, prepare anti-oxidant silicon carbide ceramics The relevant report of kiln furnitures.
Invention content
The technical problem to be solved in the present invention is to provide the silicon carbide ceramics that a kind of surface coats yttrium stable zirconium oxide coating The preparation method of kiln furnitures, method using the present invention can improve the inoxidizability and high temperature resistance of silicon carbide ceramics kiln furnitures.
In order to solve the above technical problem, the present invention provides the silicon carbide potteries that a kind of surface coats yttrium stable zirconium oxide coating The preparation method of porcelain kiln tool, includes the following steps:
1), yttrium stable zirconium oxide colloidal sol is uniformly coated on to the table of silicon carbide ceramics kiln furnitures blank by the way of spraying Face, to form coating;It is 5~7 hours dry in 45~55 DEG C of (50 DEG C or so) environment after spontaneously drying 2~3 hours (preferably 6 hours);
The yttrium stable zirconium oxide colloidal sol is the zirconia sol of the yttrium containing 3mol%, using sol-gel method preparation ;
Remarks explanation:The solid phase mass content of the yttrium-stabile zirconium dioxide colloidal sol is about 10~20%;
2) gains of step 1), are fired 72~96h in 1450~1500 DEG C (such as to burn in shuttle kiln System);Obtain product.
Surface as the present invention coats the improvement of the preparation method of the silicon carbide ceramics kiln furnitures of yttrium stable zirconium oxide coating: The preparation method (sol-gel method) of the zirconia sol of the yttrium containing 3mol% is:
By yttrium chloride and zirconium oxychloride according to 3:100 molar ratio mixing after, be dissolved in alcohol/aqueous mixtures be made it is transparent molten The amount ratio of the sum of weight of liquid, the yttrium chloride and zirconium oxychloride and alcohol/aqueous mixtures is 35.5g/100ml;Alcohol/the water The volumetric concentration of alcohol is 75% in mixture;
Then hydrogen peroxide is added and stirs 2h, to form mixed solution;The molar ratio of hydrogen peroxide and zirconium oxychloride is 5:1,
The ammonium hydroxide of 1.0mol/L and quickly stirring (speed of agitator is 500~1000 turns) are slowly added dropwise into mixed solution, Until the pH of mixed solution is 8-9;
To form the zirconia sol (that is, transparent yttrium stable zirconium oxide colloidal sol of 3mol% yttriums) of the yttrium containing 3mol%.
Remarks explanation:Hydrogen peroxide is obtained by form purchased in market, and a concentration of 27.5%~35%.
Surface as the present invention coat the preparation method of the silicon carbide ceramics kiln furnitures of yttrium stable zirconium oxide coating into one Step is improved:The alcohol is ethyl alcohol.
Surface as the present invention coat the preparation method of the silicon carbide ceramics kiln furnitures of yttrium stable zirconium oxide coating into one Step is improved:The thickness of coating in the step 1) is 0.5~2mm (being, for example, 1.5mm).
In the present invention, the preparation method of silicon carbide ceramics kiln furnitures blank is:
By silicon-carbide particle, silicon powder, starch according to 87:10:3 mass ratio mixing after in batch mixer wet mixing 0.5~2 Hour, 24 hours aftershapings of the mixture ageing mixture of gained (placing at room temperature) are made silicon carbide green body, briquetting pressure 120~ 160MPa;It is again that silicon carbide green body is 6 hours dry in 40~60 DEG C of environment, obtain silicon carbide ceramics kiln furnitures blank.
Remarks explanation:The preparation method of above-mentioned silicon carbide ceramics kiln furnitures blank belongs to routine techniques;The grain of silicon-carbide particle Diameter is 1~2mm, and the average grain diameter of silicon powder is 0.5 μm.
The oxidation resistant carbon SiClx ceramic kiln furniture production method of the present invention is inventor by long-term experiment, conscientious research institute It obtains.The technological merit of the present invention is the synthesis excellent properties for making full use of yttrium-stabile zirconium dioxide in ceramic applications.Yttrium After stabilised zirconia colloidal sol film forming, the yttrium-stabile zirconium dioxide nano-particle fusing point that is decomposed to form at high temperature is higher, object is mutually stablized, can Improve the inoxidizability and high temperature resistance of product.
The present invention coats one layer of yttrium stable zirconium oxide coating on silicon carbide ceramics kiln furnitures surface, improves silicon carbide ceramics kiln furnitures Antioxygenic property (mainly related with thermal shock resistance) and high temperature resistance.That is, invention further improves previous carbonizations Silicon ceramic kiln furniture product not resistance to oxidation the shortcomings that, substantially increase its service life.And present invention discover that different yttrium Stable Oxygen Change performance different from of the zirconium colloidal sol to the present invention.The silicon carbide ceramics kiln furniture product of method production using the present invention, can use In push plate, refractory slab, load bearing board, saggar etc., it can also be used to building materials, Ferrous Metallurgy etc..
Specific implementation mode
Embodiment 1, a kind of surface coat the preparation method of the silicon carbide ceramics kiln furnitures of yttrium stable zirconium oxide coating (that is, carbon The method that SiClx ceramic kiln furniture surface coats yttrium stable zirconium oxide coating coats one layer of yttrium on silicon carbide ceramics kiln furnitures surface and stablizes Zirconia coating), processing step is as follows:
1), 1~2mm of grain size silicon-carbide particles, average grain diameter 0.5 μm of silicon powder, starch are according to 87:10:3 mass ratio is mixed After conjunction in batch mixer wet mixing 2 hours, silicon carbide base is made in the aftershaping of mixture ageing mixture 24 hours (briquetting pressure 160MPa) Body, the silicon carbide green body are placed in 50 DEG C or so environment 6 hours dry;Silicon carbide ceramics kiln furnitures blank is obtained (for 15 cm x 15 The thin plate that 2 centimetres of cm x).
2), by yttrium stable zirconium oxide colloidal sol even application in kiln furnitures (that is, the silicon carbide ceramics kiln furnitures hair obtained by step 1) Embryo) surface, coating layer thickness 1.5mm;After spontaneously drying 2 hours, then it is placed in 50 DEG C or so environment 6 hours dry;
The yttrium stable zirconium oxide colloidal sol is the zirconia sol of the yttrium containing 3mol%, is prepared using sol-gel method;Its Preparation method is:
By yttrium chloride and zirconium oxychloride according to 3:100 molar ratio mixing after, be dissolved in alcohol/aqueous mixtures be made it is transparent molten The amount ratio of the sum of weight of liquid, yttrium chloride and zirconium oxychloride and alcohol/aqueous mixtures is 35.5g/100ml;The alcohol/water mixing The volumetric concentration of alcohol is 75% in object;The alcohol is ethyl alcohol;
Then hydrogen peroxide is added and stirs 2h, to form mixed solution;The molar ratio of hydrogen peroxide and zirconium oxychloride is 5:1;
The ammonium hydroxide of 1.0mol/L and quickly stirring (speed of agitator is 500~1000 turns) are slowly added dropwise into mixed solution, Until the PH of mixed solution is 8-9;
To form the transparent yttrium stable zirconium oxide colloidal sol of 3mol% yttriums, the solid phase quality of the yttrium-stabile zirconium dioxide colloidal sol Content is about 10%.
3), the sample (that is, gains of step 2)) after coating is placed in shuttle kiln, is fired 4 days in 1450 DEG C (96h), obtains product.
The refractoriness of product is up to 1750 DEG C, and for thermal shock resistance (1100 DEG C × 20min, air-cooled) more than 61 times, high temperature is anti- It rolls over (1400 DEG C × 0.5h) of intensity and is more than 30MPa.
Comparative example 1, a kind of preparation method for the silicon carbide ceramics kiln furnitures being not coated by any coating, that is, cancel in embodiment 1 Step 2) spraying process.Remaining is equal to embodiment 1.
The refractoriness of the product of gained is 1650 DEG C, and (1100 DEG C × 20min, air-cooled) of thermal shock resistance is no more than 50 times, (1400 DEG C × 0.5h) of high temperature break resistant intensity is less than 25MPa.
Comparative example 2 makes " zirconia coating of the yttrium containing 3mol% " in embodiment 1 into " the dioxy of the yttrium containing 8mol% Change zirconium coating ", that is, in the preparation method of colloidal sol, by " molar ratio of yttrium chloride and zirconium oxychloride " by " 3:100 " make " 8 into: 100”;The amount ratio of the sum of weight of the yttrium chloride and zirconium oxychloride and alcohol/aqueous mixtures is 39g/100ml;Remaining is equivalent In embodiment 1.
For the refractoriness of the product of gained up to 1700 DEG C, (1100 DEG C × 20min, air-cooled) of thermal shock resistance is no more than 50 Secondary, (1400 DEG C × 0.5h) of high temperature break resistant intensity is less than 28MPa.
Comparative example 3 makes the preparation method of the colloidal sol in embodiment 1 into following content:Yttrium chloride and zirconium oxychloride are pressed According to 3:After 100 molar ratio mixing, it is dissolved in alcohol/aqueous mixtures (75% ethyl alcohol) and clear solution, the yttrium chloride and oxygen is made The amount ratio of the sum of weight of zirconium chloride and alcohol/aqueous mixtures is 35.5g/80ml;Then hydrogen peroxide is added and stirs 2h, to shape At mixed solution;The molar ratio of hydrogen peroxide and zirconium oxychloride is 5:1;The ammonium hydroxide of 1.0mol/L is slowly added dropwise into mixed solution simultaneously Quickly stirring (speed of agitator is 500~1000 turns), until the PH of mixed solution is 8-9;To form the transparent of 3mol% yttriums The solid phase mass content of yttrium stable zirconium oxide colloidal sol, the yttrium-stabile zirconium dioxide colloidal sol is about 30%.
Remaining is equal to embodiment 1.
The refractoriness of the product of gained is no more than 1700 DEG C, and (1100 DEG C × 20min, air-cooled) of thermal shock resistance is no more than 45 Secondary, (1400 DEG C × 0.5h) of high temperature break resistant intensity is less than 30MPa.
Finally, it should also be noted that it is listed above be only the present invention several specific embodiments.Obviously, this hair Bright to be not limited to above example, acceptable there are many deformations.Those skilled in the art can be from present disclosure All deformations for directly exporting or associating, are considered as protection scope of the present invention.

Claims (2)

1. surface coats the preparation method of the silicon carbide ceramics kiln furnitures of yttrium stable zirconium oxide coating, it is characterized in that including following step Suddenly:
1), yttrium stable zirconium oxide colloidal sol is uniformly coated on to the surface of silicon carbide ceramics kiln furnitures blank by the way of spraying, To form coating, the thickness of coating is 0.5~2mm;After spontaneously drying 2~3 hours, dry 5 in 45~55 DEG C of environment ~7 hours;
The yttrium stable zirconium oxide colloidal sol is the zirconia sol of the yttrium containing 3mol%, is prepared using sol-gel method;
The preparation method of the zirconia sol of the yttrium containing 3mol% is:
By yttrium chloride and zirconium oxychloride according to 3:After 100 molar ratio mixing, it is dissolved in alcohol/aqueous mixtures and clear solution is made, institute The amount ratio for stating the sum of weight of yttrium chloride and zirconium oxychloride and alcohol/aqueous mixtures is 35.5g/100ml;The alcohol/water mixing The volumetric concentration of alcohol is 75% in object;
Then hydrogen peroxide is added and stirs 2h, to form mixed solution;The molar ratio of hydrogen peroxide and zirconium oxychloride is 5:1,
The ammonium hydroxide of 1.0mol/L is slowly added dropwise into mixed solution and quickly stirs, until the pH of mixed solution is 8-9;
To form the zirconia sol of the yttrium containing 3mol%;
2) gains of step 1), are fired into 72~96h in 1450~1500 DEG C;Obtain product.
2. the preparation method of the silicon carbide ceramics kiln furnitures of coating yttrium stable zirconium oxide coating in surface according to claim 1, It is characterized in that:The alcohol is ethyl alcohol.
CN201510762902.3A 2015-11-11 2015-11-11 Surface coats the preparation method of the silicon carbide ceramics kiln furnitures of yttrium stable zirconium oxide coating Active CN105418164B (en)

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CN109133955A (en) * 2017-06-19 2019-01-04 济南瑰宝新材料有限公司 A kind of Zirconium oxide fibre toughened zirconium oxide ceramic material and preparation method thereof
CN109305815A (en) * 2018-12-12 2019-02-05 雅安远创陶瓷有限责任公司 A kind of high intensity, porous ceramic and its preparation process
CN111825477B (en) * 2020-08-13 2022-05-10 中钢南京环境工程技术研究院有限公司 Preparation method of anti-oxidation silicon carbide kiln furniture
CN113185326A (en) * 2021-04-02 2021-07-30 武汉科技大学 Kiln furniture spray coating for roasting lithium battery anode material and preparation method thereof
CN113801581B (en) * 2021-09-18 2023-01-24 中国民航大学 Preparation method of high-temperature adhesive special for zirconia ceramics and titanium-based alloy
CN114085081B (en) * 2021-10-27 2022-10-21 南通三责精密陶瓷有限公司 Silicon carbide kiln furniture and manufacturing method thereof

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CN1069846C (en) * 1994-03-28 2001-08-22 中国科学技术大学 Sol-gel method for preparing yttrium oxide blended zirconium oxide ceramic micro filter film
CA2504831C (en) * 2005-04-21 2010-10-19 Standard Aero Limited Wear resistant ceramic composite coatings and process for production thereof
CN1865190A (en) * 2006-06-01 2006-11-22 上海新业喷涂机械有限公司 Zirconia/silicon carbide composite nano powder for hot spraying and its production method
CN101704671B (en) * 2009-11-27 2012-02-08 清华大学 Method for preparing black zirconia ceramics at low temperature

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Denomination of invention: Preparation method of silicon carbide ceramic kiln furniture coated with yttrium stabilized zirconia coating on the surface

Effective date of registration: 20231204

Granted publication date: 20180727

Pledgee: Zhejiang Anji Rural Commercial Bank Co.,Ltd. Xiaoyuan Branch

Pledgor: ANJI KELING MAGNETIC MATERIAL Co.,Ltd.

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