CN101508588B - Composite high-temperature deck of high-performance mullite and spinel, and method of producing the same - Google Patents

Composite high-temperature deck of high-performance mullite and spinel, and method of producing the same Download PDF

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Publication number
CN101508588B
CN101508588B CN2009100961807A CN200910096180A CN101508588B CN 101508588 B CN101508588 B CN 101508588B CN 2009100961807 A CN2009100961807 A CN 2009100961807A CN 200910096180 A CN200910096180 A CN 200910096180A CN 101508588 B CN101508588 B CN 101508588B
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powder
particle
mullite
high temperature
spinel
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CN2009100961807A
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CN101508588A (en
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王家邦
王立旺
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Zhejiang University ZJU
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Zhejiang University ZJU
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Abstract

The invention discloses a high-performance mullite-spinelle composite high temperature board and a preparation method. The matrix comprises alpha-Al2O3 powder, sheet-shaped corundum powder, magnesium oxide powder and sillimanite powder; the aggregate comprises electrically fused mullite granules, sheet-shaped corundum granules and electrically fused spinelle granules; the matrix weighed by mixing proportion is firstly mixed in a ball mill, the aggregate weighed by mixing proportion is evenly mixed in a stirring mill and then added with a binding agent for stirring, and subsequently the evenlymixed matrix materials are added for stirring and airtight standing. The high-performance mullite-spinelle composite high temperature board is finally prepared by baking after pressing moulding on a vibration pressing machine and drying. The invention has outstanding high temperature resistance and thermal shock stability, the preparation is simple and convenient, the occupancy rate in the furnace space in use is low, the chemical performance is stable, the invention can directly contact with the products to be baked, and saggar and other kiln materials are no more necessary, so that space utility rate is enhanced, energy consumption is lowered and production efficiency is improved. The invention is mainly used in the aspect of high temperature sintering of magnetic iron oxide material in electronic devices and components industry.

Description

A kind of high-performance mullite and spinel combined high temperature refractory slab and preparation method thereof
Technical field
The present invention relates to refractory materials, relate in particular to a kind of high-performance mullite and spinel combined high temperature refractory slab and preparation method thereof.
Background technology
Refractory slab is the crucial kiln furnitures in the sintered magnetic material, shape mainly is lamellar, area is bigger, and thickness is less relatively, directly contacts flame in the use, not only bear certain pressure effect, but also to bear the cold cycling of repeated multiple times, require to have good normal temperature and hot strength, excellent anti-thermal shock stability and chemical stability, good thermal conductivity and low heat storing, refractory slab itself need that outward appearance is regular, size is accurate.Present widely used refractory slab material mainly contains cordierite, zirconium white matter, the siliceous and mullite of carbonization, cordierite refractory slab thermal shock resistance excellence, long service life, but use temperature is lower, generally be no more than 1400 ℃, can not satisfy the sintering condition of soft magnetic materials; The siliceous refractory slab of carbonization also has good thermal shock resistance, use temperature is also than cordierite height, but oxidation takes place under the hot conditions easily, can only in reducing atmosphere, use for a long time, and easily and hold the product generation chemical reaction of burning, cause product rejection, in order to improve the chemical stability of silicon carbide material, patent ZL200520102193.8 and ZL200620053416.0 adopt stratiform compound mode to improve preparation technology's more complicated; Zirconium white matter use temperature is higher, but expensive raw material price; The mullite refractory slab has excellent chemical stability, and use temperature is higher, but compares with cordierite and carbonization are siliceous, and some deficiency of heat-shock resistance is easy to generate cracking, and work-ing life is limited.
Summary of the invention
Problem and shortage at present high temperature refractory slab exists the object of the present invention is to provide a kind of high-performance mullite and spinel combined high temperature refractory slab and preparation method thereof.
The technical solution adopted for the present invention to solve the technical problems is as follows:
One, a kind of high-performance mullite and spinel combined high temperature refractory slab, the feed composition that is adopted proportioning by mass percentage is as follows:
Electrofused mullite particle 40~45%,
Plate diamond spar particle 15~20%,
Electric smelting spinel particle 8~12%,
α-Al 2O 3Powder 5~10%,
Plate diamond spar powder 5~10%,
Magnesia powder 5~8%,
Sillimanite powder 8~12%,
Adding the wedding agent silica-alumina gel is 3~4% of total amount.
Two, a kind of preparation method of high-performance mullite and spinel combined high temperature refractory slab:
Electrofused mullite particle 40~45%, plate diamond spar particle 15~20%, electric smelting spinel particle 8~12%, α-Al 2O 3Powder 5~10%, plate diamond spar powder 5~10%, magnesia powder 5~8%, sillimanite powder 8~12%, adding the wedding agent silica-alumina gel is 3~4% of total amount; The step of this method is as follows:
Matrix comprises α-Al 2O 3Powder, plate diamond spar powder, four kinds of powders of magnesia powder and sillimanite powder; Aggregate comprises the electrofused mullite particle, plate diamond spar particle and electric smelting spinel particle; Matrix was mixed in ball mill 2~3 hours earlier the back well by the proportioning weighing, and aggregate is pressed the proportioning weighing and evenly added the wedding agent stirring in the back in stirrer for mixing in the back well, adds the substrate material that mixes then, stirs 20~30 minutes; Airtight placement 24~30 hours; Compression moulding on the vibrations press; Under 1550~1580 ℃ of conditions, burn till after 110 ℃ of oven dry.
Described electrofused mullite particle and electric smelting spinel particle all are to comprise 1~1.5mm and be not more than two kinds of specifications of 1mm.
Described plate diamond spar particle comprises 0.5~1mm and is not more than two kinds of specifications of 0.5mm.
The globule size of described plate diamond spar powder and magnesia powder is no more than 325 orders.
Described sillimanite is that globule size is no more than 180 orders through cleanup acid treatment.
Described wedding agent is a silica-alumina gel, is to be that raw material adopts sol-gel technology preparing with silica gel and aluminium glue, and the solid content mass percent is 15~20%.
The present invention adopts plate diamond spar and the compound preparation high-performance of electric smelting spinel high temperature refractory slab, and electrofused mullite purity height, density is big, weave construction good, creep rate is low, thermal expansion is little, good thermal shock, and chemical resistance of concrete is strong; Electric smelting spinel fusing point height, thermal expansion is little, and thermal stresses is low, good thermal shock, stable chemical performance; Plate diamond spar is to adopt the sintering process preparation, has excellent chemical stability and resistance to elevated temperatures.The present invention is with Al 2O 3-SiO 2-MgO ternary phase diagrams is a theoretical foundation, adopts electrofused mullite, the refractory slab of plate diamond spar and the compound preparation excellent combination property of electric smelting spinel.
The present invention compares the beneficial effect that has with background technology:
Adopt electrofused mullite, plate diamond spar and the compound preparation of electric smelting spinel, with the silica-alumina gel is wedding agent, burn till through high temperature, the refractory slab that makes has outstanding high temperature resistance and anti-thermal shock stability, can be under 1530~1550 ℃ hot conditions life-time service, preparation process is simple, and low in the use in the kiln space occupancy, stable chemical performance can directly contact with the product that holds burning, no longer need to use other kiln furniture materials such as saggar, can improve space availability ratio, cut down the consumption of energy, greatly enhance productivity.The present invention is mainly used in electronic devices and components industry high temperature sintering magnetic ferrites material aspect.
Embodiment
Embodiment 1:
Feed composition proportioning by mass percentage is as follows:
Electrofused mullite particle 1~1.5mm 25%,
Electrofused mullite particle≤1mm 15%
Plate diamond spar particle≤0.5mm 5%
Plate diamond spar particle 0.5~1mm 15%,
Electric smelting spinel particle 1~1.5mm 8%,
Electric smelting spinel particle≤1mm 4%
α-Al 2O 3Powder 5%,
Plate diamond spar powder 10%,
Magnesia powder 5%,
Sillimanite powder 8%,
Adding the wedding agent silica-alumina gel is 3% of total amount.
The preparation method is: earlier the matrix material was put in the ball mill blend 2 hours by proportioning, in planetary stirring machine, add aggregate then by proportioning, stirring and evenly mixing, then adding wedding agent stirs, add the matrix material that mixes at last, stir discharging in 20 minutes, built back bundle material 24 hours with Plastic film Bag, insulation was burnt till in 4 hours under the firing temperature condition at 1580 ℃ after 110 ℃ of oven dry.
Embodiment 2:
Feed composition proportioning by mass percentage is as follows:
Electrofused mullite particle 1~1.5mm 30%,
Electrofused mullite particle≤1mm 15%
Plate diamond spar particle≤0.5mm 5
Plate diamond spar particle 0.5~1mm 10%,
Electric smelting spinel particle 1~1.5mm 4%,
Electric smelting spinel particle≤1mm 4%
α-Al 2O 3Powder 10%,
Plate diamond spar powder 5%,
Magnesia powder 8%,
Sillimanite powder 9%,
Adding the wedding agent silica-alumina gel is 4% of total amount.
The preparation method is: earlier the matrix material was put in the ball mill blend 3 hours by proportioning, in planetary stirring machine, add aggregate then by proportioning, stirring and evenly mixing, then adding wedding agent stirs, add the matrix material that mixes at last, stir discharging in 30 minutes, built back bundle material 30 hours with Plastic film Bag, insulation was burnt till in 6 hours under the firing temperature condition at 1550 ℃ after 110 ℃ of oven dry.
Embodiment 3:
Feed composition proportioning by mass percentage is as follows:
Electrofused mullite particle 1~1.5mm 30%,
Electrofused mullite particle≤1mm 15%
Plate diamond spar particle≤0.5mm 5%
Plate diamond spar particle 0.5~1mm 10%,
Electric smelting spinel particle 1~1.5mm 6%,
Electric smelting spinel particle≤1mm 4%
α-Al 2O 3Powder 5%,
Plate diamond spar powder 5%,
Magnesia powder 8%,
Sillimanite powder 12%,
Adding the wedding agent silica-alumina gel is 4% of total amount.
The preparation method is: earlier the matrix material was put in the ball mill blend 2 hours by proportioning, in planetary stirring machine, add aggregate then by proportioning, stirring and evenly mixing, then adding wedding agent stirs, add the matrix material that mixes at last, stir discharging in 25 minutes, built back bundle material 30 hours with Plastic film Bag, insulation was burnt till in 6 hours under the firing temperature condition at 1550 ℃ after 110 ℃ of oven dry.
Embodiment 4:
Electrofused mullite particle 1~1.5mm 32%,
Electrofused mullite particle≤1mm 10%
Plate diamond spar particle≤0.5mm 6%
Plate diamond spar particle 0.5~1mm 12%,
Electric smelting spinel particle 1~1.5mm 4%,
Electric smelting spinel particle≤1mm 6%
α-Al 2O 3Powder 8%,
Plate diamond spar powder 8%,
Magnesia powder 6%,
Sillimanite powder 8%,
Adding the wedding agent silica-alumina gel is 3% of total amount.
The preparation method is: earlier the matrix material was put in the ball mill blend 2 hours by proportioning, in planetary stirring machine, add aggregate then by proportioning, stirring and evenly mixing, then adding wedding agent stirs, add the matrix material that mixes at last, stir discharging in 30 minutes, built back bundle material 24 hours with Plastic film Bag, insulation was burnt till in 4 hours under the firing temperature condition at 1580 ℃ after 110 ℃ of oven dry.
Adopting the high temperature refractory slab fundamental property index of above embodiment preparation is volume density 2.6~2.9g/cm 3, void content 15~20%, strength at normal temperature 〉=13MPa, cold crushing strength 〉=100MPa, refractoriness under load 〉=1540 ℃ can reach 50 times 1500 ℃ conditions following work-ing life.

Claims (7)

1. a high-performance mullite and spinel combined high temperature refractory slab is characterized in that, the raw materials quality per-cent of employing is as follows:
Matrix comprises α-Al 2O 3Powder, plate diamond spar powder, four kinds of powders of magnesia powder and sillimanite powder; Aggregate comprises the electrofused mullite particle, plate diamond spar particle and electric smelting spinel particle; Matrix was mixed in ball mill 2~3 hours earlier the back well by the proportioning weighing, and aggregate is pressed the proportioning weighing and evenly added the wedding agent stirring in the back in stirrer for mixing in the back well, adds the substrate material that mixes then, stirs 20~30 minutes; Airtight placement 24~30 hours; Compression moulding on the vibrations press; Under 1550~1580 ℃ of conditions, burn till after 110 ℃ of oven dry.
2. the preparation method of a high-performance mullite and spinel combined high temperature refractory slab is characterized in that: electrofused mullite particle 40~45%, plate diamond spar particle 15~20%, electric smelting spinel particle 8~12%, α-Al 2O 3Powder 5~10%, plate diamond spar powder 5~10%, magnesia powder 5~8%, sillimanite powder 8~12%, adding the wedding agent silica-alumina gel is 3~4% of total amount; The step of this method is as follows:
Matrix comprises α-Al 2O 3Powder, plate diamond spar powder, four kinds of powders of magnesia powder and sillimanite powder; Aggregate comprises the electrofused mullite particle, plate diamond spar particle and electric smelting spinel particle; Matrix was mixed in ball mill 2~3 hours earlier the back well by the proportioning weighing, and aggregate is pressed the proportioning weighing and evenly added the wedding agent stirring in the back in stirrer for mixing in the back well, adds the substrate material that mixes then, stirs 20~30 minutes; Airtight placement 24~30 hours; Compression moulding on the vibrations press; Under 1550~1580 ℃ of conditions, burn till after 110 ℃ of oven dry.
3. the preparation method of a kind of high-performance mullite and spinel combined high temperature refractory slab according to claim 2 is characterized in that: described electrofused mullite particle and electric smelting spinel particle all are to comprise 1~1.5mm and be not more than two kinds of specifications of 1mm.
4. the preparation method of a kind of high-performance mullite and spinel combined high temperature refractory slab according to claim 2 is characterized in that: described plate diamond spar particle comprises 0.5~1mm and is not more than two kinds of specifications of 0.5mm.
5. the preparation method of a kind of high-performance mullite and spinel combined high temperature refractory slab according to claim 2 is characterized in that: the globule size of described plate diamond spar powder and magnesia powder is no more than 325 orders.
6. the preparation method of a kind of high-performance mullite and spinel combined high temperature refractory slab according to claim 2 is characterized in that: described sillimanite is that globule size is no more than 180 orders through cleanup acid treatment.
7. the preparation method of a kind of high-performance mullite and spinel combined high temperature refractory slab according to claim 2, it is characterized in that: described wedding agent is a silica-alumina gel, be to be that raw material adopts sol-gel technology preparing with silica gel and aluminium glue, the solid content mass percent is 15~20%.
CN2009100961807A 2009-02-19 2009-02-19 Composite high-temperature deck of high-performance mullite and spinel, and method of producing the same Expired - Fee Related CN101508588B (en)

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CN101955366B (en) * 2010-10-26 2012-07-04 揭东县热金宝新材料科技有限公司 High performance and large-area fire resistance hollow slab kiln and production method thereof
CN103482993A (en) * 2013-09-13 2014-01-01 湖南仁海科技材料发展有限公司 Adamantine spar and mullite composite material sagger and method for manufacturing sagger
CN113149620A (en) * 2021-03-24 2021-07-23 无锡尚臻新材料有限公司 Light mullite-spinel hollow sphere sagger pressurization forming process
CN113548884B (en) * 2021-08-04 2023-01-03 浙江吉昌新材料有限公司 Sagger containing cordierite and composite spinel mullite and preparation method thereof
CN113603469B (en) * 2021-08-04 2022-12-16 江苏晶邦新型材料有限公司 Composite spinel-mullite ceramic refractory material and preparation method thereof

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