CN1106565C - Kiln furniture made of sic and the process for production thereof - Google Patents

Kiln furniture made of sic and the process for production thereof Download PDF

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Publication number
CN1106565C
CN1106565C CN95103594A CN95103594A CN1106565C CN 1106565 C CN1106565 C CN 1106565C CN 95103594 A CN95103594 A CN 95103594A CN 95103594 A CN95103594 A CN 95103594A CN 1106565 C CN1106565 C CN 1106565C
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sic
weight
powder
kiln furniture
respect
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CN1125840A (en
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白川浩
山川治
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NGK Insulators Ltd
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NGK Insulators Ltd
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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
    • C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/64—Burning or sintering processes
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
    • F27D5/00—Supports, screens, or the like for the charge within the furnace
    • F27D5/0031—Treatment baskets for ceramic articles
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
    • C04B2235/3208—Calcium oxide or oxide-forming salts thereof, e.g. lime
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
    • C04B2235/3239—Vanadium oxides, vanadates or oxide forming salts thereof, e.g. magnesium vanadate
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment

Abstract

The invention provides a kiln furniture made of oxide-containing SiC with the following characteristics : 0.01 to 0.7wt.% V2 O5 , 0.01 to 0.7wt.% CaO and 0.01 to 5wt.% clay are added to SiC powder with its maximum particle diameter of 4mm or less to produce powder. The powder is baked to form SiC kiln furniture, wherein each of a surface layer and a central part of the SiC kiln furniture is measured by an X-ray refraction for powder and then a ratio of height of refraction peak value of cristobalite with 2&theta being 21.9 deg. in respect to a height of refraction peak value of silicon carbide with 2&theta against CuK&alpha ray being 34.0 deg. is calculated. At this time, this SiC kiln furniture is made such that a rate of a value of ratio at the central part in respect to a value of ratio at the surface layer is 20% or more, a refraction strength at a normal temperature is within &plusmn 20% of a refraction strength at 1400 DEG C.

Description

Kiln furniture made of sic and manufacture method thereof
The present invention relates to ware, watt etc. the shelf (refractory slab), the backing plate kiln furnitures such as (applying plate) that use in the calcining.
In the past, carborundum (SiC) material of anti-combustion the, because its good hear resistance and flame resistance, thereby industrial in occupation of critical positions, for example kiln furnitures such as the shelf used of burning ceramics device, backing plate, sheath be used a lot.
As everyone knows, a kind of as in this SiC material of anti-the combustion, be with the metal oxide of SiC particle and trace etc. be mixed together, moulding, in oxidizing atmosphere,, make the oxidation of SiC particulate fraction, the silica (SiO that generates by its partial oxidation by calcining 2), combine, form the so-called SiC matter thing of anti-combustion that is combined with oxide with the SiC particle.Because this SiC sintered body low price that is combined with oxide etc., thereby by the kiln furniture of purposes ware calcining usefulness widely.
But, because the SiC material of anti-combustion that is combined with oxide and the what is called that forms by SiC particle and combinations such as silicon nitride be combined with the SiC material of anti-combustion of nitride and again the crystal type SiC material of anti-the combustion compare, low, the anti-spallation of its intensity is bad, thus usually its life-span short.
And, recently in order to enhance productivity and energy-conservation etc., often need to carry out quick burning, also strengthen load kiln furniture.
Thereby, need improve performances such as the anti-spallation of the SiC matter thing of anti-combustion that is combined with oxide, oxidative resistance, creep resistants, but it is a lot of to hinder the factor that these characteristics improve, and is difficult to make it balancedly to improve mutually.
In view of the foregoing, the purpose of this invention is to provide and a kind ofly can balancedly improve anti-spallation, the SiC matter kiln furniture and the manufacture method thereof that are combined with oxide of oxidative resistance, creep resistant.
The invention provides a kind of SiC matter kiln furniture, it is characterized in that kiln furniture made by the material that mainly contains SiC, the method for making of this material is through for adding the V with respect to 0.01～0.7 weight % of this SiC amount in the SiC powder below the 4mm to maximum grain 2O 5, the CaO of 0.01～0.7 weight % and the clay of 0.01～5 weight %, the mixed-powder that obtains is carried out moulding, its calcination is become SiC matter kiln furniture: use Cuk α line and the angle of diffraction 2 θ with powder X-ray diffractometry, measure the top layer part of this SiC matter kiln furniture and the diffraction peak height of core respectively, the diffraction peak height of the christobalite that makes surface portion in 2 θ=21.9 ° is Y 1, the diffraction peak height of the SiC of surface portion in 2 θ=34.0 ° is Y 2, the diffraction peak height of the christobalite that makes core again in 2 θ=21.9 ° is Y 1', the diffraction peak height of the SiC that makes core again in 2 θ=34 ° is Y 2', satisfy (Y between them 1'/Y 2')/(y 1/ Y 2) 〉=0.2: in the bending strength of normal temperature is during at 1400 ℃ within bending strength ± 20% scope.
In addition, the present invention also provides the method for making kiln furniture from the material that mainly contains SiC, comprises the following steps: that to maximum grain warp be in the SiC powder below the 4mm, adds the V with respect to 0.01～0.7 weight % of this SiC amount 2O 5, the CaO of 0.01～0.7 weight % and the clay of 0.01～5 weight %, make mixed-powder, the mixed-powder that obtains is mediated with an amount of water and organic binder bond, kneaded material is shaped to desired shape, after the formed body drying that obtains,, and then be 1300～1500 ℃ of scopes and carry out 2～10 hours continuous calcining 1300 ℃ or above temperature province through carrying out the limit calcining that heated up more than 10 hours 700～1100 ℃ of scopes in maximum temperature.
The kiln furniture that the present invention makes from the material that mainly contains SiC is by being in the SiC powder of 4mm to maximum grain warp, adds the V with respect to 0.01～0.7 weight % of this SiC amount 2O 5, the CaO of 0.01～0.7 weight % and 0.01～5 weight % clay and the powder thing that obtains makes.Use this powder, following character is arranged with the SiC matter kiln furniture of the condition manufacturing that provides in the following manufacture method.
That is to say, measure the top layer part and the core of this SiC matter kiln furniture respectively by powder method with X-ray diffraction, obtaining 2 θ is the diffraction maximum height of 21.9 ° christobalite when being 34.0 ° the ratio of diffraction maximum height of SiC with respect to 2 θ, and the above-mentioned ratio of core is more than 20% with respect to the ratio of the above-mentioned ratio of top layer part.
Above-mentioned powder after moulding, is calcined in oxidizing atmosphere then, and the SiC particle will generate SiO by partial oxidation 2, it with by CaO and V 2O 5The trace meter oxide agent reaction of forming, form with SiC particle strong bonded in conjunction with mutually, at this moment, a part of SiO that produces by the SiC oxidation 2, transform as parafacies remainingly to christobalite from the nature of glass, still, if at the top layer of kiln furniture part and core, this christobalite amount has excessive difference, will be owing at nature of glass SiO 2It is big that the thermal stress that expansion when the christobalite phase transformation is shunk becomes, and cause its anti-spallation to degenerate, and therefore, the above-mentioned ratio relation for top layer part and core among the present invention has been made regulation.When satisfying aforesaid ratio relation, can obtain good anti-spallation.
Alleged top layer part is meant that from the part of kiln furniture surface to 1/3 wall thickness, so-called core is meant kiln furniture on thickness direction among the present invention, is positioned at 1/3 wall thickness part of core.
In addition, SiC matter kiln furniture of the present invention bending strength at normal temperatures is in bending strength ± 20% scope in the time of 1400 ℃.For example, if be 500kg/cm 1400 ℃ bending strength 2, the bending strength at normal temperature is exactly 400～600kg/cm so 2Why the present invention has stipulated the bending strength relation of above-mentioned normal temperature and 1400 ℃, is that this will cause anti-spallation decline because if the intensity difference when normal temperature and heating strengthens, heating makes the strength characteristics with respect to temperature become imbalance.That is to say, if the bending strength during normal temperature not in the scope of 1400 ℃ bending strength ± 20%, thereby will cause that anti-spallation decline causes inapplicable.
Below, describe for the manufacture method of relevant SiC matter kiln furniture of the present invention.
The kiln furniture that the present invention mainly contains SiC is by being in the SiC powder below the 4mm to maximum grain warp, adds the V with respect to 0.01～0.7 weight % of this SiC amount 2O 5, the CaO of 0.01～0.7 weight % and 0.01～5 weight % clay and the powder that obtains makes.
Because SiC matter kiln furniture, for example the common wall thickness of shelf is about 10～20mm, so consider from the viewpoint of its characteristic aspect and production technology aspect,, is preferably below the 3mm through being below the 4mm as the maximum grain of the SiC powder of aggregate.The particle size range that can be suitable for making the SiC powder of kiln furniture is: 500 μ are above be 35～50 weight %, 88～500 μ be 20～30 weight %, 88 μ or following be 30～35 weight %.
In the middle of the composition that in this SiC powder, adds, V wherein 2O 5The time play oxidation accelerator (co-catalyst) effect in calcining, promote internal oxidation, the difference of itself and top layer part degree of oxidation is reduced.In addition, V 2O 5With the SiO that generates by the oxidation of SiC particulate fraction 2Reaction forms vitreous film, can prevent oxygen to immerse kiln furniture inside, oxidative resistance is improved on the kiln furniture surface.And with respect to SiC amount of powder V 2O 5Addition can be 0.01～0.7 weight %, be preferably 0.01～0.5 weight %, 0.01～0.3 weight % preferably.Above-mentioned effect is insufficient during less than 0.01 weight %, surpass 0.7 weight % then cause surface oxidation excessively, internal oxidation reduces.
CaO wherein has the effect of easy generation glass, so it and V 2O 5Help the raising of oxidative resistance equally.Addition with respect to SiC amount of powder CaO can be 0.01～0.7 weight %, be preferably 0.01～0.5 weight %, 0.01～0.3 weight % preferably.Above-mentioned effect is insufficient when less than 0.01 weight %, surpasses that the viscosity that 0.7 weight % then causes the glass that generates descends, bending resistance descends.
Clay wherein, the density when being the raising moulding can be used as plasticizer and are added into.With respect to the addition of SiC amount of powder clay can be 0.01～5 weight %, preferable be 0.1～4 weight %.Effect is insufficient when less than 0.01 weight %, surpasses 5 weight % then because Al 2O 3Composition and impurity increase, make it bending resistance and descends.
In addition, the present invention also can add the amorphous Si O below the 5 weight % again in above-mentioned powder 2Add amorphous Si O 2Thereby, transform crystallization to christobalite in the time of can helping calcination, improve the characteristic of kiln furniture.
Above-mentioned Powdered (mixing) material and an amount of water and organic binder bond are mixed together, make it to be shaped to desired shape.With after the formed body drying that obtains, carry out intensification limit, limit calcining more than 10 hours 700～1100 ℃ temperature provinces.700～1100 ℃ of temperature ranges through more than 10 hours, by heating up lentamente, can promoting internal oxidation.The intensification does not here need to be undertaken by certain programming rate, can change aptly on programming rate or certain (a bit) temperature in temperature-rise period to keep the regular hour.
In manufacture method of the present invention, carry out the first above-mentioned calcining continuously, and then maximum temperature be set at 1300～1500 ℃ carry out second the calcining, carrying out 2～10 hours for the temperature range that is implemented in more than 1300 ℃ during this calcining: for example maximum temperature is set at 1400 ℃, if the intensification that reaches maximum temperature, carry out with 50 ℃/hour programming rates, then in reaching the temperature-rise period of maximum temperature, just need with intensification in 2 hours, so the calcination time that reaches after the maximum temperature should be below 8 hours 1300～1400 ℃ temperature provinces.By calcine, can limit the amount of oxidation of top layer part of SiC particle with this condition, can suppress the difference of top layer part and core christobalite growing amount to a certain extent.
If maximum temperature is lower than 1300 ℃, then the SiC oxidation of top layer part is insufficient, do not generate firm glass plasma membrane on the surface, therefore non-oxidizability is bad, on the other hand, if surpass 1500 ℃, then the amount of oxidation of top layer part is too much, degenerate with the balance of core.Equally, the time more than 1300 ℃ as being less than 2 hours, then the SiC oxidation of top layer part is insufficient, non-oxidizability is bad, and if surpassed 10 hours the amount of oxidation of top layer part too much, degenerate with the balance of core.
Illustrate in greater detail the present invention with embodiment below, but the present invention is not subjected to the restriction of these embodiment.
At first the SiC powder is adjusted to and makes its maximum grain through being the value that provides in table 1 and the table 2, in order to add the following granularity blend ratio that is applicable to kiln furniture, in the SiC powder of having adjusted granularity, add various additives as shown in Table 1 and Table 2, and then adding is as the carboxy methyl cellulose 0.03 weight % and the soluble starch 0.05 weight % of organic binder bond, and water 6 weight %, mix with wet pan.
The granularity blend ratio:
Above 35～50 weight % of 500 μ
88～500 μ, 20～30 weight %
Following 30～35 weight % of 88 μ
The base soil that obtains like this after slaking on the 1st, is carried out vibration moulding in about 20 seconds with the vibration shaping machine that pneumatic vibrator is installed, obtained tabular formed body.After this formed body drying, calcine with the various calcination conditions shown in table 1 and the table 2 (intensification condition and maximum temperature condition), obtain size and be the test body of 400mm * 350mm * 10mm.The details of intensification condition of representing with I～X in table 1 and table 2 and the maximum temperature condition represented with A～H are as shown in table 3.
Respectively test body for what obtain, carry out the mensuration and the evaluation of rerum natura as follows, its result provides in table 1 and table 2.
[apparent porosity, apparent specific gravity, Bulk Specific Gravity]
Press JISR 2205-74 standard test.
[bending strength]
JISR 2213-78 standard is pressed in relevant condition aspect.The normal temperature bending strength uses high temperature beam test machine to measure at 1400 ℃ with omnipotent precise materials testing machine (trade name ォ-ト グ ラ Off) mensuration, high-temperature bending strength.Use from the test body cut size as the sample of 130mm * 25mm * 10mm,, measure as the 100mm three-point bending method with spacing.
[SiO 2(christobalite) SiC ratio]
Cut the top layer part (counting the part that thickness is 2mm from the surface) and the core (part of wall thickness center 2mm thickness) of test body, pulverize, measure the powder that obtains separately respectively with X-ray diffraction method.With the peak of the 2 θ=21.9 ° CuK α line of locating to form as SiO 2The reference peaks of (christobalite) with the peak of the 2 θ=34.0 ℃ reference peaks as SiC, is measured the height of both reference peaks, obtains SiO 2The reference peaks height of (christobalite) is obtained the ratio of the above-mentioned ratio of core with respect to the above-mentioned ratio of top layer part again with respect to the ratio of the reference peaks height of SiC.
[anti-spallation]
With 280mm * 240mm * 20mmAl 2O 3Plate be placed on the test body (central authorities of 400mm * 350mm * 10mm), with electric furnace with Al 2O 3Plate and test body all are heated to design temperature.After design temperature keeps 2.5 hours, take out and put into room temperature, whether the checkout facility body crackle takes place.At first test, increase 25 ℃ at every turn, test to testing body and have crackle to take place repeatedly at test body when crackle does not take place, design temperature since 250 ℃ of design temperatures, the design temperature when crackle takes place is as fail temperature.
[creep resistance]
The sample of the 130mm * 25mm * 10mm that cuts out from the test body with the spacing support of 100mm adds 150kg/cm in the centre 2Loading, with this state after 1350 ℃ keep 100 hours, the amount of bow of working sample.
[non-oxidizability]
Will be from the sample of 130mm * 25mm * 10mm of cutting of test body, at O 2Concentration is in 60% the atmosphere, kept 200 hours at 1150 ℃, obtains the weight increase of sample.
Table 1
Try test No. 1 2* 3* 4* 5* 6 7 8* 9* 10* 11* 12 13* 14* 15 16*
System makes condition SIC maximum particle diameter (mm) 2.83 2.83 2.83 2.83 2.83 2.83 2.83 2.83 2.83 2.83 2.83 2.83 2.83 2.83 2.83 2.83
Adding ingredient V 2O 5(weight %) 0 0.01 0.1 0.3 0.7 0.8 0.3 0.3 0.3 0.3 0.3 0.3 0.3 0.3 0.3 0.3
CaO (weight %) 0.1 0.1 0.1 0.1 0.1 0.1 0 0.01 0.1 0.3 0.7 0.8 0.3 0.3 0.3 0.3
Clay (weight %) 0.5 0.5 0.5 0.5 0.5 0.5 0 0.5 0.5 0.5 0.5 0.5 1 5 6 0.5
The No SiO that formalizes 2(weight %) 0 0 0 0 0 0 0 0 0 0 0 0 0 0 0 2
Burning is forged Noboru temperature condition 1) V V V V V V V V V V V V V V V V
The maximum temperature condition 2) D D D D D D D D D D D D D D D D
Rerum natura and evaluation The performance porosity (%) 11.1 10.1 9.3 8.3 7.1 6.2 8.7 8.7 8.4 9.1 9.8 10.8 10.1 8.4 10.0 6.5
Apparent specific gravity 3.05 3.00 3.01 3.00 2.96 2.90 2.99 3.00 2.98 3.00 3.00 2.99 2.98 2.97 3.01 2.95
Bulk specific gravity 2.71 2.70 2.73 2.75 2.75 2.72 2.73 2.74 2.73 2.73 2.71 2.67 2.68 2.72 2.71 2.76
Normal temperature bending strength (kg/cm 2) 313 376 404 450 420 415 405 422 424 415 438 450 444 408 429 445
High-temperature bending strength (kg/cm 2) 288 351 428 475 382 325 532 493 471 401 365 343 405 365 333 429
The SiO of core 2/ SiC ratio is with respect to top layer part SiO 2The ratio of/SiC ratio (%) 10 20 35 45 40 15 45 40 40 40 35 25 35 30 20 45
Anti-spallation fail temperature (℃) 275 400 425 475 400 350 350 375 425 450 400 350 450 400 300 475
Creep resistance amount of bow (mm) 2.3 1.2 1.0 0.7 0.8 1.5 0.7 0.8 0.9 1.0 1.1 2.1 0.9 1.0 1.3 0.6
Non-oxidizability weight increase (%) 1.9 1.1 0.8 0.7 0.6 0.6 0.7 0.8 0.8 0.9 0.9 1.0 0.9 1.0 1.2 0.6
Overall merit 3) × △ ○ ○ △ × × △ ○ ○ △ × ○ △ × ○
1), 2) ... referring to table 3.
3) ... zero expression is fine, and △ represents that well * expression is bad.
In the test that condition and range of the present invention carries out, has the * mark on the right side of test No..
Table 2
Try test No. 17 18 19 20* 21* 22 23 24* 25* 26* 27* 28 29 30 31* 32* 33 34*
System makes condition SIC maximum particle diameter (mm) 2.83 2.83 2.83 2.83 2.83 2.83 2.83 2.83 2.83 2.83 2.83 2.83 2.83 2.83 2.83 2.83 4.76 2.00
Adding ingredient V 2O 5(weight %) 0.3 0.3 0.3 0.3 0.3 0.3 0.3 0.3 0.3 0.3 0.3 0 0.8 0.4 0.3 0.3 0.3 0.3
CaO (weight %) 0.3 0.3 0.3 0.3 0.3 0.3 0.3 0.3 0.3 0.3 0.3 0.3 0.8 0.4 0.3 0.3 0.3 0.3
Clay (weight %) 0.5 0.5 0.5 0.5 0.5 0.5 0.5 0.5 0.5 0.5 0.5 1.0 1.0 0 1.0 1.0 0.5 0.5
The No SiO that formalizes 2(weight %) 0 0 0 0 0 0 0 0 0 0 0 0 0 0 3 5 0 0
Calcining Noboru temperature condition 1) I II III IV V VI VII VIII IX X IX III V VII V V V V
The maximum temperature condition 2) D D C G E F II D A D B D E C D D D D
Rerum natura and comment rank Apparent porosity (%) 11.3 8.7 5.8 10.3 6.8 11.9 12.0 7.1 10.3 8.7 8.4 10.1 9.8 8.7 6.5 5.2 8.7 8.7
Apparent specific gravity 3.02 2.98 2.90 3.02 2.95 3.03 3.01 2.96 3.00 2.98 2.98 3.00 2.97 2.99 2.94 2.91 2.98 3.00
Bulk specific gravity 2.68 2.72 2.73 2.71 2.75 2.67 2.65 2.75 2.69 2.72 2.73 2.70 2.68 2.73 2.75 2.76 2.72 2.74
Normal temperature bending strength (kg/cm 2) 419 433 526 485 493 441 355 465 388 395 422 375 366 383 403 383 315 556
High-temperature bending strength (kg/cm 2) 326 418 475 419 450 385 281 444 369 411 390 322 285 336 381 390 290 512
The SiO of core 2/ SiC ratio is with respect to top layer part SiO 2The ratio of/SiC ratio (%) 10 35 15 25 45 15 5 40 35 30 35 15 20 5 40 45 35 30
Anti-spallation fail temperature (℃) 300 475 350 400 475 375 250 475 425 400 450 350 350 350 425 400 350 425
Creep resistance amount of bow (mm) 2.1 0.8 1.0 1.0 0.7 1.0 2.6 0.5 1.0 0.8 1.0 1.8 1.5 1.9 0.6 0.5 2.5 1.0
Non-oxidizability weight increase (%) 0.9 0.7 1.0 0.6 0.5 0.9 1.0 0.8 0.7 0.9 0.9 2.1 0.8 0.9 0.5 0.4 0.9 0.9
Overall merit 3) × ○ × △ ○ × × ○ ○ ○ ○ × × × ○ ○ × ○
1), 2) ... referring to table 3.
3) ... zero expression is fine, and △ represents that well * expression is bad.
In the test that condition and range of the present invention carries out, has the * mark on the right side of test No..
Table 3
The intensification condition I Programming rate with 50 ℃/hour rises to maximum temperature
II Programming rate with 40 ℃/hour rises to maximum temperature
III Programming rate with 30 ℃/hour rises to maximum temperature
IV By 50 ℃/hour be warming up to 700 ℃ → 700 ℃ keep 10 hours → be warming up to maximum temperature by 50 ℃/hour
V By 50 ℃/hour be warming up to 900 ℃ → 900 ℃ keep 10 hours → be warming up to maximum temperature by 50 ℃/hour
VI By 50 ℃/hour be warming up to 1100 ℃ → 1100 ℃ keep 10 hours → be warming up to maximum temperature by 50 ℃/hour
VII By 50 ℃/hour be warming up to 1200 ℃ → 1200 ℃ keep 10 hours → be warming up to maximum temperature by 50 ℃/hour
VIII By 50 ℃/hour be warming up to 850 ℃ → 850 ℃ keep 15 hours → be warming up to maximum temperature by 50 ℃/hour
IX By 50 ℃/hour be warming up to 700 ℃ → by 40 ℃/hour be warming up to 1100 ℃ → be warming up to maximum temperature by 50 ℃/hour
X By 50 ℃/hour be warming up to 700 ℃ → 700 ℃ keep 5 hours → by 50 ℃/hour be warming up to 1100 ℃ → 1100 ℃ keep 5 hours → be warming up to maximum temperature by 50 ℃/hour
The maximum temperature condition A Kept 5 hours at 1300 ℃
B Kept 10 hours at 1300 ℃
C Kept 12 hours at 1300 ℃
D Kept 5 hours at 1400 ℃
E Kept 8 hours at 1400 ℃
F Kept 10 hours at 1400 ℃
G Kept 5 hours at 1500 ℃
H Kept 8 hours at 1500 ℃
As shown in Table 1 and Table 2, the test body of making of the condition that satisfies manufacture method of the present invention demonstrates premium properties: core SiO 2The ratio of/SiC is with respect to the SiO of top layer part 2The ratio of the ratio of/SiC (the diffraction maximum height of christobalite is with respect to the ratio of carborundum diffraction maximum height) all 20% or more than, and the bending strength of normal temperature, within the scope of 1400 ℃ of bending strength ± 209%, anti-spallation, creep resistance and non-oxidizability can both balancedly improve, and are gratifying as kiln furniture.
As mentioned above, the present invention obtained characteristics such as anti-spallation, creep resistance and non-oxidizability all can be balanced that improve, can satisfy that kiln furniture requires, as to be combined with oxide SiC matter kiln furniture.

Claims (4)

1. by mainly containing the kiln furniture that the SiC material is made, it is characterized in that:
In maximum particle diameter is SiC powder below the 4mm, add V with respect to 0.01～0.7 weight % of this SiC amount 2O 5, the CaO of 0.01～0.7 weight % and the clay of 0.01-5 weight %, will be sintered into SiC matter kiln furniture after the powder moulding that obtain;
Top layer part and core with this main SiC matter kiln furniture, use CuK α line to measure with powder X-ray diffractometry respectively, when the christobalite diffraction maximum height of trying to achieve 2 θ and be 21.9 ° was 34.0 ° the ratio of carborundum diffraction maximum height with respect to 2 θ, the above-mentioned ratio of core was more than 20% with respect to the ratio of the above-mentioned ratio of top layer part;
Bending strength during normal temperature is in the scope of bending strength ± 20% in the time of 1400 ℃.
2. make the method for kiln furniture by the material that mainly contains SiC, it is characterized in that: in maximum particle diameter is SiC powder below the 4mm, add V with respect to 0.01～0.7 weight % of this SiC amount 2O 5, the CaO of 0.01～0.7 weight % and the clay of 0.01～5 weight %, the powder that obtains and an amount of water and organic bond are mixed together, it is shaped to desired shape, after the gained formed body drying, temperature range at 700～1100 ℃, the limit is through the intensification more than 10 hours, the limit calcining, and then be 1300～1500 ℃ of scopes and carried out continuous calcining through 2～10 hours in the temperature range more than 1300 ℃ with maximum temperature.
3. according to claim 2ly make the method for kiln furniture, it is characterized in that:, add V with respect to the 0.01-0.7 weight % of this SiC amount being in the SiC powder below the 4mm to maximum particle diameter by the material that mainly contains SiC 2O 5, the CaO of 0.01～0.7 weight % and 0.01～5 weight % clay after, in resulting powder, add the following amorphous Si O of 5 weight % again 2
4. the material that mainly contains SiC according to claim 2 is made the method for kiln furniture, it is characterized in that maximum particle diameter wherein is that the grain size proportion of the following SiC powder of 4mm is, 500 μ above for 35-50 weight %, 88～500 μ be 20～30 weight %, 88 μ following be 30～35 weight %.
CN95103594A 1994-12-27 1995-03-27 Kiln furniture made of sic and the process for production thereof Expired - Lifetime CN1106565C (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
JP325267/94 1994-12-27
JP32526794A JP3373312B2 (en) 1994-12-27 1994-12-27 SiC-based kiln tool and method of manufacturing the same
JP325267/1994 1994-12-27

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CN1125840A CN1125840A (en) 1996-07-03
CN1106565C true CN1106565C (en) 2003-04-23

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JP4704111B2 (en) * 2005-06-01 2011-06-15 日本碍子株式会社 Oxide bonded silicon carbide material
JP5108311B2 (en) * 2007-01-19 2012-12-26 日本碍子株式会社 Oxide-bonded silicon carbide sintered body and manufacturing method thereof
EP2138474B1 (en) * 2008-06-23 2018-08-08 Imerys Kiln Furniture Hungary Ltd. Sic material
CN101654362B (en) * 2009-08-31 2013-01-23 成都蜀冶新材料有限责任公司 Silicon oxynitride combined carborundum high-temperature ceramic material and preparation method thereof

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JPH08178548A (en) 1996-07-12
CN1125840A (en) 1996-07-03

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