CN107417287A - A kind of microwave metallurgical kiln car corundum silicon oxynitride composite refractory - Google Patents
A kind of microwave metallurgical kiln car corundum silicon oxynitride composite refractory Download PDFInfo
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- CN107417287A CN107417287A CN201710736091.9A CN201710736091A CN107417287A CN 107417287 A CN107417287 A CN 107417287A CN 201710736091 A CN201710736091 A CN 201710736091A CN 107417287 A CN107417287 A CN 107417287A
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- corundum
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- 239000010431 corundum Substances 0.000 title claims abstract description 69
- 229910052593 corundum Inorganic materials 0.000 title claims abstract description 69
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 39
- 239000010703 silicon Substances 0.000 title claims abstract description 39
- 239000002131 composite material Substances 0.000 title claims abstract description 28
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 239000000463 material Substances 0.000 claims abstract description 58
- 239000000843 powder Substances 0.000 claims abstract description 39
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 25
- 239000011863 silicon-based powder Substances 0.000 claims abstract description 22
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 21
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 21
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 21
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 21
- 239000012298 atmosphere Substances 0.000 claims abstract description 11
- 238000002360 preparation method Methods 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 26
- 239000007767 bonding agent Substances 0.000 claims description 15
- 229910052757 nitrogen Inorganic materials 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 11
- 238000010792 warming Methods 0.000 claims description 10
- 230000032683 aging Effects 0.000 claims description 9
- 239000003595 mist Substances 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 7
- 239000008187 granular material Substances 0.000 claims description 6
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 5
- 239000011449 brick Substances 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 238000005121 nitriding Methods 0.000 claims description 5
- 238000007493 shaping process Methods 0.000 claims description 5
- 230000003647 oxidation Effects 0.000 claims description 4
- 238000007254 oxidation reaction Methods 0.000 claims description 4
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 4
- 150000001875 compounds Chemical class 0.000 claims description 3
- 239000010453 quartz Substances 0.000 claims description 3
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 2
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims description 2
- 239000004375 Dextrin Substances 0.000 claims description 2
- 229920001353 Dextrin Polymers 0.000 claims description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 2
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 2
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims description 2
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims description 2
- 235000019425 dextrin Nutrition 0.000 claims description 2
- 239000000428 dust Substances 0.000 claims description 2
- 229910001651 emery Inorganic materials 0.000 claims description 2
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- 239000005011 phenolic resin Substances 0.000 claims description 2
- 229920001568 phenolic resin Polymers 0.000 claims description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 2
- 235000019422 polyvinyl alcohol Nutrition 0.000 claims description 2
- 239000003265 pulping liquor Substances 0.000 claims description 2
- 239000001301 oxygen Substances 0.000 claims 1
- 229910052760 oxygen Inorganic materials 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 9
- 230000035939 shock Effects 0.000 abstract description 8
- 238000005245 sintering Methods 0.000 abstract description 7
- 239000011159 matrix material Substances 0.000 abstract description 4
- 230000008569 process Effects 0.000 abstract description 3
- 239000011819 refractory material Substances 0.000 description 10
- 238000011065 in-situ storage Methods 0.000 description 7
- 238000003723 Smelting Methods 0.000 description 6
- 238000009413 insulation Methods 0.000 description 5
- 229910052799 carbon Inorganic materials 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 230000003628 erosive effect Effects 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 238000007789 sealing Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 229910000863 Ferronickel Inorganic materials 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 235000013312 flour Nutrition 0.000 description 3
- 229910052500 inorganic mineral Inorganic materials 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000011707 mineral Substances 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 235000013339 cereals Nutrition 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 239000010432 diamond Substances 0.000 description 2
- 229910003460 diamond Inorganic materials 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 230000005672 electromagnetic field Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000002893 slag Substances 0.000 description 2
- 230000035882 stress Effects 0.000 description 2
- 230000008646 thermal stress Effects 0.000 description 2
- 241001062472 Stokellia anisodon Species 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003139 buffering effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 229910052863 mullite Inorganic materials 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 239000012779 reinforcing material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000009738 saturating Methods 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
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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
- C04B35/66—Monolithic refractories or refractory mortars, including those whether or not containing clay
-
- 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
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
- C04B35/101—Refractories from grain sized mixtures
-
- 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
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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
- 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
- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3418—Silicon oxide, silicic acids or oxide forming salts thereof, e.g. silica sol, fused silica, silica fume, cristobalite, quartz or flint
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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
- 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
- C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
- C04B2235/428—Silicon
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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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
- C04B2235/9669—Resistance against chemicals, e.g. against molten glass or molten salts
- C04B2235/9676—Resistance against chemicals, e.g. against molten glass or molten salts against molten metals such as steel or aluminium
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Furnace Details (AREA)
- Ceramic Products (AREA)
Abstract
The invention discloses a kind of low electromagnetic wave absorptivity, excellent wave, high volume stability is good, good thermal shock, anti-erosion excellent microwave metallurgical kiln car corundum silicon oxynitride composite refractory and preparation method thereof.Original material is：Corundum aggregate, corundum fine powder, SiO2Powder, Si powder, are molded using briquetting process, in N2It is prepared under atmosphere by situ nitridation reaction sintering.The principal crystalline phase of corundum silicon oxynitride composite refractory of the present invention is corundum and silicon oxynitride, while has a small amount of β Si in matrix3N4, β Sialon and O ' Sialon, bulk density is in 3.0g/cm3More than, cold crushing strength：170 190MPa, strength at normal temperature：25 30MPa, dielectric loss angle tangent：0.0014 0.0033, there is good wave.
Description
Technical field
The present invention relates to a kind of microwave metallurgical kiln car refractory material, more particularly to one kind is by adding Si powder and Si02Powder
Reaction in-situ prepares corundum-silicon oxynitride composite refractory and preparation method thereof.
Background technology
With the continuous development of science and technology, environmental protection obtains higher and higher attention in life, production.Traditional heavy industry
The particularly hot industry such as metal smelt, there is an urgent need to change the mode of production to adapt to national development requirement.Microwave heating technique
Appearance cause high-temperature heating have more energy efficient environmentally friendly mode of heating, wherein with microwave heat mode claimed come metal smelting
It is the new technology of rising in recent years for green metallurgical.
Due to the appearance of microwave metallurgical technology, microwave metallurgical kiln car refractory material carries mainly as the kiln car of carrying material
Body uses, and material enters on kiln car from kiln, is discharged after microwave is smelted from kiln tail.Due to being rapidly heated for microwave heating
With discharging when kiln car directly discharging at room temperature, so there is higher performance requirement to kiln car refractory material：（1）Low electromagnetic wave
Absorptivity and excellent wave：First, prevent the electromagnetic energy that refractory material own absorption is more under Electromagnetic Field from causing temperature
Spend high and material is damaged, second, the energy can be saved, limited electromagnetic energy is absorbed by metallurgical material, shorten smelting
Refine the time；（2）Excellent thermal shock resistance：Larger thermal stress can be resisted in microwave heats rapid heating condition to rush material
Hit；（3）Good mechanical behavior under high temperature：Furnace lining material will bear various structural stress machinery works in microwave metallurgical course of reaction
With；（4）Corrosion resistance is excellent：Refractory material at high temperature for a long time contacted with metallurgical material, easily with metallurgical material
Learning reaction causes structure of refractory to be destroyed.
Corundum and mullite are the metallurgical most commonly used refractory materials of microwave current, and it has good thermal shock performance, but
The erosion performance of its alkali resistance slag and undesirable to the through performance of electromagnetic wave.Pure corundum material dielectric constant is generally 8 ~
10, aluminum oxide absorbs that microwave ability is weak, and wave is good under low temperature.But the dielectric constant of corundum can raise with the rise of temperature,
It can increase its thermal losses in electromagnetic field, and the thermal shock resistance of corundum material is bad, is not suitable for doing the furnace lining of microwave heating
And kiln car material.Quartz-ceramics has the dielectric constant for having very little below 1000 DEG C, and its dielectric constant is only 4 or so, wave
It is good, and the coefficient of expansion of quartz-ceramics is small, it is widely used in microwave metallurgical.But because quartz is easily sent out at high temperature
Raw crystal transfer, its maximum operation (service) temperature are not suitable for using in high temperature microwave metallurgy no more than 1150 DEG C.
There is presently no the research for microwave metallurgical refractory material system, if it is possible to which research and development, which are prepared, meets microwave
The refractory material of metallurgical kiln car use environment, it can not only increase the service life of kiln car, improve metallurgical efficiency, reduction is produced into
This, the also utilization relatively reasonable to resource less and less on the earth, reduces the waste and consumption of resource.
The content of the invention
Requirement of the microwave metallurgical kiln car to its performance can not be met to solve current refractory material, the present invention provides a kind of low electromagnetism
Ripple absorptivity, excellent wave, high volume stability is good, good thermal shock, and the excellent microwave metallurgical kiln car of anti-erosion is used
Corundum-silicon oxynitride composite refractory and preparation method thereof.
To achieve these goals, the technical solution adopted by the present invention is：
A kind of corundum-silicon oxynitride composite refractory, original material are：Corundum aggregate, corundum fine powder, SiO2Powder, Si powder, use
Briquetting process is molded, in N2It is prepared under atmosphere by situ nitridation reaction sintering.
The addition parts by weight of the original material of the present invention are：Corundum aggregate 30-45 parts that granularity is 3-1mm, granularity 1-0mm
Corundum aggregate 20-25 parts, corundum fine powder 15-25 parts, SiO2Micro mist 3-6 parts, Si powder 10-15 parts, bonding agent addition are original
The 3-6% for gross weight of expecting.
The corundum aggregate be plate diamond spar, fused brown corundum, electric smelting dense alumina and one kind in fused white corundum or
It is two or more；
Wherein add granularity be 3-1mm and 1-0mm corundum aggregates be in order to：It can see by the fracture apperance figure of the present invention,
The silicon oxynitride of short cylinder and the silicon nitride of long column shape, silicon oxynitride and nitridation are grown in corundum in granules is the material of skeleton
Silicon growth plays a part of buffering stress in material internal, improves the tough of composite in corundum aggregate surface or stomata
Property, be advantageous to the thermal shock resistance lifting and the reduction of the coefficient of expansion of final products.
The corundum fine powder be plate diamond spar, fused brown corundum, electric smelting dense alumina and one kind in fused white corundum or
It is two or more；Granularity is one or two grain size intervals in≤0.088mm and≤0.045mm；
The size distribution of wherein corundum fine powder be in order to：Because corundum fine powder part granularity has reached Ultramicro-powder level, these micro mists
Infiltration in the crystalline phase finally given, in addition to having silicon oxynitride and silicon nitride, also the Sialon crystalline phases of part they with
Corundum is well combined, and improves the intensity and wave of material.
The SiO2Micro mist be one or both of ultra-fine natural quartz emery dust, silicon powder and gaseous oxidation silicon powder with
On；Purity >=98%, particle diameter are less than 10 μm.
Wherein SiO2The size distribution of micro mist be in order to：SiO2Granularity has reached micro powder grade, SiO2Powder can be fully infiltrated into raw material
Gap in, the principal crystalline phase for making final products is generated in-situ silicon oxynitride crystalline phase because generation silicon oxynitride crystalline phase tool
There are low electromagnetic wave absorptivity and excellent wave.
Si powder purity >=99%, granularity≤0.045mm；
Wherein Si powder reacts the thing phases such as in-situ preparation silicon nitride, silicon oxynitride in sintering process with nitrogen, promotes material
Sintering, while improving composite hot strength and wave, the consistency for adding material improves corrosion resistance.Si powder
Granularity≤0.045mm；Purpose is that nitridation forms silicon oxynitride in order to allow silica flour to be easier under preparation temperature completely.
The corundum aggregate and fine powder wherein added is that the principal crystalline phase of material plays skeleton function, the SiO in matrix2Micro mist and Si
Powder generates Si in temperature flowing nitrogen situ2N2O is simultaneously combined together with corundum aggregate, because the superfluous of Si powder and part are super
The presence of micro- schmigel, except Si in matrix2N2There is part Si outside O3N4Generated with Sialon phases.Si2N2The non-oxidized substances such as O are brilliant
Mutually it is in the form of a column and is grown in corundum aggregate surface, not only increase the strength of materials and wave of final products, and has buffered material
Expect built-in thermal stress, improve the toughness of composite, be advantageous to thermal shock resistance raising and the reduction of the coefficient of expansion.
The bonding agent is phenolic resin, dextrin, polyvinyl alcohol, carboxymethyl cellulose, one kind in spent pulping liquor or several
Kind is compound.
The present invention this microwave metallurgical kiln car be with the preparation method of corundum-silicon oxynitride composite refractory：
Step 1: first by corundum fine powder 15-25 parts, SiO2Micro mist 3-6 parts, Si powder 10-15 parts, are put into ball mill according to corundum
Ball and material ratio 1:1, in the case where rotating speed is 1000 ~ 1200rpm, 120-180 minutes are ground, obtain being pre-mixed fine powder；
Step 2: by corundum aggregate 30-45 parts that granularity is 3-1mm, granularity is poured into mixed for 1-0mm corundum aggregate 20-25 parts
In mill, 3-6 is then addedwt% bonding agents, kolleroang stirring 5-10min is opened, makes bonding agent uniform adhesion in corundum in granules
Surface soaks with it, adds the premixing fine powder that step 1 obtains, and stirs 10-20min, material is sufficiently mixed uniformly；
Step 3: it is to be put in 50-60% air atmosphere that mixed material is fitted into hermetic bag into air humidity at room temperature
12-24h ageing mixtures；
Step 4: after ageing mixture, with hydraulic press under 120MPa pressure adobe is made in well mixed material, by the brick after shaping
Base is dried 24 hours in 120 DEG C of drying boxes；
Step 5: being transported into after dried sample is weighed in nitriding furnace, sealing fire door is passed through nitrogen, in pressure-fired flowing nitrogen
1100 DEG C are warming up to 5-8 DEG C/min heating rate under atmosphere, insulation is warming up to 1-5 DEG C/min speed again after 2 hours
1450 DEG C and be incubated 24 hours, then cool to room temperature with the furnace, you can obtain corundum-silicon oxynitride composite refractory.
Wherein step 1 is first corundum fine powder, SiO2Powder and Si powder are pre-mixed, in order to SiO2Powder, Si powder and
Corundum fine powder can be mixed uniformly, and the short cylinder crystal silicon oxynitride for making to be formed after nitridation is uniformly distributed, the intensity of reinforcing material and
Wave.
Wherein step 3 the purpose of be in order that in its bonding agent uniform moisture distribution, improve the processability of blank, make
Adobe aggregate and fine powder are uniformly distributed, and do not produce segregation, so that final products have low electromagnetic wave absorptivity and excellent saturating
Ripple.
Because nitridation reaction starts at this temperature, 1450 DEG C of long-time heat preservations have for insulation at 1100 DEG C wherein in step 5
Beneficial to the generation of more silicon oxynitrides and the further sintering of material.
The present invention by corundum be base-material, introduces the optimum organization, reasonable of a certain amount of ultrafine silica powder and silica flour, raw material
Grain size proportion, burnt till using the step of in situ nitridation reaction one under high temperature nitrogen atmosphere and prepare corundum-silicon oxynitride composite fire
Material, the principal crystalline phase of the material is corundum and silicon oxynitride, and secondary crystalline phase is β-Si3N4, β-Sialon, O '-Sialon etc. it is non-oxide
Thing combination phase, therefore there is excellent wave, good high volume stability, thermal shock resistance and erosion-resisting characteristics.
Burnt till present invention employs reaction in-situ and prepare corundum-silicon oxynitride composite, without using directly in raw material
Silicon oxynitride is added, because silicon oxynitride with corundum belongs to high-melting-point thing phase, it is necessary to higher firing temperature or plus help
Agent is burnt, while is also unfavorable for that material is preferably compound, large effect is had to the high-temperature behavior of composite.The present invention uses
Reaction in-situ, which is burnt till, prepares corundum-silicon oxynitride composite, can not only reduce sintering temperature, generated in-situ nitrogen oxidation
Silicon can be combined more preferably with corundum, while a small amount of β-Si generated in preparation process3N4And Sialon solid solution, these generations
Thing is all greatly improved to the wave of material, thermal expansion and intensity.
The present invention has selected relatively cheap ultrafine silica powder and Si powder as raw material, compared with nitrogen oxidation silica flour,
The production cost of material is significantly reduced while corundum of good performance-silicon oxynitride composite refractory is made.
Because the material used in the present invention is mainly corundum, corundum is neutral oxide material, to acid and basic slag all
There is good corrosion resistance, therefore the present invention, for sintering the material of any material, can use as the refractory material of kiln car
Scope is wider.
The principal crystalline phase of corundum of the present invention-silicon oxynitride composite refractory is corundum and silicon oxynitride, while
There are a small amount of β-Si in matrix3N4, β-Sialon and O '-Sialon, bulk density is in 3.0g/cm3More than, the resistance to pressure of normal temperature
Degree：170-190MPa, strength at normal temperature：25-30MPa, at 1400 DEG C hot modulus of rupture in 20-30MPa or so, according to
1100 DEG C-water cooling of YB/T376.1-1995 standards number is 10-50 times, normal temperature dielectric constant：8-9, dielectric loss angle tangent：
0.0014-0.0033, there is good wave.
Embodiment
Implementation and the feature of the present invention is exemplified below, but the present invention is not limited to following embodiments.
Embodiment 1：
Step 1: first by 17 parts of corundum fine powder, SiO23 parts of powder, SiO21-5 μm of powder footpath, 10 parts of Si powder, is put into ball mill
According to corundum ball and material ratio 1:1, in the case where rotating speed is 1000 ~ 1200rpm, it is pre-mixed 120 minutes, obtains being pre-mixed fine powder；
Step 2: by 45 parts of the corundum aggregate that granularity is 3-1mm, granularity is that 1-0mm 25 parts of corundum aggregate is poured into kolleroang,
Then 6 are addedwt% bonding agents, kolleroang stirring 10min is opened, makes bonding agent uniform adhesion in corundum in granules surface and Qi Run
It is wet, the premixing fine powder that step 1 obtains is added, 20min is stirred, material is sufficiently mixed uniformly；
Put Step 3: mixed material is fitted into hermetic bag in the air atmosphere that room temperature air humidity is 50-60%
12-24h ageing mixtures；
Step 4: after ageing mixture, well mixed material is made under 120MPa pressure with hydraulic press 65mm × 114mm ×
230mm mark shaped brick adobe, the adobe after shaping is dried 24 hours in 120 DEG C of drying boxes；
Step 5: being transported into after dried sample is weighed in nitriding furnace, sealing fire door is passed through nitrogen, in pressure-fired flowing nitrogen
1100 DEG C are warming up to 5-8 DEG C/min heating rate under atmosphere, insulation is warming up to 1-5 DEG C/min speed again after 2 hours
1450 DEG C and be incubated 24 hours, then cool to room temperature with the furnace, you can obtain corundum-silicon oxynitride composite refractory.
The performance indications of products obtained therefrom are：Apparent porosity：16.3%, bulk density：3.08g/cm3, cold crushing strength：
182MPa, strength at normal temperature：27MPa, hot modulus of rupture at 1400 DEG C：20MPa or so, marked according to YB/T376.1-1995
Accurate 1100 DEG C-water cooling number：42 times, normal temperature dielectric constant：8.17 dielectric loss angle tangent：0.0014, wave is good.It is anti-
Erosion experiment result is shown, best to the anti-erosion effect of ferronickel mineral.
Embodiment 2：
Step 1: first by 18 parts of corundum fine powder, SiO25 parts of powder, SiO22-3 μm of powder footpath, 10 parts of Si powder, is put into ball mill
According to corundum ball and material ratio 1:1, in the case where rotating speed is 1000 ~ 1200rpm, it is pre-mixed 50 minutes, obtains being pre-mixed fine powder；
Step 2: by 45 parts of the corundum aggregate that granularity is 3-1mm, granularity is that 1-0mm 22 parts of corundum aggregate is poured into kolleroang,
Then 5 are addedwt% bonding agent, kolleroang stirring 5min is opened, bonding agent uniform adhesion is soaked on corundum in granules surface with it,
The premixing fine powder that step 1 obtains is added, 10min is stirred, material is sufficiently mixed uniformly；
Put Step 3: mixed material is fitted into hermetic bag in the air atmosphere that air at room temperature humidity is 50-60%
12-24h ageing mixtures；
Step 4: after ageing mixture, well mixed material is made under 120MPa pressure with hydraulic press 65mm × 114mm ×
230mm mark shaped brick adobe, the adobe after shaping is dried 24 hours in 120 DEG C of drying boxes；
Step 5: being transported into after dried sample is weighed in nitriding furnace, sealing fire door is passed through nitrogen, in pressure-fired flowing nitrogen
1100 DEG C are warming up to 5-8 DEG C/min heating rate under atmosphere, insulation is warming up to 1-5 DEG C/min speed again after 2 hours
1450 DEG C and be incubated 24 hours, then cool to room temperature with the furnace, you can obtain corundum-silicon oxynitride composite refractory.
The performance indications of products obtained therefrom are：Apparent porosity：16.0%, bulk density：3.00g/cm3, cold crushing strength：
172.91MPa, strength at normal temperature：25.62MPa, hot modulus of rupture at 1400 DEG C：24.27MPa or so, according to YB/
T376.1-1995 standards 1100 DEG C-water cooling number:35 times, normal temperature dielectric constant：9.14 dielectric loss angle tangent：0.0033,
With good wave.It is good to resist the erosion effect of microwave smelting ferronickel mineral material,
Embodiment 3：
Step 1: first by 25 parts of corundum fine powder, SiO26 parts of powder, SiO25-10 μm of powder footpath, 14 parts of Si powder, is put into ball mill
According to corundum ball and material ratio 1:1, in the case where rotating speed is 1000 ~ 1200rpm, it is pre-mixed 40 minutes, obtains being pre-mixed fine powder；
Step 2: by 30 parts of the corundum aggregate that granularity is 3-1mm, granularity is that 1-0mm 25 parts of corundum aggregate is poured into kolleroang,
Then 6 are addedwt% bonding agents, kolleroang stirring 10min is opened, makes bonding agent uniform adhesion in corundum in granules surface and Qi Run
It is wet, the premixing fine powder that step 1 obtains is added, 20min is stirred, material is sufficiently mixed uniformly；
Step 3: mixed material is fitted into hermetic bag 12-24h is put in the air atmosphere that air humidity is 50-60%
Ageing mixture；
Step 4: after ageing mixture, well mixed material is made under 120MPa pressure with hydraulic press 65mm × 114mm ×
230mm mark shaped brick adobe, the adobe after shaping is dried 48 hours in 120 DEG C of drying boxes；
Step 5: being transported into after dried sample is weighed in nitriding furnace, sealing fire door is passed through nitrogen, in pressure-fired flowing nitrogen
1100 DEG C are warming up to 5-8 DEG C/min heating rate under atmosphere, insulation is warming up to 1-5 DEG C/min speed again after 2 hours
1450 DEG C and be incubated 24 hours, then cool to room temperature with the furnace, you can obtain corundum-silicon oxynitride composite refractory.
The performance indications of products obtained therefrom are：Apparent porosity：16.4%, bulk density：3.06g/cm3, cold crushing strength：
190.90MPa, strength at normal temperature：28.09MPa, hot modulus of rupture at 1400 DEG C：22.06MPa or so, according to YB/
T376.1-1995 standards 1100 DEG C-water cooling number:27 times, normal temperature dielectric constant：8.72 dielectric loss angle tangent：0.0018,
With best wave.The erosion effect for resisting microwave smelting ferronickel mineral material is good.
Claims (6)
- A kind of 1. microwave metallurgical kiln car corundum-silicon oxynitride composite refractory, it is characterised in that:The addition weight of original material Measuring number is：Corundum aggregate 20-25 parts that corundum aggregate 30-45 parts that granularity is 3-1mm, granularity are 1-0mm, corundum fine powder 15-25 parts, SiO2Micro mist 3-6 parts, Si powder 10-15 parts, bonding agent addition are the 3-6% of original material gross weight.
- 2. a kind of microwave metallurgical kiln car corundum-silicon oxynitride composite refractory according to claim 1, its feature exist In：SiO2Micro mist is more than one or both of ultra-fine natural quartz emery dust, silicon powder and gaseous oxidation silicon powder.
- 3. a kind of microwave metallurgical kiln car corundum-silicon oxynitride composite refractory according to claim 2, its feature exist In：SiO2Micro mist purity >=98%, particle diameter are less than 10 μm.
- 4. a kind of microwave metallurgical kiln car corundum-silicon oxynitride composite refractory according to claim 1, its feature exist In：Si powder purity >=99%, granularity≤0.045mm.
- 5. a kind of microwave metallurgical kiln car corundum-silicon oxynitride composite refractory according to claim 1, its feature exist In：Bonding agent is one or more of compound in phenolic resin, dextrin, polyvinyl alcohol, carboxymethyl cellulose, spent pulping liquor.
- A kind of 6. preparation side of microwave metallurgical kiln car corundum-silicon oxynitride composite refractory according to claim 1 Method, it is characterised in that：Step 1: first by corundum fine powder 15-25 parts, SiO2Micro mist 3-6 parts, Si powder 10-15 parts, are put into ball mill According to corundum ball and material ratio 1:1, in the case where rotating speed is 1000 ~ 1200rpm, 120-180 minutes are ground, it is thin to obtain premixing Powder；Step 2: by corundum aggregate 30-45 parts that granularity is 3-1mm, granularity is that 1-0mm corundum aggregate 20-25 parts pour into mixed grind In machine, 3-6 is then addedwt% bonding agents, kolleroang stirring 5-10min is opened, makes bonding agent uniform adhesion in corundum in granules table Face soaks with it, adds the premixing fine powder that step 1 obtains, and stirs 10-20min, material is sufficiently mixed uniformly；Step 3rd, mixed material is fitted into storing 12-24h in the air atmosphere that air humidity is 50-60% at room temperature in hermetic bag to be stranded Material；Step 4: after ageing mixture, with hydraulic press under 120MPa pressure adobe is made in well mixed material, by the brick after shaping Base is dried 24 hours in 120 DEG C of drying boxes；Step 5: being transported into after dried sample is weighed in nitriding furnace, fire door is sealed Nitrogen is passed through, 1100 DEG C are warming up to 5-8 DEG C/min heating rate under pressure-fired flowing nitrogen atmosphere, after being incubated 2 hours 1450 DEG C are warming up to 1-5 DEG C/min speed again and are incubated 24 hours, then cool to room temperature with the furnace, you can obtain corundum-oxygen Silicon nitride composite refractory.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111138205A (en) * | 2020-02-18 | 2020-05-12 | 中钢洛耐新材料科技有限公司 | Anti-erosion sialon corundum product and preparation method thereof |
| CN115745579A (en) * | 2023-01-02 | 2023-03-07 | 洛阳科创新材料股份有限公司 | Composite air brick with high strength and low heat conductivity coefficient and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103896610A (en) * | 2014-03-11 | 2014-07-02 | 郑州大学 | Method for manufacturing silicon oxynitride-bonded high aluminum-silicon carbide prefabricated member |
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2017
- 2017-08-24 CN CN201710736091.9A patent/CN107417287B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103896610A (en) * | 2014-03-11 | 2014-07-02 | 郑州大学 | Method for manufacturing silicon oxynitride-bonded high aluminum-silicon carbide prefabricated member |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111138205A (en) * | 2020-02-18 | 2020-05-12 | 中钢洛耐新材料科技有限公司 | Anti-erosion sialon corundum product and preparation method thereof |
| CN115745579A (en) * | 2023-01-02 | 2023-03-07 | 洛阳科创新材料股份有限公司 | Composite air brick with high strength and low heat conductivity coefficient and preparation method thereof |
| CN115745579B (en) * | 2023-01-02 | 2023-09-22 | 洛阳科创新材料股份有限公司 | Composite air brick with high strength and low heat conductivity coefficient and preparation method thereof |
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