CN107324818A - A kind of Tercod and preparation method thereof - Google Patents
A kind of Tercod and preparation method thereof Download PDFInfo
- Publication number
- CN107324818A CN107324818A CN201710444747.XA CN201710444747A CN107324818A CN 107324818 A CN107324818 A CN 107324818A CN 201710444747 A CN201710444747 A CN 201710444747A CN 107324818 A CN107324818 A CN 107324818A
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- parts
- powder
- coke
- tercod
- sintering
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- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 66
- 238000005245 sintering Methods 0.000 claims abstract description 43
- 239000000843 powder Substances 0.000 claims abstract description 40
- 239000000571 coke Substances 0.000 claims abstract description 33
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 33
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000006004 Quartz sand Substances 0.000 claims abstract description 25
- 239000002994 raw material Substances 0.000 claims abstract description 19
- 239000000203 mixture Substances 0.000 claims abstract description 17
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000009768 microwave sintering Methods 0.000 claims abstract description 13
- 238000002156 mixing Methods 0.000 claims abstract description 12
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 12
- 239000004411 aluminium Substances 0.000 claims abstract description 9
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 9
- YDEXUEFDPVHGHE-GGMCWBHBSA-L disodium;(2r)-3-(2-hydroxy-3-methoxyphenyl)-2-[2-methoxy-4-(3-sulfonatopropyl)phenoxy]propane-1-sulfonate Chemical compound [Na+].[Na+].COC1=CC=CC(C[C@H](CS([O-])(=O)=O)OC=2C(=CC(CCCS([O-])(=O)=O)=CC=2)OC)=C1O YDEXUEFDPVHGHE-GGMCWBHBSA-L 0.000 claims abstract description 9
- 239000011819 refractory material Substances 0.000 claims abstract description 9
- 229910052582 BN Inorganic materials 0.000 claims abstract description 8
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims abstract description 8
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 8
- 239000010445 mica Substances 0.000 claims abstract description 8
- 229910052618 mica group Inorganic materials 0.000 claims abstract description 8
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 8
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910021538 borax Inorganic materials 0.000 claims abstract description 7
- UQGFMSUEHSUPRD-UHFFFAOYSA-N disodium;3,7-dioxido-2,4,6,8,9-pentaoxa-1,3,5,7-tetraborabicyclo[3.3.1]nonane Chemical compound [Na+].[Na+].O1B([O-])OB2OB([O-])OB1O2 UQGFMSUEHSUPRD-UHFFFAOYSA-N 0.000 claims abstract description 7
- 235000010339 sodium tetraborate Nutrition 0.000 claims abstract description 7
- 239000004328 sodium tetraborate Substances 0.000 claims abstract description 7
- 230000032683 aging Effects 0.000 claims abstract description 6
- 235000013312 flour Nutrition 0.000 claims abstract description 6
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 27
- 238000000034 method Methods 0.000 claims description 22
- 230000008569 process Effects 0.000 claims description 19
- 238000010438 heat treatment Methods 0.000 claims description 15
- 150000001875 compounds Chemical class 0.000 claims description 12
- 239000003795 chemical substances by application Substances 0.000 claims description 11
- 230000004048 modification Effects 0.000 claims description 10
- 238000012986 modification Methods 0.000 claims description 10
- 238000010792 warming Methods 0.000 claims description 10
- 229920003257 polycarbosilane Polymers 0.000 claims description 8
- 238000012545 processing Methods 0.000 claims description 8
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 7
- 239000012298 atmosphere Substances 0.000 claims description 7
- 230000001681 protective effect Effects 0.000 claims description 6
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 5
- 229920005610 lignin Polymers 0.000 claims description 5
- 238000007781 pre-processing Methods 0.000 claims description 5
- 229910052708 sodium Inorganic materials 0.000 claims description 5
- 239000011734 sodium Substances 0.000 claims description 5
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims description 5
- 239000011335 coal coke Substances 0.000 claims description 4
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 4
- 238000000498 ball milling Methods 0.000 claims description 3
- 230000035939 shock Effects 0.000 abstract description 13
- 229920000548 poly(silane) polymer Polymers 0.000 abstract description 4
- 239000000463 material Substances 0.000 description 35
- 229910052799 carbon Inorganic materials 0.000 description 13
- 238000006243 chemical reaction Methods 0.000 description 11
- 239000013078 crystal Substances 0.000 description 9
- 239000000835 fiber Substances 0.000 description 8
- YGANSGVIUGARFR-UHFFFAOYSA-N dipotassium dioxosilane oxo(oxoalumanyloxy)alumane oxygen(2-) Chemical compound [O--].[K+].[K+].O=[Si]=O.O=[Al]O[Al]=O YGANSGVIUGARFR-UHFFFAOYSA-N 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 229910052627 muscovite Inorganic materials 0.000 description 5
- 238000007254 oxidation reaction Methods 0.000 description 5
- 230000035882 stress Effects 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 239000003963 antioxidant agent Substances 0.000 description 4
- 230000003078 antioxidant effect Effects 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
- 238000007873 sieving Methods 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 239000003610 charcoal Substances 0.000 description 3
- 239000003245 coal Substances 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 239000000376 reactant Substances 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 2
- 229910052581 Si3N4 Inorganic materials 0.000 description 2
- 229910003978 SiClx Inorganic materials 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 2
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 229910052796 boron Inorganic materials 0.000 description 2
- 239000011449 brick Substances 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 238000010310 metallurgical process Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000005011 phenolic resin Substances 0.000 description 2
- 229920001568 phenolic resin Polymers 0.000 description 2
- 239000012779 reinforcing material Substances 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000005945 translocation Effects 0.000 description 2
- 229910052726 zirconium Inorganic materials 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000002679 ablation Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000003064 anti-oxidating effect Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000007767 bonding agent Substances 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 230000009970 fire resistant effect Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000002309 gasification Methods 0.000 description 1
- 229910021397 glassy carbon Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000003863 metallic catalyst Substances 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 125000000325 methylidene group Chemical group [H]C([H])=* 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- VDGJOQCBCPGFFD-UHFFFAOYSA-N oxygen(2-) silicon(4+) titanium(4+) Chemical compound [Si+4].[O-2].[O-2].[Ti+4] VDGJOQCBCPGFFD-UHFFFAOYSA-N 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000002006 petroleum coke Substances 0.000 description 1
- -1 poly- carbon silicon Alkane Chemical class 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
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Abstract
The present invention relates to technical field of refractory materials.A kind of Tercod, includes the raw material of following parts by weight：50 ~ 70 parts of silicon carbide powder, 4 ~ 12 parts of silica flour, 15 ~ 20 parts of aluminium powder, 2 ~ 5 parts of titanium dioxide powder, 47 parts of alumina powder, 3 ~ 5 parts of white mica powder, 2 ~ 4 parts of sericite in powder, 2 ~ 6 parts of boron nitride powder, 1 ~ 3 part of Paris white, 1 ~ 3 part of silicon dioxide powder, 5 ~ 6 parts of sodium lignin sulfonate, 1 ~ 2 part of graphite powder, 5 ~ 10 parts of sodium tetraborate, 10 ~ 15 parts of polysilane.A kind of preparation method of Tercod, comprises the following steps：Mixed after coke is pre-processed with quartz sand and carry out microwave sintering again, obtain silicon carbide powder, then by sodium lignin sulfonate and water with 1:1 ratio mixing, is sufficiently mixed after then adding remaining raw material, then compressing drying and then sintering after ageing mixture.The present invention has good intensity, toughness and strong thermal shock resistance and inoxidizability.
Description
Technical field
The present invention relates to a kind of technical field of refractory materials, in particular to a kind of Tercod and its preparation
Method.
Background technology
In metallurgical process, smelting furnace liner is frequently subjected to temperature violent change with molten steel water conservancy diversion, flow-controlled device, to these position institutes
The refractory material requirement used has very high resistance to heat shocks.Because graphite is in environment temperature violent change, heat can be quickly conducted
Amount, reduces material internal thermograde, reduces thermal stress, so that protection materials thermal shock is not ftractureed, so carbon containing refractory is wide
It is general to be applied to the strong position of thermal shock in metallurgical process.
Current carbon containing refractory generally makees bonding agent using phenolic resin, and high temperature forms vitreous carbon combined fire resistant after burning till
Material.But there are two shortcomings in the combination carbon of this glassy state：One is that inoxidizability is poor, the glass formed after phenolic resin charing
Glass carbon begins to oxidation ablation from 500 DEG C, with reference to the oxidation of carbon material can be caused to lose adhesion, structure becomes loose, easily
Peel off or be melted metal erosion；Two be low intensity, in glass fragility, in the presence of certain stress, it may occur that cracking situation
Even can occur brittle fracture.
It is poor for the inoxidizability that combines carbon, it is general using it is internal mix antioxidant and surface application antioxidant coating come
Protect carbon containing refractory.The antioxidant mixed is generally some metal dusts more oxidizable than combining carbon, because its
Incorporation is limited, so antioxidation can only be played in a short time.Smelting furnace liner carbon containing refractory and molten metal
Water conservancy diversion, flow control submerge position in the molten metal with carbon containing refractory, and the inoxidzable coating on surface is by molten metal
Corrosion can gradually lose the protection against oxidation to carbonaceous material.Some bituminizing carbon containing refractories, due to surface it is smooth and
The limitation of use condition is difficult to apply antioxidant coating, is easy to occur carbon combination oxidation in baking.
Therefore a kind of carborundum fire proofed wood with good intensity, toughness and strong thermal shock resistance inoxidizability is needed at present
Material.
The content of the invention
There is provided a kind of with good intensity, toughness and strong thermal shock resistance, the carbon of inoxidizability in order to solve the above problems
SiClx refractory material, the present invention uses following technical method：
A kind of Tercod, includes the raw material of following parts by weight：
It is 50 ~ 70 parts of silicon carbide powder, 4 ~ 12 parts of silica flour, 15 ~ 20 parts of aluminium powder, 2 ~ 5 parts of titanium dioxide powder, 4-7 parts of alumina powder, white
3 ~ 5 parts of mica powder, 2 ~ 4 parts of sericite in powder, 2 ~ 6 parts of boron nitride powder, 1 ~ 3 part of Paris white, 1 ~ 3 part of silicon dioxide powder, lignin
5 ~ 6 parts of sodium sulfonate, 1 ~ 2 part of graphite powder, 5 ~ 10 parts of sodium tetraborate, 10 ~ 15 parts of polysilane.
First present invention employs the scheme that white mica powder and thin,tough silk white mica powder are used in conjunction with, being firstly added muscovite can be with
The toughness and mechanical strength of material are improved, and sericite belongs to monoclinic crystal, can be with the wearability of reinforcing material, both make in cooperation
Used time, muscovite and sericite are filled in the space between carborundum crystals, and sericite can be filled out because crystal is finer and closely woven
The gap that muscovite can not be filled is charged into, is easy to the mixing of raw material, muscovite and thin,tough silk muscovite melt at high temperature, enhance crystalline substance
Bond strength between body, further increases the toughness and internal intensity of refractory material.
Secondly present invention uses sodium lignin sulfonate, due to there are various activity in the institutional framework of sodium lignin sulfonate
Base, thus hydrogen bond action can occur with carborundum crystals surface, the structural strength of crystal can be strengthened, so as to strengthen refractory material
Intensity.
Polysilane makes the methyl on side chain in the form of methylene, led in the hot translocation reaction of heating process in sintering process
Between the silicon atom for entering main chain, Polycarbosilane is formed, and Polycarbosilane can further be cracked into silicon carbide fibre containing zirconium.High temperature
The silicon carbide fibre formed is cracked in sintering processes, can be in one layer of fine and close titanium dioxide of Surface Creation due to the influence of temperature
Silicon, with the extension of high-temperature oxydation time, this layer of compact silicon dioxide progressive additive gets up internal package, prevents further oxygen
Change, so that the inoxidizability of refractory brick is enhanced, and also other materials can be bonded by silicon carbide fibre containing zirconium, be enhanced
The intensity and toughness and thermal shock resistance of the present invention, so that refractory brick has excellent slag-resistant permeability, resistance to flaking and resisted
The slagging of retractory.
The silicon carbide fibre that Polycarbosilane is formed has good tensile strength, heat-transfer capability and relatively low thermal expansion system
Number.Because the tensile strength of material is high, therefore improve that the internal stress that material can bear is big, reduce that material ftractures can
Energy；And the thermal conductivity height of material can allow material quickly to conduct heat when heated, so as to reduce material internal
Thermograde, so as to reduce the internal stress that material internal is produced because of thermograde；And low coefficient of thermal expansion causes material
Formation internal stress is small when inside has thermograde, and it is the possibility ftractureed in heating to reduce material.In general, poly- carbon silicon
Alkane effectively reduces the internal stress of material internal, enhances the resistance to heat shocks of material, the situation for preventing material from ftractureing, simultaneously
Also increase the inoxidizability of material.
In addition invention also uses the scheme that boron nitride, aluminium powder, alumina powder and sodium tetraborate are used cooperatively, in sintering
During the compound of boron carbide-aluminium can be generated in carborundum, the compound and silicon carbide fibre are collectively forming network structure,
Can be with the toughness of reinforcement material, wearability, thermal conductivity and impact strength, while playing improvement material with titanium dioxide collective effect
The effect of the surface wettability of material, can cause carborundum and other raw materials are easy to infiltration, so as to reduce reaction temperature and
Sintering time, it is cost-effective.Simultaneous reactions also have a small amount of silicon nitride and produced, and a small amount of silicon nitride can play cohesive carbonization
Silicon crystal can also suppress the growth of crystal so as to the effect of the thermal shock resistance of reinforcing material, in addition boron nitride so that the present invention
The granularity of interior crystal is more fine and closely woven, contributes to the intensity of the enhancing present invention.
And due to there is the addition of the materials such as boron and aluminium in the silicon carbide fibre produced, make silicon carbide fibre stability and
Heat-resisting quantity is further improved, while can prevent silicon carbide fibre from softening in high temperature to cause material structure to be destroyed, influence
The intensity of material.
Preferably, described silicon carbide powder is made by the raw material of following parts by weight：55 ~ 60 parts of quartz sand, coke 40 ~
45 parts.
In the present invention, the higher coke of the parts by weight of quartz sand is less, is so fully protected during carborundum is prepared
Demonstrate,prove quartz sand and wrapped coke gasification reaction, contribute to the progress of reaction
Preferably, being sieved using preceding to described quartz sand, quartz sand of the diameter at 1 ~ 5 micron is taken.
Preferably, described silicon dioxide powder passes through modification, described modification comprises the following steps：
A. dodecyl sodium sulfate is mixed with water, configuration concentration is 0.2 ~ 0.5mol/L modifying agent；
B. by modifying agent and silicon dioxide powder with 2：1 mass ratio is mixed, and is then stirred, is stirred under the conditions of 75 ~ 90 DEG C
Mix rotating speed is 400 ~ 450r/min, and mixing time is 1 ~ 2h.
By being modified processing to silicon dioxide powder, it is mixed with by dodecyl sodium sulfate and water as modification
Agent, is be combined with each other by dodecyl sodium sulfate and silica, forms monomolecular adsorption layer, so as to strengthen silica
Dispersiveness, so as to improve the activity of silica, improve the reciprocation of silica and carborundum, help titanium dioxide
Silicon is preferably distributed in material, because the addition of silica is conducive to that the inoxidizability of material can be improved.
A kind of preparation method of Tercod, comprises the following steps：
（1）Prepare silicon carbide powder：After coke is pre-processed, the coke by pretreatment is mixed with quartz sand, obtained
Mixture, described mixture is put into microwave agglomerating furnace, is carried out microwave sintering, is obtained silicon carbide powder；
（2）Dispensing prepares：By sodium lignin sulfonate and water with 1:1 ratio mixing, is sufficiently mixed after then adding remaining raw material,
Again compound is obtained after 3 ~ 4h of ageing mixture；
（3）Green compact processing：Will be in above-mentioned steps（2）In compound be pressed, green compact are obtained, then by described life
Base is dried；
（4）Sintering processes：Will be in step（3）Described in the green compact of drying be put into sintering furnace and be sintered, obtain carborundum
Refractory material finished product.
Preferably, in step（1）Described in coke use ature of coal coke, described preprocessing process is will be described
Coke carries out ball milling, and sieving obtains coke powder after drying, and takes coke powder of the diameter between 50 ~ 100 microns.
First, the present invention uses ature of coal coke, because ature of coal coke has the characteristic for being easy to grinding compared with petroleum coke, is easy to
Ball milling operation is carried out, because reaction is that occur on the interface of quartz sand and coke, is occurred instead because quartz sand wraps coke
Should, therefore the granule size of coke directly determines the granule size of carborundum, the granularity of coke is smaller in general, the carbon of production
SiClx granularity is smaller, and the granularity of carborundum is small, and has under this reaction temperature a silicon carbide whisker generation, and crystal is fine and closely woven and crystalline substance
The link of the whisker of carborundum must be both contributed to, the intensity and toughness of carborundum is favorably improved.But, implemented in the present invention
Cheng Zhong, it is found that when coke diameter is below 50 microns, the phenomenon that carborundum is reunited has instead resulted in the intensity of carborundum
Decline, so the coke powder present invention employs diameter between 50 ~ 100 microns.
Preferably, in step（1）Described in microwave sintering heating rate be 40 ~ 45 DEG C/min, sintering temperature is
1400~1600℃。
The present invention produces carborundum by microwave sintering, first microwave sintering be the special wave band that has using microwave with
The basic fine structure coupling of material and produce heat, the dielectric loss of material makes its material integrally be heated to sintering temperature and reality
The method being now densified, traditional heating is different with microwave heating, and different heating mode causes different reaction process.Add in tradition
Hanker, reactant is by heat radiation and conduction heating, and reactant external temperature is reacted first since outside higher than inside, raw
Into CO can vapor away, be unfavorable for CO partial pressures raising and SiC whiskers synthesis.In microwave heating, reactant internal temperature
It is higher, react first since inside, be conducive to CO to accumulate, meanwhile, microwave heating ramp rate is fast, can give birth within a short period of time
Into a large amount of SiO and CO, be conducive to increasing partial pressure, promote the progress and the generation of SiC whiskers of gas-gas reaction.Therefore, using micro-
Wave heating is expected to significantly improve the yield of whisker, while avoiding introducing impurity using metallic catalyst, simultaneous reactions speed is fast
The reaction time can be reduced, improving efficiency reduces cost.
Preferably, in step（4）During, when being warming up to 400 ~ 500 DEG C keeping temperature it is interval herein in 1 ~ 2h, followed by
Continuous to be warming up to sintering temperature, sintering temperature is 1500 ~ 1700 DEG C, and sintering time is 10 ~ 15h, and nitrogen is used in sintering process
Atmosphere is used as protective atmosphere.
It can ensure that polysilane is fully carried out in the hot translocation reaction of heating process in 400 ~ 500 DEG C of insulating processes, fully
Polycarbosilane is generated, influence of the air to sintering can be prevented using nitrogen as protective atmosphere, prevent Tercod from existing
Being oxidized in sintering procedure causes the situation of cracking to occur.
The beneficial effects of the present invention are：（1）Material produced by the invention has good intensity, toughness and strong anti-thermal shock
Property（2）Material has good inoxidizability（3）The heat-agglomerating process time of the present invention is short, and energy consumption is low.
Embodiment
Embodiment 1
A kind of Tercod includes the raw material of following parts by weight：
It is 50 ~ 70 parts of silicon carbide powder, 4 ~ 12 parts of silica flour, 15 ~ 20 parts of aluminium powder, 2 ~ 5 parts of titanium dioxide powder, 4-7 parts of alumina powder, white
3 ~ 5 parts of mica powder, 2 ~ 4 parts of sericite in powder, 2 ~ 6 parts of boron nitride powder, 1 ~ 3 part of Paris white, 1 ~ 3 part of silicon dioxide powder, lignin
5 ~ 6 parts of sodium sulfonate, 1 ~ 2 part of graphite powder, 5 ~ 10 parts of sodium tetraborate, 10 ~ 15 parts of Polycarbosilane.
And silicon carbide powder is made by the raw material of following parts by weight：55 parts of quartz sand, 40 parts of coke, coke are burnt using ature of coal
Charcoal.
Described quartz sand is sieved using preceding first, the quartz sand of 1 micron of diameter is taken.
Then modification is passed through to silicon dioxide powder, described modification comprises the following steps：
A. dodecyl sodium sulfate is mixed with water, configuration concentration is 0.5mol/L modifying agent；
B. by modifying agent and silicon dioxide powder with 2：1 mass ratio is mixed, and is then stirred under the conditions of 90 DEG C, and stirring turns
Speed is 450r/min, and mixing time is 2h.
Then a kind of preparation of Tercod of the invention is carried out, preparation method comprises the following steps：
（1）Prepare silicon carbide powder：After coke is pre-processed, described preprocessing process is that described coke is carried out into ball
Mill, dry after sieving obtain coke powder, take coke powder of the diameter at 50 microns, then by by pretreatment coke with
Quartz sand is mixed, and obtains mixture, described mixture is put into microwave agglomerating furnace, carries out microwave sintering, described microwave
Sintering heating rate is 40 DEG C/min, and sintering temperature is 1500 DEG C, obtains silicon carbide powder；
（2）Dispensing prepares：By sodium lignin sulfonate and water with 1:1 ratio mixing, is sufficiently mixed after then adding remaining raw material,
Again compound is obtained after ageing mixture 4h；
（3）Green compact processing：Will be in above-mentioned steps（2）In compound be pressed, green compact are obtained, then by described life
Base is dried；
（4）Sintering processes：Will be in step（3）Described in the green compact of drying be put into sintering furnace and be sintered, be warming up to 500 DEG C
When keeping temperature it is interval herein in 2h be further continued for being warming up to sintering temperature, sintering temperature is 1700 DEG C, and sintering time is 15h,
Protective atmosphere is used as using nitrogen atmosphere in sintering process.
Embodiment 2
A kind of Tercod includes the raw material of following parts by weight：
It is 50 ~ 70 parts of silicon carbide powder, 4 ~ 12 parts of silica flour, 15 ~ 20 parts of aluminium powder, 2 ~ 5 parts of titanium dioxide powder, 4-7 parts of alumina powder, white
3 ~ 5 parts of mica powder, 2 ~ 4 parts of sericite in powder, 2 ~ 6 parts of boron nitride powder, 1 ~ 3 part of Paris white, 1 ~ 3 part of silicon dioxide powder, lignin
5 ~ 6 parts of sodium sulfonate, 1 ~ 2 part of graphite powder, 5 ~ 10 parts of sodium tetraborate, 10 ~ 15 parts of Polycarbosilane.
And silicon carbide powder is made by the raw material of following parts by weight：55 parts of quartz sand, 40 parts of coke, coke are burnt using ature of coal
Charcoal.
Described quartz sand is sieved using preceding first, the quartz sand of 1 micron of diameter is taken.
Then modification is passed through to silicon dioxide powder, described modification comprises the following steps：
A. dodecyl sodium sulfate is mixed with water, configuration concentration is 0.5mol/L modifying agent；
B. by modifying agent and silicon dioxide powder with 2：1 mass ratio is mixed, and is then stirred under the conditions of 90 DEG C, and stirring turns
Speed is 450r/min, and mixing time is 2h.
Then a kind of preparation of Tercod of the invention is carried out, preparation method comprises the following steps：
（1）Prepare silicon carbide powder：After coke is pre-processed, described preprocessing process is that described coke is carried out into ball
Mill, dry after sieving obtain coke powder, take coke powder of the diameter at 50 microns, then by by pretreatment coke with
Quartz sand is mixed, and obtains mixture, described mixture is put into microwave agglomerating furnace, carries out microwave sintering, described microwave
Sintering heating rate is 40 DEG C/min, and sintering temperature is 1500 DEG C, obtains silicon carbide powder；
（2）Dispensing prepares：By sodium lignin sulfonate and water with 1:1 ratio mixing, is sufficiently mixed after then adding remaining raw material,
Again compound is obtained after ageing mixture 4h；
（3）Green compact processing：Will be in above-mentioned steps（2）In compound be pressed, green compact are obtained, then by described life
Base is dried；
（4）Sintering processes：Will be in step（3）Described in the green compact of drying be put into sintering furnace and be sintered, be warming up to 500 DEG C
When keeping temperature it is interval herein in 2h be further continued for being warming up to sintering temperature, sintering temperature is 1700 DEG C, and sintering time is 15h,
Protective atmosphere is used as using nitrogen atmosphere in sintering process.
Embodiment 3
A kind of Tercod includes the raw material of following parts by weight：
It is 50 ~ 70 parts of silicon carbide powder, 4 ~ 12 parts of silica flour, 15 ~ 20 parts of aluminium powder, 2 ~ 5 parts of titanium dioxide powder, 4-7 parts of alumina powder, white
3 ~ 5 parts of mica powder, 2 ~ 4 parts of sericite in powder, 2 ~ 6 parts of boron nitride powder, 1 ~ 3 part of Paris white, 1 ~ 3 part of silicon dioxide powder, lignin
5 ~ 6 parts of sodium sulfonate, 1 ~ 2 part of graphite powder, 5 ~ 10 parts of sodium tetraborate, 10 ~ 15 parts of Polycarbosilane.
And silicon carbide powder is made by the raw material of following parts by weight：55 parts of quartz sand, 40 parts of coke, coke are burnt using ature of coal
Charcoal.
Described quartz sand is sieved using preceding first, the quartz sand of 1 micron of diameter is taken.
Then modification is passed through to silicon dioxide powder, described modification comprises the following steps：
A. dodecyl sodium sulfate is mixed with water, configuration concentration is 0.5mol/L modifying agent；
B. by modifying agent and silicon dioxide powder with 2：1 mass ratio is mixed, and is then stirred under the conditions of 90 DEG C, and stirring turns
Speed is 450r/min, and mixing time is 2h.
Then a kind of preparation of Tercod of the invention is carried out, preparation method comprises the following steps：
（1）Prepare silicon carbide powder：After coke is pre-processed, described preprocessing process is that described coke is carried out into ball
Mill, dry after sieving obtain coke powder, take coke powder of the diameter at 50 microns, then by by pretreatment coke with
Quartz sand is mixed, and obtains mixture, described mixture is put into microwave agglomerating furnace, carries out microwave sintering, described microwave
Sintering heating rate is 40 DEG C/min, and sintering temperature is 1500 DEG C, obtains silicon carbide powder；
（2）Dispensing prepares：By sodium lignin sulfonate and water with 1:1 ratio mixing, is sufficiently mixed after then adding remaining raw material,
Again compound is obtained after ageing mixture 4h；
（3）Green compact processing：Will be in above-mentioned steps（2）In compound be pressed, green compact are obtained, then by described life
Base is dried；
（4）Sintering processes：Will be in step（3）Described in the green compact of drying be put into sintering furnace and be sintered, be warming up to 500 DEG C
When keeping temperature it is interval herein in 2h be further continued for being warming up to sintering temperature, sintering temperature is 1700 DEG C, and sintering time is 15h,
Protective atmosphere is used as using nitrogen atmosphere in sintering process.
The thermal conductivity factor of the preferred embodiment of the present invention 3 is 15w/m.k, the apparent porosity 10% of material, refractoriness under load
1690 DEG C, cold crushing strength 40MPa, hardness (HRA) is 68.4, for the detection of thermal shock resistance.
The thermal conductivity factor of the preferred embodiment of the present invention 3 is 20w/m.k, the apparent porosity 8% of material, refractoriness under load
1790 DEG C, the MPa of cold crushing strength 55, hardness (HRA) is 84.6, for the detection of thermal shock resistance, of the invention by embodiment 3
Material by 1450 degrees Celsius 3 hours processing survey its rupture strength, rupture strength be 19.8MPa then 1100 degrees Celsius guarantor
Chilling in 20 degrees Celsius of cold water again after warm 20min, is repeated 10 times, rupture strength is 11.2MPa.
Tercod of the present invention has good intensity, toughness and strong thermal shock resistance inoxidizability.
Claims (8)
1. a kind of Tercod, it is characterised in that include the raw material of following parts by weight：
It is 50 ~ 70 parts of silicon carbide powder, 4 ~ 12 parts of silica flour, 15 ~ 20 parts of aluminium powder, 2 ~ 5 parts of titanium dioxide powder, 4-7 parts of alumina powder, white
3 ~ 5 parts of mica powder, 2 ~ 4 parts of sericite in powder, 2 ~ 6 parts of boron nitride powder, 1 ~ 3 part of Paris white, 1 ~ 3 part of silicon dioxide powder, lignin
5 ~ 6 parts of sodium sulfonate, 1 ~ 2 part of graphite powder, 5 ~ 10 parts of sodium tetraborate, 10 ~ 15 parts of Polycarbosilane.
2. a kind of Tercod according to claim 1, it is characterised in that：Described silicon carbide powder is by following
The raw material of parts by weight is made：55 ~ 60 parts of quartz sand, 40 ~ 45 parts of coke.
3. a kind of Tercod according to claim 2, it is characterised in that：It is preceding to described quartz sand using
Sieved, take quartz sand of the diameter at 1 ~ 5 micron.
4. a kind of Tercod according to claim 1, it is characterised in that：Described silicon dioxide powder is by changing
Property processing, described modification comprises the following steps：
A. dodecyl sodium sulfate is mixed with water, configuration concentration is 0.2 ~ 0.5mol/L modifying agent；
B. by modifying agent and silicon dioxide powder with 2：1 mass ratio is mixed, and is then stirred, is stirred under the conditions of 75 ~ 90 DEG C
Mix rotating speed is 400 ~ 450r/min, and mixing time is 1 ~ 2h.
5. a kind of preparation method of Tercod according to one of claim 1-4, it is characterised in that including with
Lower step：
（1）Prepare silicon carbide powder：After coke is pre-processed, the coke by pretreatment is mixed with quartz sand, obtained
Mixture, described mixture is put into microwave agglomerating furnace, is carried out microwave sintering, is obtained silicon carbide powder；
（2）Dispensing prepares：By sodium lignin sulfonate and water with 1:1 ratio mixing, is sufficiently mixed after then adding remaining raw material,
Again compound is obtained after 3 ~ 4h of ageing mixture；
（3）Green compact processing：Will be in above-mentioned steps（2）In compound be pressed, green compact are obtained, then by described life
Base is dried；
（4）Sintering processes：Will be in step（3）Described in the green compact of drying be put into sintering furnace and be sintered, obtain carborundum
Refractory material finished product.
6. a kind of preparation method of Tercod according to claim 5, it is characterised in that：In step（1）In
Described coke uses ature of coal coke, and described preprocessing process is that described coke is carried out into ball milling, sieves and obtains after drying
Coke powder, takes coke powder of the diameter between 50 ~ 100 microns.
7. a kind of preparation method of Tercod according to claim 5, it is characterised in that：In step（1）In
Described microwave sintering heating rate is 40 ~ 45 DEG C/min, and sintering temperature is 1400 ~ 1600 DEG C.
8. a kind of preparation method of Tercod according to claim 5, it is characterised in that：In step（4）Cross
Interval interior 1 ~ 2h is further continued for being warming up to sintering temperature keeping temperature herein when 400 ~ 500 DEG C are warming up in journey, and sintering temperature is
1500 ~ 1700 DEG C, sintering time is 10 ~ 15h, and protective atmosphere is used as using nitrogen atmosphere in sintering process.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710444747.XA CN107324818A (en) | 2017-06-13 | 2017-06-13 | A kind of Tercod and preparation method thereof |
Applications Claiming Priority (1)
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| CN111269017A (en) * | 2020-03-02 | 2020-06-12 | 宜兴市海科耐火材料制品有限公司 | Special high-temperature-resistant anti-corrosion lining material for hazardous waste gas melting furnace and preparation method thereof |
| CN112028644A (en) * | 2020-08-17 | 2020-12-04 | 武汉重远炉窑工程技术服务有限公司 | Fire-resistant binder for coke oven and preparation method thereof |
| CN112552053A (en) * | 2020-12-08 | 2021-03-26 | 首钢集团有限公司 | Silicon carbide refractory brick for coke dry quenching furnace and preparation method thereof |
| CN115028463A (en) * | 2022-05-23 | 2022-09-09 | 中钢洛耐(洛阳)新材料有限公司 | Processing technology of refractory brick with low thermal conductivity |
| CN115806443A (en) * | 2023-02-06 | 2023-03-17 | 成都超纯应用材料有限责任公司 | Connecting material of silicon carbide substrate, preparation method and application |
| CN116143523A (en) * | 2023-04-21 | 2023-05-23 | 成都超纯应用材料有限责任公司 | Pressureless sintered silicon carbide blank intermediate, silicon carbide ceramic and preparation method |
| CN116179919A (en) * | 2023-03-07 | 2023-05-30 | 宋艺楠 | Nano metal composite ceramic material and preparation method thereof |
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| CN116143523A (en) * | 2023-04-21 | 2023-05-23 | 成都超纯应用材料有限责任公司 | Pressureless sintered silicon carbide blank intermediate, silicon carbide ceramic and preparation method |
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