CN1562883A - Firebrick made from silicom nitride combined with silicon carbide in use for sidewall of electrobath for making aluminium - Google Patents
Firebrick made from silicom nitride combined with silicon carbide in use for sidewall of electrobath for making aluminium Download PDFInfo
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- CN1562883A CN1562883A CNA2004100307868A CN200410030786A CN1562883A CN 1562883 A CN1562883 A CN 1562883A CN A2004100307868 A CNA2004100307868 A CN A2004100307868A CN 200410030786 A CN200410030786 A CN 200410030786A CN 1562883 A CN1562883 A CN 1562883A
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- silicon carbide
- tib
- add
- refractory brick
- zrb
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 96
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 96
- 229910052782 aluminium Inorganic materials 0.000 title claims description 27
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims description 23
- 239000004411 aluminium Substances 0.000 title description 5
- 150000004767 nitrides Chemical class 0.000 title 1
- 239000000463 material Substances 0.000 claims abstract description 125
- 239000011449 brick Substances 0.000 claims abstract description 98
- 229910052581 Si3N4 Inorganic materials 0.000 claims abstract description 69
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims abstract description 68
- 239000000843 powder Substances 0.000 claims abstract description 24
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 13
- 238000002156 mixing Methods 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims abstract description 10
- 239000000654 additive Substances 0.000 claims abstract description 9
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims abstract description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 53
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 27
- 239000000377 silicon dioxide Substances 0.000 claims description 22
- 238000000034 method Methods 0.000 claims description 18
- 238000005121 nitriding Methods 0.000 claims description 14
- 229910052757 nitrogen Inorganic materials 0.000 claims description 13
- 235000013312 flour Nutrition 0.000 claims description 12
- 238000003825 pressing Methods 0.000 claims description 12
- 239000002245 particle Substances 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 10
- 239000004576 sand Substances 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 7
- 239000004375 Dextrin Substances 0.000 claims description 6
- 229920001353 Dextrin Polymers 0.000 claims description 6
- 235000019425 dextrin Nutrition 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 5
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 3
- 229920005551 calcium lignosulfonate Polymers 0.000 claims description 3
- RYAGRZNBULDMBW-UHFFFAOYSA-L calcium;3-(2-hydroxy-3-methoxyphenyl)-2-[2-methoxy-4-(3-sulfonatopropyl)phenoxy]propane-1-sulfonate Chemical compound [Ca+2].COC1=CC=CC(CC(CS([O-])(=O)=O)OC=2C(=CC(CCCS([O-])(=O)=O)=CC=2)OC)=C1O RYAGRZNBULDMBW-UHFFFAOYSA-L 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 3
- 229910001873 dinitrogen Inorganic materials 0.000 claims 1
- 150000002148 esters Chemical class 0.000 claims 1
- 229910001610 cryolite Inorganic materials 0.000 abstract description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 3
- 150000001875 compounds Chemical class 0.000 abstract description 3
- 239000011863 silicon-based powder Substances 0.000 abstract description 3
- QYEXBYZXHDUPRC-UHFFFAOYSA-N B#[Ti]#B Chemical compound B#[Ti]#B QYEXBYZXHDUPRC-UHFFFAOYSA-N 0.000 abstract 3
- 229910033181 TiB2 Inorganic materials 0.000 abstract 3
- 229910007948 ZrB2 Inorganic materials 0.000 abstract 3
- VWZIXVXBCBBRGP-UHFFFAOYSA-N boron;zirconium Chemical compound B#[Zr]#B VWZIXVXBCBBRGP-UHFFFAOYSA-N 0.000 abstract 3
- 230000000996 additive effect Effects 0.000 abstract 2
- 239000011230 binding agent Substances 0.000 abstract 1
- 239000008151 electrolyte solution Substances 0.000 abstract 1
- 238000010304 firing Methods 0.000 abstract 1
- 239000002994 raw material Substances 0.000 description 9
- KLZUFWVZNOTSEM-UHFFFAOYSA-K Aluminum fluoride Inorganic materials F[Al](F)F KLZUFWVZNOTSEM-UHFFFAOYSA-K 0.000 description 8
- 235000013339 cereals Nutrition 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 5
- 239000011819 refractory material Substances 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- 239000000567 combustion gas Substances 0.000 description 4
- 239000002131 composite material Substances 0.000 description 4
- 239000000295 fuel oil Substances 0.000 description 4
- 238000009413 insulation Methods 0.000 description 4
- 238000010792 warming Methods 0.000 description 4
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical compound [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 3
- 210000005056 cell body Anatomy 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 238000000465 moulding Methods 0.000 description 3
- -1 silicon powder nitride Chemical class 0.000 description 3
- 238000002791 soaking Methods 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000003628 erosive effect Effects 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000012466 permeate Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- IATRAKWUXMZMIY-UHFFFAOYSA-N strontium oxide Chemical compound [O-2].[Sr+2] IATRAKWUXMZMIY-UHFFFAOYSA-N 0.000 description 2
- 230000003245 working effect Effects 0.000 description 2
- 210000004027 cell Anatomy 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
Images
Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/25—Process efficiency
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- Ceramic Products (AREA)
Abstract
The characteristic is that ZrB2 material, TiB2 material as silicon-carbide and fine powder, silicon powder, additional normal temp. binding agent are put into forced stirring sand-mixing machine to be mixed, weight percentage ratio of said compounds are: silicon-carbide 60-80, silicon powder 10-25, ZrB2 and TiB2 0.1-20, firing additive agent 0.2-10, rare-earth oxide is used as additive agent. The ability of anti-corroding of cryolite electrolyte solution of silicon nitride and silicon carbide combined refactory brick is increased and corroding speed is reduced since that ZrB2 and TiB2 materials are added into the refactory brick body.
Description
Technical field
The present invention relates to a kind of high-temperature furnace body---aluminum electrolytic bath side wall is with containing ZrB
2Material and TiB
2Silicon nitride combined silicon carbide refractory brick of material and preparation method thereof belongs to the refractory materials preparing technical field.
Background technology
High-temperature refractory is the structured material with insulation and heat insulating function that uses in the high-temperature furnace body.Nearly all elevated temperature vessel and device interior all need supporting refractory materials to realize the work of the long-term stability of pyritous technical matters condition and protection furnace binding.Supporting refractory materials high temperature resistance melt erosive ability directly affects the life-span of refractory materials and the working life of high temperature service in the high temperature service.
The refractory materials that aluminum electrolytic bath side wall uses at present is carbon refractory brick, silicon nitride combined silicon carbide refractory brick, silicon nitride combined silicon carbide refractory brick and carbon refractory brick compound composite brick structure.Carbon refractory brick is easy to be damaged the problem that causes the aluminium electrolysis cell body life time short by high temperature oxidation, and the anti-sodium aluminum fluoride ionogen of silicon nitride combined silicon carbide refractory brick liquation erosional competency is not very satisfactory, be generally about 5 years the life of domestic aluminium cell cell body, general with the actual service life of external aluminium cell cell body above 7 years, there is bigger gap in the advanced level that reaches more than 12 years that has, and this gap shows that mainly the anti-sodium aluminum fluoride ionogen of silicon nitride combined silicon carbide refractory brick liquation erosional competency is relatively poor.Usually taking method is to increase the working life that the thickness of silicon nitride combined silicon carbide refractory brick prolongs silicon nitride combined silicon carbide refractory brick.But the thickness of increase silicon nitride combined silicon carbide refractory brick is used the brick cost except increase electrolytic aluminum groove side wall, and the manufacturing process of returning silicon nitride combined silicon carbide refractory brick has increased a lot of difficulties.For example, the increase of silicon nitride combined silicon carbide refractory brick thickness, nitrogen can not be penetrated into brick body inside effectively and generate silicon nitride bonded silicon mutually with silica flour generation nitrogenizing reaction in brick body sintering process, cause quality problems such as the inner silicon powder nitride of silicon nitride combined silicon carbide refractory brick is incomplete, the layering of brick body, the brick body is sandwich, brick strength is low easily, thereby directly influence the quality and the result of use of silicon nitride combined silicon carbide refractory brick.
ZrB
2Material and TiB
2Material has good anti-sodium aluminum fluoride ionogen liquation erosional competency, have advantages such as fusing point height, good, the anti-sodium aluminum fluoride corrosive power of thermal conductivity be strong simultaneously, in time below 1100 ℃ resistance of oxidation is preferably arranged, be suitable for very much the high temperature resistant corrosion material of anti-sodium aluminum fluoride of aluminum electrolytic bath side wall liner.But ZrB
2Material and TiB
2Material is the covalent linkage compound, is difficult to be sintered to large compact material brick body.
Summary of the invention
Purpose of the present invention is exactly at the carbon refractory brick of existing aluminum electrolytic bath side wall use at present and the problems referred to above of silicon nitride combined silicon carbide refractory brick existence, and a kind of ZrB of containing is provided
2Material and TiB
2The novel silicon nitride combined silicon carbide refractory brick of material.The present invention is with ZrB
2Material and TiB
2Material joins in the silicon nitride combined silicon carbide material, and the silicon nitride that produces by reaction is with ZrB
2Material and TiB
2Material combines and obtains intensity, forms a kind of ZrB that contains
2Material and TiB
2The novel silicon nitride combined silicon carbide refractory brick of material is used for the good electrolytic aluminum groove side wall of the anti-sodium aluminum fluoride ionogen of requirement liquation erosional competency.
The aluminum electrolytic bath side wall that the present invention proposes is with novel silicon nitride combined silicon carbide refractory brick, and it is characterized in that: interpolation contains ZrB
2Material and TiB
2The embodiment of the silicon nitride combined silicon carbide brick of material is ZrB in the blending process of silicon nitride combined silicon carbide brick
2Material and TiB
2Material is followed silicon-carbide particle and fine powder, silica flour and is added the normal temperature wedding agent and adds together force to stir in the sand mill and mix; The mass percent of total add-on of described silicon carbide is 60~80%, and described silica flour add-on is 10~25%, described interpolation ZrB
2Material and TiB
2The quantity of material is 0.1%~20% of total batching quality, is describedly containing ZrB
2Material and TiB
2The Si of material
3N
4In conjunction with adding sinter additives in the SiC brick be---rare earth oxide, as yttrium oxide, strontium oxide etc., adopt the mode that adds to add, add-on is 0.2~10% of total batching quality.Described normal temperature wedding agent is industrial dextrin solution or calcium lignosulfonate solution or polyvinyl alcohol solution, adopts the mode that adds to add, and add-on is 0.2~10% of total batching quality.
Use in the silicon nitride combined silicon carbide refractory brick the described ZrB that contains at above-mentioned aluminum electrolytic bath side wall
2ZrB in the material
2Greater than 90%, Fe
2O
3Less than 0.3%, granularity is between 1mm to 0.1um; The described TiB that contains
2TiB in the material
2Greater than 90%, Fe
2O
3Less than 0.3%, granularity is between 1mm to 0.1um.
Above-mentioned aluminum electrolytic bath side wall with silicon nitride combined silicon carbide refractory brick in, described silicon-carbide particle be SiC content greater than 97.5%, Fe
2O
3Content is less than 0.5%, and grain graininess is 5.0mm~0.5um, and carbide fine powder is less than 0.08mm.
Above-mentioned aluminum electrolytic bath side wall with novel silicon nitride combined silicon carbide refractory brick in, described silica flour be Si content greater than 97.5%, Fe
2O
3Content is less than 0.5%, and grain graininess is less than the silica fine powder of 0.08mm.
The aluminum electrolytic bath side wall that the present invention the proposes preparation method of silicon nitride combined silicon carbide refractory brick, it is characterized in that: described method is followed successively by:
(1) with ZrB
2Material and TiB
2Material, carbide fine powder, silica fine powder, sinter additives and add the normal temperature wedding agent and add in the mixing machinery together and mix, the material after mixing is pressed into adobe in brick pressing machine; Brick pressing machine can adopt friction press and vibration pressure forming machine.
(2) with the brick bat drying of above-mentioned forming.Drying can adopt steam heating oven dry, far-infrared heating oven dry etc., and the final moisture of drying adobe that makes is less than 0.4%.
(3) above-mentioned drying is good adobe places the nitriding furnace heating to burn till, in the process of heat temperature raising, feed high pure nitrogen simultaneously, the process of heat temperature raising is the process that heats up continuously, heat-up rate is controlled at 20 ℃~300 ℃/hour, during to 1370 ℃~1450 ℃ temperature ranges and be incubated 3~50 hours under this temperature range;
Logical nitrogen can be stopped when (4) being cooled to 900~500 ℃, ZrB can be obtained containing after being cooled to room temperature
2Material and TiB
2The novel silicon nitride combined silicon carbide refractory brick of material.
Since the present invention aluminum electrolytic bath side wall with silicon nitride combined silicon carbide refractory brick body in interpolation contain ZrB
2Material and TiB
2Material, can improve the ability that the anti-sodium aluminum fluoride ionogen of silicon nitride combined silicon carbide refractory brick liquation corrodes and permeates greatly, suffer sodium aluminum fluoride ionogen liquation erosive speed in the aluminium cell thereby effectively slow down silicon nitride combined silicon carbide refractory brick, reach obvious prolongation and contain ZrB
2Material and TiB
2The purpose in novel silicon nitride combined silicon carbide refractory brick work-ing life of material.Simultaneously, avoided coming Mi to mend the defective in silicon nitride combined silicon carbide refractory brick work life-span, guaranteed to contain ZrB by the thickness that increases silicon nitride combined silicon carbide refractory brick
2Material and TiB
2The consistence and the stability of the novel silicon nitride combined silicon carbide refractory brick quality of material.
Description of drawings
Fig. 1 is the composite brick body synoptic diagram of the reinforced embodiment preparation of layering of the present invention.
Embodiment:
Be illustrated in figure 1 as the synoptic diagram of the reinforced composite brick body for preparing of layering of the embodiment of the invention.Mode by layering and batch charging when being pressed into adobe in brick pressing machine is easy to realize containing ZrB
2Material and TiB
2The novel silicon nitride combined silicon carbide material of material and do not contain ZrB
2Material and TiB
2The control adjustment of different thickness between the silicon nitride combined silicon carbide material of material can be made the ZrB that contains of different costs
2Material and TiB
2The composite structure brick body of the novel silicon nitride combined silicon carbide brick of material.
The present invention will be further described below in conjunction with embodiment:
Technical scheme of the present invention is: add ZrB at aluminum electrolytic bath side wall in silicon nitride combined silicon carbide refractory brick body
2Material and TiB
2Material, can improve the ability that the anti-sodium aluminum fluoride ionogen of silicon nitride combined silicon carbide refractory brick liquation corrodes and permeates greatly, slow down silicon nitride combined silicon carbide refractory brick effectively and suffer sodium aluminum fluoride ionogen liquation to corrode the speed of damage, reach and prolong aluminum electrolytic bath side wall with the novel silicon nitride combined silicon carbide refractory brick purpose in work-ing life.
Add and contain ZrB
2Material and TiB
2Material (ZrB
2Greater than 90%, Fe
2O
3Less than 0.3%; TiB
2Greater than 90%, Fe
2O
3Less than 0.3%) the embodiment of silicon nitride combined silicon carbide brick be: in the blending process of the silicon nitride combined silicon carbide brick of production technique ZrB
2Material and TiB
2Material is followed silicon-carbide particle, and (SiC is greater than 97.5%, Fe
2O
3Less than 0.5%, grain graininess is 5.0mm~0.5um, contains the carbide fine powder less than 0.08mm.The mass percent of total add-on of silicon carbide is 60~80%) and silica flour (the Si content requirement is greater than 96.5%, Fe
2O
3Content requirement is less than 0.5%.Grain graininess requires to be the silica fine powder less than 0.08mm, add-on is 10~25%) and add the normal temperature wedding agent (generally can adopt concentration is that about 30% industrial dextrin, concentration are that about 30% calcium lignosulfonate solution or concentration are about 10% polyvinyl alcohol solution, add-on be total batching quality 0.2~10%) add together to force to stir in the sand mill and mixed 20 minutes.Add ZrB
2Material and TiB
2The granularity of material is added ZrB between 1mm to 0.1um
2Material and TiB
2The quantity of material is 0.1%~20% of total batching quality, the ZrB of interpolation
2Material and TiB
2The mutual ratio of material can be regulated arbitrarily.
The material that mixes is pressed into adobe in brick pressing machine, brick pressing machine can be the large-scale vibrating pressure forming machine, also can be 200~1000 tons friction press, also can be high tonnage hydropress.The adobe of forming is dry under 30 ℃~200 ℃ temperature, and the moisture of dry back adobe should be controlled at less than 0.4%.The good adobe of drying is placed nitriding furnace and feeds high pure nitrogen (N
2Greater than 99.99%) continuous heat temperature raising, nitriding furnace can be with electrically heated, it also can be the Ma Fushi nitriding furnace of fuel oil or combustion gas, heat-up rate is controlled at 20~300 ℃/hour, when being warming up to 1370 ℃~1450 ℃ temperature ranges and under this temperature range, be incubated 3~50 hours and (decide soaking time with products thickness, products thickness is big more, and soaking time is long more.For example, the goods that 90mm is thick, soaking time generally will reach more than 20 hours).Can stop logical nitrogen when being cooled to 900~500 ℃.Be cooled to the ZrB that contains that can obtain the present invention relates to after the room temperature
2Material and TiB
2The novel silicon nitride combined silicon carbide refractory brick of material.
Contain ZrB
2Material and TiB
2The production process of material silicon nitride combined silicon carbide brick:
Raw material:
The sic raw material specification of quality is, SiC is greater than 97.5%, Fe
2O
3Less than 0.5%.
The proportioning of each silicon-carbide particle granularity is: 5.0mm~3mm accounts for 10%; 3~1mm accounts for 20%; 1~0.5mm, 8%; ≤ 0.5mm accounts for 8%, less than the carbide fine powder 14% of 0.08mm; Total add-on of silicon carbide is 60% (mass percent).
The silica flour raw materials quality requires, and Si is greater than 97.5%, Fe
2O
3Less than 0.5%.Grain graininess is the silica fine powder less than 0.08mm, and add-on is 20%.
Add ZrB
2Material and TiB
2The granularity of material is between 1mm~0.1um, the ZrB of interpolation
2Material and TiB
2The mutual ratio of material is 1: 1, adds ZrB
2Material and TiB
2The quantity of material is 20% of total batching quality.
Batching:
Earlier the silicon-carbide particle adding of each granularity is forced to stir in the sand mill and mixed back adding carbide fine powder, silica flour and ZrB 3 minutes
2Material and TiB
2Behind the material remix 5 minutes, add that to add normal temperature wedding agent concentration be about 30% industrial dextrin, add-on be 4% of total batching quality, after forcing to stir in the sand mill mixing 20 minutes together.
Moulding:
The material that mixes is suppressed into the thick goods of the wide 90mm of the long 450mm of 500mm in brick pressing machine, brick pressing machine can be the large-scale vibrating pressure forming machine, also can be 1000 tons friction press, also can be 3000 tons high tonnage hydropress.
Dry:
The ZrB of forming
2Material and TiB
2The silicon nitride combined silicon carbide firebrick billet of material is dry under 30 ℃~200 ℃ temperature, and the moisture of dry back adobe should be controlled at less than 0.4%.
Nitrogenize is burnt till:
The good adobe of drying is placed nitriding furnace and feeds high pure nitrogen (N
2Greater than 99.99%) continuous heat temperature raising, nitriding furnace can be electrically heated, it also can be the Ma Fushi nitriding furnace of fuel oil or combustion gas, heat-up rate is controlled at 20~300 ℃/hour, stops heating and naturally cooling after 20 hours when being warming up to 1370 ℃~1450 ℃ temperature ranges and in insulation under this temperature range.Can stop logical nitrogen when being cooled to 900~500 ℃.Be cooled to the ZrB that contains that can obtain the present invention relates to after the room temperature
2Material and TiB
2The novel silicon nitride combined silicon carbide refractory brick of material.
The physicochemical property of brick body is: silicon carbide, 57.66%; Silicon nitride, 26.22%; ZrB
2, 7.55%; TiB
2, 7.60%; Impurity, 0.97%.Apparent porosity, 19%; Volume density, 2.62g/cm
3Compressive strength, 178.3Mpa; Strength at normal temperature, 43.1Mpa; 1400 ℃ of folding strengths, 47.3Mpa.Crucible method cryolite resistant ability is in a ratio of special excellent with the silicon nitride combined silicon carbide brick.
Embodiment 2
Contain ZrB
2Material and TiB
2The production process of material silicon nitride combined silicon carbide brick:
Raw material:
The sic raw material specification of quality is, SiC is greater than 97.5%, Fe
2O
3Less than 0.5%.
The proportioning of each silicon-carbide particle granularity is: 5.0mm~3mm accounts for 15%; 3~1mm accounts for 24%; 1~0.5mm, 9%; ≤ 0.5mm accounts for 11%, less than the carbide fine powder 21% of 0.08mm; Total add-on of silicon carbide is 80% (mass percent).
The silica flour raw materials quality requires, and Si is greater than 97.5%, Fe
2O
3Less than 0.5%.Grain graininess is the silica fine powder less than 0.08mm, and add-on is 10%.
Add ZrB
2Material and TiB
2The granularity of material is between 1mm~0.1um, the ZrB of interpolation
2Material and TiB
2The mutual ratio of material is 1: 1, adds ZrB
2Material and TiB
2The quantity of material is 10% of total batching quality.
Batching:
Earlier the silicon-carbide particle adding of each granularity is forced to stir in the sand mill and mixed back adding carbide fine powder, silica flour and ZrB 3 minutes
2Material and TiB
2Behind the material remix 5 minutes, add that to add normal temperature wedding agent concentration be about 30% industrial dextrin, add-on be 5% of total batching quality, after forcing to stir in the sand mill mixing 20 minutes together.
Moulding:
The material that mixes is suppressed into the thick goods of the wide 90mm of the long 450mm of 500mm in brick pressing machine, brick pressing machine can be the large-scale vibrating pressure forming machine, also can be 1000 tons friction press, also can be 3000 tons high tonnage hydropress.
Dry:
The ZrB of forming
2Material and TiB
2The silicon nitride combined silicon carbide firebrick billet of material is dry under 30 ℃~200 ℃ temperature, and the moisture of dry back adobe should be controlled at less than 0.3%.
Nitrogenize is burnt till:
The good adobe of drying is placed nitriding furnace and feeds high pure nitrogen (N
2Greater than 99.99%) continuous heat temperature raising, nitriding furnace can be electrically heated, it also can be the Ma Fushi nitriding furnace of fuel oil or combustion gas, heat-up rate is controlled at 20~300 ℃/hour, stops heating and naturally cooling after 20 hours when being warming up to 1370 ℃~1450 ℃ temperature ranges and in insulation under this temperature range.Can stop logical nitrogen when being cooled to 900~500 ℃.Be cooled to the ZrB that contains that can obtain the present invention relates to after the room temperature
2Material and TiB
2The novel silicon nitride combined silicon carbide refractory brick of material.
The physicochemical property of brick body is: silicon carbide, 78.42%; Silicon nitride, 13.87%; ZrB
2, 3.45%; TiB
2, 3.38%; Impurity, 0.88%.Apparent porosity, 21%; Volume density, 2.60g/cm
3Compressive strength, 171.3Mpa; Strength at normal temperature, 41.1Mpa; 1400 ℃ of folding strengths, 46.3Mpa.Crucible method cryolite resistant ability is in a ratio of special excellent with the silicon nitride combined silicon carbide brick.
Embodiment 3
Contain ZrB
2Material and TiB
2The production process of material silicon nitride combined silicon carbide brick:
Raw material:
The sic raw material specification of quality is, SiC is greater than 97.5%, Fe
2O
3Less than 0.5%.
The proportioning of each silicon-carbide particle granularity is: 5.0mm~3mm accounts for 15%; 3~1mm accounts for 24%; 1~0.5mm, 9%; ≤ 0.5mm accounts for 11%, less than the carbide fine powder 21% of 0.08mm; Total add-on of silicon carbide is 80% (mass percent).
The silica flour raw materials quality requires, and Si is greater than 97.5%, Fe
2O
3Less than 0.5%.Grain graininess is the silica fine powder less than 0.08mm, and add-on is 18%.
Add ZrB
2Material and TiB
2The granularity of material is between 1mm~0.1um, the ZrB of interpolation
2Material and TiB
2The mutual ratio of material is 1: 1, adds ZrB
2Material and TiB
2The quantity of material is 2% of total batching quality.
Batching:
Earlier the silicon-carbide particle adding of each granularity is forced to stir in the sand mill and mixed back adding carbide fine powder, silica flour and ZrB 3 minutes
2Material and TiB
2Behind the material remix 5 minutes, add that to add normal temperature wedding agent concentration be about 30% industrial dextrin, add-on be 5% of total batching quality, after forcing to stir in the sand mill mixing 20 minutes together.
Moulding:
The material that mixes is suppressed into the thick goods of the wide 90mm of the long 450mm of 500mm in brick pressing machine, brick pressing machine can be the large-scale vibrating pressure forming machine, also can be 1000 tons friction press, also can be 3000 tons high tonnage hydropress.
Dry:
The ZrB of forming
2Material and TiB
2The silicon nitride combined silicon carbide firebrick billet of material is dry under 30 ℃~200 ℃ temperature, and the moisture of dry back adobe should be controlled at less than 0.3%.
Nitrogenize is burnt till:
The good adobe of drying is placed nitriding furnace and feeds high pure nitrogen (N
2Greater than 99.99%) continuous heat temperature raising, nitriding furnace can be electrically heated, it also can be the Ma Fushi nitriding furnace of fuel oil or combustion gas, heat-up rate is controlled at 20~300 ℃/hour, stops heating and naturally cooling after 20 hours when being warming up to 1370 ℃~1450 ℃ temperature ranges and in insulation under this temperature range.Can stop logical nitrogen when being cooled to 900~500 ℃.Be cooled to the ZrB that contains that can obtain the present invention relates to after the room temperature
2Material and TiB
2The novel silicon nitride combined silicon carbide refractory brick of material.
The physicochemical property of brick body is: silicon carbide, 76.22%; Silicon nitride, 21.46%; ZrB
2, 0.75%; TiB
2, 0.78%; Impurity, 0.79%.Apparent porosity, 21%; Volume density, 2.60g/cm
3Compressive strength, 171.3Mpa; Strength at normal temperature, 41.1Mpa; 1400 ℃ of folding strengths, 46.3Mpa.Crucible method cryolite resistant ability is in a ratio of slightly excellent with the silicon nitride combined silicon carbide brick.
Claims (7)
1, aluminum electrolytic bath side wall silicon nitride combined silicon carbide refractory brick, it is characterized in that: described refractory brick is to contain ZrB
2Material and TiB
2The Si of material
3N
4In conjunction with the SiC brick; Add and contain ZrB
2Material and TiB
2The embodiment of the silicon nitride combined silicon carbide brick of material is ZrB in blending process
2Material and TiB
2Material follows silicon-carbide particle and fine powder, silica fine powder, add sinter additives and add the normal temperature wedding agent adds together to force to stir in the sand mill and mixes; The mass percent of the add-on of described silicon carbide is 55~89%, and described silica fine powder add-on is 10~25%, described interpolation ZrB
2Material and TiB
2The quantity of material is 0.1%~20% of total batching quality, and the described sinter additives that adds is 0.2~10% of total batching quality, and the described add-on that adds the normal temperature wedding agent is 0.2~10% of total batching quality.
2, aluminum electrolytic bath side wall according to claim 1 silicon nitride combined silicon carbide refractory brick, it is characterized in that: add sinter additives in the described refractory brick and be one or more of various rare earth oxides and its esters, total add-on of sinter additives is generally in 6%.
3, aluminum electrolytic bath side wall according to claim 1 silicon nitride combined silicon carbide refractory brick is characterized in that: the described ZrB of containing
2The specification of quality of material is: ZrB
2Content is greater than 90%, Fe
2O
3Content is less than 0.3%, and granularity is between 1.5mm to 0.1um; Described TiB
2The specification of quality of material is: TiB
2Content is greater than 90%, Fe
2O
3Content is less than 0.3%, and granularity is between 1.5mm to 0.1um.
4, aluminum electrolytic bath side wall according to claim 1 silicon nitride combined silicon carbide refractory brick, it is characterized in that: the specification of quality of silicon carbide is in the described refractory brick: SiC content is greater than 96%, Fe
2O
3Content is less than 1.5%, and granular size is 5.0mm~0.1mm, and carbide fine powder is less than 0.08mm.
5, aluminum electrolytic bath side wall according to claim 1 silicon nitride combined silicon carbide refractory brick, it is characterized in that: the specification of quality of silica flour is in the described refractory brick: Si content is greater than 96%, Fe
2O
3Less than 1.5%, the silica fine powder granularity is less than 0.08mm's.
6, aluminum electrolytic bath side wall according to claim 1 silicon nitride combined silicon carbide refractory brick is characterized in that: add the normal temperature wedding agent in the described refractory brick and adopt industrial dextrin solution or calcium lignosulfonate solution or polyvinyl alcohol solution.
7, the preparation aluminum electrolytic bath side wall as claimed in claim 1 method of silicon nitride combined silicon carbide refractory brick, it is characterized in that: described method is followed successively by:
A) with ZrB
2Material and TiB
2Material, silicon-carbide particle and fine powder, silica fine powder, sinter additives and add the normal temperature wedding agent and add in the mixing machinery together and mix, the material after mixing is pressed into adobe in brick pressing machine;
B), and make dry back moisture less than 0.4% with the brick bat drying of above-mentioned forming;
C) above-mentioned drying is good adobe places the nitriding furnace heating to burn till, and feeds high pure nitrogen in the process of heat temperature raising simultaneously, and nitrogen gas purity should be greater than 99.90%.The process of heat temperature raising is the process that heats up continuously, and heat-up rate is controlled at 10 ℃~300 ℃/hour, during to 1370 ℃~1450 ℃ temperature ranges and be incubated 3~50 hours under this temperature range;
Logical nitrogen can be stopped when d) being cooled to 900~500 ℃, ZrB can be obtained containing after being cooled to room temperature
2Material and TiB
2The silicon nitride combined silicon carbide refractory brick of material.
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CNA2004100307868A CN1562883A (en) | 2004-04-09 | 2004-04-09 | Firebrick made from silicom nitride combined with silicon carbide in use for sidewall of electrobath for making aluminium |
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Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CNA2004100307868A CN1562883A (en) | 2004-04-09 | 2004-04-09 | Firebrick made from silicom nitride combined with silicon carbide in use for sidewall of electrobath for making aluminium |
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CN100381399C (en) * | 2006-09-21 | 2008-04-16 | 武汉钢铁(集团)公司 | High thermal shock abrasive brick for dry quenched coke oven chute pillar and manufacture method |
CN100412234C (en) * | 2005-09-20 | 2008-08-20 | 东北大学设计研究院(有限公司) | Large-scale aluminium electrolysis pre-baking tank |
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Publication number | Priority date | Publication date | Assignee | Title |
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CN100412234C (en) * | 2005-09-20 | 2008-08-20 | 东北大学设计研究院(有限公司) | Large-scale aluminium electrolysis pre-baking tank |
CN100417625C (en) * | 2005-09-21 | 2008-09-10 | 日本碍子株式会社 | Kiln furniture for use in a non-oxidizing atmosphere |
CN100381399C (en) * | 2006-09-21 | 2008-04-16 | 武汉钢铁(集团)公司 | High thermal shock abrasive brick for dry quenched coke oven chute pillar and manufacture method |
CN102228983A (en) * | 2011-06-17 | 2011-11-02 | 任灵成 | Electrolytic aluminum discharging pipe device with cleaning-free two-man ladle |
CN103998654A (en) * | 2011-09-28 | 2014-08-20 | 钴碳化钨硬质合金公司 | Titanium diboride-silicon carbide composites useful in electrolytic aluminum production cells and methods for producing the same |
CN102765953A (en) * | 2012-08-07 | 2012-11-07 | 营口鲅鱼圈耐火材料有限公司 | Magnesia carbon brick containing composite antioxidant and preparation thereof |
CN102765953B (en) * | 2012-08-07 | 2013-12-11 | 营口鲅鱼圈耐火材料有限公司 | Magnesia carbon brick containing composite antioxidant and preparation thereof |
CN104529484A (en) * | 2014-12-08 | 2015-04-22 | 东北大学 | Preparation method for sintering-free SiC refractory material for electrolytic aluminium tanks |
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