CN103922773A - Boron nitride ceramic side seal plate for continuous thin-strip casting and manufacturing method of side seal plate - Google Patents
Boron nitride ceramic side seal plate for continuous thin-strip casting and manufacturing method of side seal plate Download PDFInfo
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- CN103922773A CN103922773A CN201410161765.3A CN201410161765A CN103922773A CN 103922773 A CN103922773 A CN 103922773A CN 201410161765 A CN201410161765 A CN 201410161765A CN 103922773 A CN103922773 A CN 103922773A
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Abstract
The invention discloses a boron nitride ceramic side seal plate for continuous thin-strip casting. The boron nitride ceramic side seal plate is characterized by comprising the following chemical components by mass percent: 20%-75% of hexagonal boron nitride, 10%-55% of aluminum nitride powder, 5%-40% of magnesium aluminate spinel, 5%-20% of mullite and 0.5%-15% of an additive, wherein the additive is selected from one or combination of several of MgAlON, AlON, CaAl4O7, CaZrO3 and CaTiO3. The boron nitride ceramic side seal plate manufactured by adopting novel ceramic formula and preparation method is relatively high in density, fire-resistant degree and rupture strength, so that the side seal plate is fully ensured to be not softened in a use process. Meanwhile, the side seal plate is low in heat conduction rate and good in thermal shock resistance, so that the side seal plate can well resist the thermal shock of molten steel in the use process and the service life of the side seal plate is prolonged.
Description
Technical field
The present invention relates to continuous casting of iron and steel technical field, refer to particularly boron nitride pottery side seal board and preparation method thereof for a kind of thin strap continuous casting.
Background technology
Thin strap continuous casting is the revolutionary short processes flow process of in iron and steel band field of industrial production, it has fundamentally changed the production process of the slim steel of Iron And Steel Industry, a series of conventional operations such as continuous casting (ingot casting), roughing, hot continuous rolling and relevant heating, crop have been cancelled, started molten steel is directly poured into a mould through tundish, and Direct Rolling becomes latest model technology and the technique of efficient, energy-saving and environmental protection of the slim sheet material of number mm thick.Side seal board technology is one of most critical technology in strip continuous casting technology, is the key factor that affects casting strip quality and technology stability in strip casting process.At present, mainly contain electromagnetic side sealing, gas side seal and three kinds of side seal modes of solid side seal, wherein gas side seal is just proposed by people as a kind of new side dam technology, mostly in the fundamental research stage.Electromagnetic side sealing technology exists equipment complicated, and magnetic field is wayward, and state of the art reaches far away the requirement of suitability for industrialized production.Solid side seal be current technology the most ripe, be also a kind of side sealing method that approaches Practical Condition most.
At present, the solid side seal board overwhelming majority of research and development all can not meet industrial requirement both at home and abroad, as: the < < Ceramic plates for side dams of twin-drum continuous strip casters > > (people such as Nose, what US Patent No. 7208433) use is a kind of rare-earth garnet that utilizes, Sialon and BN (boron nitride) matrix material is prepared ceramic side seal board, in patent, report that this kind of side seal board has lower thermal conductivity (thermal conductivity≤10W/mK), and there is good thermal shock resistance.< < Pressure-sintered polycpystalline mixed materials with a base of hexagonal boron nitride, the oxides and carbides > > (people such as Sindlhauser, US Patent No. 4885264) boron nitride-oxide-base matrix material and boron nitride-non-oxidized substance matrix material are prepared to ceramic side seal board and are studied, in experiment at BN-ZrO
2in matrix, add respectively SiC, ZrC, under vacuum condition, in 1500～1800 ℃ of hot pressed sinterings, be prepared into ceramic composite.The performance test results of this bi-material is as follows: reach respectively 94% and 95% of theoretical density, thermal conductivity is respectively 18W (mK)
-1and 14W (mK)
-1(1000 ℃), test result also finds simultaneously, two kinds of side seal board materials of this that make are very fine and close, and tool has good wearability, heat-shock resistance and resistance to fouling.The < < Composite material > > (people such as Guillo, US Patent No. 6667263) take hexagonal boron nitride-oxide compound (oxide compound of Al, Mg, Si, Ti) is matrix, add nitride (nitride of Al, Si, Zr, Ti), under vacuum state, hot pressed sintering has been prepared ceramic side seal board matrix material.Experimental result shows, BN-Al
2o
3-Si
3n
4performance is best, Al
2o
3and Si
3n
4formed sosoloid, heat-shock resistance, wear resistance, solidity to corrosion and non wettability that material has been had.< < Ceramic plate for side weir of twin-drum type continu-ous casting apparatus > > (people such as Takeuchi, US Patent No. 6843304) has prepared BN-AlN-Si
3n
4the ceramic side seal board matrix material of-Al (or Equivalent of Al), its thermal conductivity is less than 8W (mK)
-1, thermal shock resistance and anti-molten steel erosion performance are good.(keep one's word in Xu Hongjie and field for < < side sealing plate for thin-belt continuous casting and manufacture method > >, Chinese patent CN102161082A) utilize boron nitride, zirconium boride 99.5004323A8ure, graphite and carbon fiber to prepare the ceramic side seal board of thin strap continuous casting, in this patent, report that its thermal conductivity is 22W (mK)
-1, antioxidant property and abrasion resistance properties are better, but this kind of side seal board is short work-ing life.< < twin-roll thin-strip casting side sealing plate and preparation method thereof the > > (people from field such as keep one's word, Chinese patent CN101648260A) a kind of composite lateral sealing plate that utilized a kind of panel of boron nitride material and substrate manufacture that a kind of aluminium silicon is heat preserving and insulating material, the heat-insulating property of reporting this kind of composite lateral sealing plate in this patent is good, but the thermal shock resistance of this side seal board is not good, cause side seal board not long work-ing life.< < ceramic composite for thin-strip casting side sealing plate and preparation method thereof the > > (people such as Wang Yujin, Chinese patent CN102173792A) in this patent, system has been reported and is utilized boron nitride, carbide, nitride and oxide compound as the making method of side seal board, the prepared side seal board density of this patent is 94%～99%, room temperature bending strength is 260～420MPa, and fracture toughness property is 3～8MPam
1/2although, aspect intensity, having met the service requirements of side seal board, in its use procedure, because the thermal shocking of opposing molten steel is poor, work-ing life is very short.In general, side seal board material has all been carried out to a large amount of research both at home and abroad, external side seal board small part has been carried out commercialization production, domestic side seal board research is still in the middle of laboratory study and simulated experiment, also fail to produce the ceramic side seal board that meets service requirements, this gordian technique is still restricting the process of industrialization of thin strap continuous casting.The problems such as although external prepared side seal board is better than domestic side seal board, and more or less existence is as not good in anti-molten steel chemical corrosion, and heat-shock resistance is poor and wear no resistance.Over-all properties is side seal board preferably, in its long-time use procedure, still can have the problems referred to above.This be because, generally, when guaranteeing the heat-shock resistance that side seal board has had, can not guarantee that side seal board has low thermal conductivity, this just makes side seal board surface be easy to produce cold, thereby causes side seal board to be worn, shortening the life-span.Another aspect, when the side seal board of sintering large volume high-compactness, is difficult to make the phase composite of side seal board thing and microtexture homogeneous, and this just makes side seal board inside occur that thermal expansion do not mate, thereby cause side seal board that thermal shock in use occurs, destroys.If side seal board selects material poor with molten steel non wettability, side seal board in use more easily and molten steel generation erosion damage.Therefore, research and development high-performance ceramic side seal board material is significant to the suitability for industrialized production of thin strap continuous casting.
Summary of the invention
Object of the present invention will provide boron nitride pottery side seal board and preparation method thereof for a kind of thin strap continuous casting exactly, the present invention consists of the new formula of development of new side seal board, and adjust its preparation method make side seal board have simultaneously high temperature resistant, intensity is high, anti-thermal shock and the low performance characteristics of thermal conductivity.
For realizing this object, boron nitride pottery side seal board for the designed thin strap continuous casting of the present invention, it is characterized in that, the Chemical Composition of this boron nitride pottery side seal board is by mass percentage: hexagonal boron nitride 20～75%, aluminium nitride (AlN) powder 10～55%, magnesium-aluminium spinel 5～40%, mullite 5～20% and additive 0.5～15%, wherein, additive is MgAlON (magnesium A Long), AlON (A Long), CaAl
4o
7, CaZrO
3and CaTiO
3in one or more combination.Adopt this proportioning, can make full use of the good characteristic that hexagonal boron nitride material itself has, high thermal resistance, oilness, low thermal expansivity and fabulous chemical stability.Hexagonal boron nitride has the lamellar structure that is similar to graphite, only under the nitrogen pressure of 300kPa, in 3000 ℃, melts above, and at high temperature without ruckbildung, thereby hot pressing hexagonal boron nitride has higher use temperature and Burning corrosion resistance energy.Therefore employing hexagonal boron nitride is main raw material, the raw materials such as auxiliary low-expansion aluminum nitride powder are prepared compound multiphase ceramic, can obtain high temperature resistant, anti-thermal shock and erosion-resistant ceramic side seal board.
Further, to account for the weight percent of described boron nitride pottery side seal board be 20～70% to described hexagonal boron nitride.
Further, described additive is MgAlON, AlON and CaAl
4o
7, the weight percent that described MgAlON accounts for described boron nitride pottery side seal board is that the weight percent that 5%, AlON accounts for described boron nitride pottery side seal board is 3%, CaAl
4o
7the weight percent that accounts for described boron nitride pottery side seal board is 2%.
Optionally, described additive is MgAlON, CaZrO
3and CaTiO
3, the weight percent that described MgAlON accounts for described boron nitride pottery side seal board is 2%, described CaZrO
3the weight percent that accounts for described boron nitride pottery side seal board is 2%, described CaTiO
3the weight percent that accounts for described boron nitride pottery side seal board is 1%.
Optionally, described additive is AlON, CaAl
4o
7, CaZrO
3and CaTiO
3, the weight percent that described AlON accounts for described boron nitride pottery side seal board is 5%, CaAl
4o
7the weight percent that accounts for described boron nitride pottery side seal board is 2%, CaZrO
3the weight percent that accounts for described boron nitride pottery side seal board is 2%, CaTiO
3the weight percent that accounts for described boron nitride pottery side seal board is 1%.
Optionally, described additive is MgAlON, AlON, CaZrO
3and CaTiO
3, the weight percent that the weight percent that described MgAlON accounts for described boron nitride pottery side seal board is 1%, AlON accounts for described boron nitride pottery side seal board is 1%, CaZrO
3the weight percent that accounts for described boron nitride pottery side seal board is 2%, CaTiO
3the weight percent that accounts for described boron nitride pottery side seal board is 1%.
A preparation method for boron nitride pottery side seal board for thin strap continuous casting, it comprises the steps:
Step 1: by hexagonal boron nitride powder, aluminum nitride powder, magnesium aluminium spinel powder, mullite powder and additive adopt wet ball grinding method to carry out ball-milling processing at least 12 hours with ball mill respectively, form respectively hexagonal boron nitride slurry, aluminium nitride slurry, magnesium-aluminium spinel slurry, mullite slurry and additive slurry, ball milling solvent in ball-milling processing process is that dehydrated alcohol or acetone or purity are more than 95% industrial spirit, in this ball-milling processing process, control hexagonal boron nitride slurry, aluminium nitride slurry, magnesium-aluminium spinel slurry, in mullite slurry and additive slurry, solid particulate granularity is 0.5～8 μ m, and then by hexagonal boron nitride slurry, aluminium nitride slurry, magnesium-aluminium spinel slurry, mullite slurry and additive slurry are dried respectively and are formed hexagonal boron nitride powder, aluminium nitride powder, magnesium-aluminium spinel powder, porzite powder and additive powder, described additive is MgAlON, AlON, CaAl
4o
7, CaZrO
3and CaTiO
3in one or more combination, adopt the reason of above processing parameter to be that sufficient Ball-milling Time can guarantee the granularity of particle, and thin grain graininess can increase the specific surface area of raw material, thereby improve the activity of raw material,
Step 2: be by mass percentage: hexagonal boron nitride 20～75%, aluminum nitride powder 10～55%, magnesium-aluminium spinel 5～40%, powder in mullite 5～20% and additive 0.5～15% selecting step 1 after drying and processing, and by ball mill by above-mentioned hexagonal boron nitride powder, aluminium nitride powder, magnesium-aluminium spinel powder, porzite powder and additive powder carry out wet ball grinding combination treatment, the ball milling solvent adopting in wet ball grinding combination treatment is that dehydrated alcohol or acetone or purity are more than 95% industrial spirit, wet ball grinding combination treatment is until hexagonal boron nitride powder, aluminium nitride powder, magnesium-aluminium spinel powder, porzite powder and additive powder mix, without layering, occur, it is form mixed slurry, by adopting wet ball grinding to mix, can be so that each raw material abundant dispersing and mixing be each other convenient to form uniform thing phase in sintering process,
Step 3: mixed slurry is carried out to drying treatment, form mixed powder, recycling nodulizer carries out granulation processing to the mixed powder forming after dry, in granulation treating processes, control mixed powder particle size range and account for 10～20% below 0.5mm, particle size range accounts for 30～50% 0.5～1mm's, particle size range accounts for 10～35% 1.0～2.0mm's, and what particle size range was greater than 2mm accounts for 5～20%; By nodulizer, can obtain uniform spheroidal particle, and be convenient to control the particle diameter of particle; Adopt the granulated of different-grain diameter to become grating, be convenient to compression moulding;
Step 4: all mixed powders that above-mentioned granulation is processed to resulting different-grain diameter are put into mixer and evenly mixed, and obtain coordinating powder;
Step 5: above-mentioned cooperation powder is put into graphite jig, adopt discharge plasma sintering process sintering to prepare side seal board base substrate, final sintering temperature in discharge plasma sintering process is 1400～2000 ℃, and in discharge plasma sintering process, corresponding atmosphere pressures is 5～50MPa during final sintering; Control sintering temperature and pressure and can obtain the pottery that density is high.
Step 6: adopt lathe to carry out processing treatment the side seal board base substrate after above-mentioned sintering, obtain boron nitride pottery side seal board for thin strap continuous casting.
Further, in described step 1, the purity of hexagonal boron nitride powder, aluminum nitride powder, magnesium aluminium spinel powder, mullite powder and additive all will reach analytical pure rank.
Further, the Ball-milling Time of the wet ball grinding combination treatment of described step 2 is 12～48 hours.
Further, the drying treatment of described step 3 is vacuum freeze-drying method or micro-wave drying method.
Beneficial effect of the present invention: adopt new ceramics formula and preparation method, the thin strap continuous casting of manufacture has higher density, refractoriness and folding strength with boron nitride pottery side seal board, fully guarantees that side seal board in use can not soften.Meanwhile, side seal board of the present invention has low thermal conductivity and good thermal shock resistance, and assurance side seal board in use can be resisted molten steel thermal shocking preferably, has extended the work-ing life of side seal board.The present invention is with respect to traditional side seal board, owing to having adopted new ceramic formula to form, in preparation technology, raw material and various processing parameter have been accomplished to Precise control, thus make the inner thing phase constitution of prepared side seal board evenly, side seal board thermal expansivity and thermal conductivity little.In macroscopic view, show as the thermal shock resistance of side seal board, anti-molten steel erosion performance and wear resisting property more excellent with respect to traditional side seal board.Thereby, work-ing life and the stability in use of side seal board can be effectively improved, thereby thin strap continuous casting production cost can be reduced, there is obvious economic benefit.
Thin strap continuous casting of the present invention is 94～98% by the density of boron nitride pottery side seal board, refractoriness is more than 1700 ℃, room temperature folding strength is 200～400MPa, thermal conductivity is 5～30W/ (mK) (room temperature), simultaneously, there is RT (room temperature room temperature) between 1100 ℃, the thermal shock resistance that water-cooled is not broken for 40 times.Above-mentioned parameter compare with existing side seal board explanation the present invention have high temperature resistant, intensity is high, good thermal shock and the low feature of thermal conductivity.
Accompanying drawing explanation
Fig. 1 is the microstructure picture after the thin strap continuous casting of embodiment 3 preparations amplifies 5000 times with boron nitride pottery side seal board sample.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in further detail:
Embodiment 1:
Step 1: by hexagonal boron nitride powder, aluminum nitride powder, magnesium aluminium spinel powder, mullite powder, MgAlON powder, AlON powder and CaAl
4o
7powder adopts wet ball grinding method to carry out ball-milling processing 24 hours with ball mill respectively, ball milling solvent in ball-milling processing process is dehydrated alcohol, above-mentioned raw materials purity need reach analytical pure rank, in above-mentioned ball-milling processing process, control hexagonal boron nitride slurry, aluminium nitride slurry, magnesium-aluminium spinel slurry, mullite slurry, MgAlON slurry, AlON slurry, CaAl
4o
7in slurry, solid particulate granularity is 2 μ m, and then above-mentioned slurry is dried, and forms corresponding powder;
Step 2: be by mass percentage: hexagonal boron nitride 70%, aluminum nitride powder 10%, magnesium-aluminium spinel 5%, mullite 5%, MgAlON5%, AlON3%, CaAl
4o
7powder in 2% selecting step 1 after drying and processing, and by ball mill, above-mentioned powder is carried out to wet ball grinding combination treatment, the time of wet ball grinding combination treatment is 12 hours, until compound evenly mixes, without layering, occurs, forms mixed slurry;
Step 3: utilize vacuum freeze-drying method to carry out drying treatment to mixed slurry, form mixed powder, recycling nodulizer carries out granulation processing to the mixed powder forming after dry, in granulation treating processes, control mixed powder particle size range and account for 20% below 0.5mm, particle size range accounts for 50% 0.5～1mm's, particle size range accounts for 20% 1.0～2.0mm's, and what particle size range was greater than 2mm accounts for 10%;
Step 4: all mixed powders that above-mentioned granulation is processed to resulting different-grain diameter are put into mixer and evenly mixed, and obtain coordinating powder;
Step 5: above-mentioned cooperation powder is put into graphite jig, adopt discharge plasma sintering process sintering to prepare side seal board base substrate, final sintering temperature in discharge plasma sintering process is 2000 ℃, and in discharge plasma sintering process, corresponding atmosphere pressures is 50MPa during final sintering;
Step 6: adopt lathe to carry out processing treatment the side seal board base substrate after above-mentioned sintering, obtain boron nitride pottery side seal board for thin strap continuous casting.
After tested, the thin strap continuous casting that the present embodiment 1 obtains is as follows by the performance of boron nitride pottery side seal board:
Pottery side seal board density is 98%, and refractoriness is 1800 ℃, and room temperature folding strength is 350MPa, thermal conductivity is 20W/ (mK) (room temperature), meanwhile, there is RT (room temperature room temperature) between 1100 ℃, the thermal shock resistance that water-cooled is not broken for 40 times.
As can be seen here embodiment 1 have high temperature resistant, intensity is high, good thermal shock and the low feature of thermal conductivity.
Embodiment 2:
Step 1: by hexagonal boron nitride powder, aluminum nitride powder, magnesium aluminium spinel powder, mullite powder, MgAlON powder, CaZrO
3powder and CaTiO
3powder adopts wet ball grinding method to carry out ball-milling processing 36 hours with ball mill respectively, ball milling solvent in ball-milling processing process is acetone, above-mentioned raw materials purity need reach analytical pure rank, controls hexagonal boron nitride slurry, aluminium nitride slurry, magnesium-aluminium spinel slurry, mullite slurry, MgAlON slurry, CaZrO in above-mentioned ball-milling processing process
3slurry and CaTiO
3in slurry, solid particulate granularity is 4 μ m, and then above-mentioned slurry is dried, and forms corresponding powder;
Step 2: be by mass percentage: hexagonal boron nitride 60%, aluminum nitride powder 15%, magnesium-aluminium spinel 10%, mullite 10%, MgAlON2%, CaZrO
32% and CaTiO
3powder in 1% selecting step 1 after drying and processing, and by ball mill, above-mentioned powder is carried out to wet ball grinding combination treatment, the time of wet ball grinding combination treatment is 24 hours, until compound evenly mixes, without layering, occurs, forms mixed slurry;
Step 3: utilize micro-wave drying method to carry out drying treatment to mixed slurry, form mixed powder, recycling nodulizer carries out granulation processing to the mixed powder forming after dry, in granulation treating processes, control mixed powder particle size range and account for 20% below 0.5mm, particle size range accounts for 40% 0.5～1mm's, particle size range accounts for 30% 1.0～2.0mm's, and what particle size range was greater than 2mm accounts for 10%;
Step 4: all mixed powders that above-mentioned granulation is processed to resulting different-grain diameter are put into mixer and evenly mixed, and obtain coordinating powder;
Step 5: above-mentioned cooperation powder is put into graphite jig, adopt discharge plasma sintering process sintering to prepare side seal board base substrate, final sintering temperature in discharge plasma sintering process is 1900 ℃, and in discharge plasma sintering process, corresponding atmosphere pressures is 30MPa during final sintering;
Step 6: adopt lathe to carry out processing treatment the side seal board base substrate after above-mentioned sintering, obtain boron nitride pottery side seal board for thin strap continuous casting.
After tested, the thin strap continuous casting that the present embodiment 2 obtains is as follows by the performance of boron nitride pottery side seal board:
Pottery side seal board density is 97%, and refractoriness is 1750 ℃, and room temperature folding strength is 264MPa, thermal conductivity is 5W/ (mK) (room temperature), meanwhile, there is RT (room temperature room temperature) between 1100 ℃, the thermal shock resistance that water-cooled is not broken for 40 times.
As can be seen here embodiment 2 have high temperature resistant, intensity is high, good thermal shock and the low feature of thermal conductivity.
Embodiment 3:
Step 1: by hexagonal boron nitride powder, aluminum nitride powder, magnesium aluminium spinel powder, mullite powder, AlON powder, CaAl
4o
7powder, CaZrO
3powder and CaTiO
3powder adopts wet ball grinding method to carry out ball-milling processing 36 hours with ball mill respectively, ball milling solvent in ball-milling processing process is that purity is more than 95% industrial spirit, above-mentioned raw materials purity need reach analytical pure rank, controls hexagonal boron nitride slurry, aluminium nitride slurry, magnesium-aluminium spinel slurry, mullite slurry, AlON slurry, CaAl in above-mentioned ball-milling processing process
4o
7slurry, CaZrO
3slurry and CaTiO
3in slurry, solid particulate granularity is 6 μ m, and then above-mentioned slurry is dried, and forms corresponding powder;
Step 2: be by mass percentage: hexagonal boron nitride 30%, aluminium nitride 30%, magnesium-aluminium spinel 20%, mullite 10%, AlON5%, CaAl
4o
72%, CaZrO
32% and CaTiO
31%, the powder in selecting step 1 after drying and processing, and by ball mill, above-mentioned powder is carried out to wet ball grinding combination treatment, the time of wet ball grinding combination treatment is 36 hours, until compound evenly mixes, without layering, occurs, forms mixed slurry;
Step 3: utilize vacuum freeze-drying method to carry out drying treatment to mixed slurry, form mixed powder, recycling nodulizer carries out granulation processing to the mixed powder forming after dry, in granulation treating processes, control mixed powder particle size range and below 0.5mm, account for 10%, particle size range accounts for 50% 0.5～1mm's, particle size range accounts for 30% 1.0～2.0mm's, and what particle size range was greater than 2mm accounts for 10%;
Step 4: all mixed powders that above-mentioned granulation is processed to resulting different-grain diameter are put into mixer and evenly mixed, and obtain coordinating powder;
Step 5: above-mentioned cooperation powder is put into graphite jig, adopt discharge plasma sintering process sintering to prepare side seal board base substrate, final sintering temperature in discharge plasma sintering process is 1650 ℃, and in discharge plasma sintering process, corresponding atmosphere pressures is 50MPa during final sintering;
Step 6: adopt lathe to carry out processing treatment the side seal board base substrate after above-mentioned sintering, obtain boron nitride pottery side seal board for thin strap continuous casting.
After tested, the thin strap continuous casting that the present embodiment 3 obtains is as follows by the performance of boron nitride pottery side seal board:
Pottery side seal board density is 94%, and refractoriness is 1750 ℃, and room temperature folding strength is 246MPa, thermal conductivity is 15W/ (mK) (room temperature), meanwhile, there is RT (room temperature room temperature) between 1100 ℃, the thermal shock resistance that water-cooled is not broken for 40 times.
As can be seen here embodiment 3 have high temperature resistant, intensity is high, good thermal shock and the low feature of thermal conductivity.
Embodiment 4:
Step 1: by hexagonal boron nitride powder, aluminum nitride powder, magnesium aluminium spinel powder, mullite powder, MgAlON powder, AlON powder, CaZrO
3powder and CaTiO
3powder adopts wet ball grinding method to carry out ball-milling processing 36 hours with ball mill respectively, ball milling solvent in ball-milling processing process is that purity is more than 95% industrial spirit, above-mentioned raw materials purity need reach analytical pure rank, in above-mentioned ball-milling processing process, control hexagonal boron nitride slurry, aluminium nitride slurry, magnesium-aluminium spinel slurry, mullite slurry, MgAlON slurry, AlON slurry, CaZrO
3slurry and CaTiO
3in slurry, solid particulate granularity is 8 μ m, and then above-mentioned slurry is dried, and forms corresponding powder;
Step 2: be by mass percentage: hexagonal boron nitride 20%, aluminium nitride 30%, magnesium-aluminium spinel 40%, mullite 5%, MgAlON1%, AlON1%, CaZrO
32% and CaTiO
31%, the powder in selecting step 1 after drying and processing, and by ball mill, above-mentioned powder is carried out to wet ball grinding combination treatment, the time of wet ball grinding combination treatment is 48 hours, until compound evenly mixes, without layering, occurs, forms mixed slurry;
Step 3: utilize micro-wave drying method to carry out drying treatment to mixed slurry, form mixed powder, recycling nodulizer carries out granulation processing to the mixed powder forming after dry, in granulation treating processes, control mixed powder particle size range and below 0.5mm, account for 15%, particle size range accounts for 45% 0.5～1mm's, particle size range accounts for 20% 1.0～2.0mm's, and what particle size range was greater than 2mm accounts for 20%;
Step 4: all mixed powders that above-mentioned granulation is processed to resulting different-grain diameter are put into mixer and evenly mixed, and obtain coordinating powder;
Step 5: above-mentioned cooperation powder is put into graphite jig, adopt discharge plasma sintering process sintering to prepare side seal board base substrate, final sintering temperature in discharge plasma sintering process is 1850 ℃, and in discharge plasma sintering process, corresponding atmosphere pressures is 50MPa during final sintering;
Step 6: adopt lathe to carry out processing treatment the side seal board base substrate after above-mentioned sintering, obtain boron nitride pottery side seal board for thin strap continuous casting.
After tested, the thin strap continuous casting that the present embodiment 4 obtains is as follows by the performance of boron nitride pottery side seal board:
Pottery side seal board density is 96%, and refractoriness is 1800 ℃, and room temperature folding strength is 325MPa, thermal conductivity is 30W/ (mK) (room temperature), meanwhile, there is RT (room temperature room temperature) between 1100 ℃, the thermal shock resistance that water-cooled is not broken for 40 times.
As can be seen here embodiment 4 have high temperature resistant, intensity is high, good thermal shock and the low feature of thermal conductivity.
From Fig. 1, can find, prepared side seal board interior tissue even compact, crystal grain is tiny, and most crystal grain is all below 5 μ m, and this heterogeneous microstructure contributes to the raising of side seal board intensity, heat conductivility and thermal shock resistance.
The content that this specification sheets is not described in detail belongs to the known prior art of professional and technical personnel in the field.
Claims (10)
1. boron nitride pottery side seal board for a thin strap continuous casting, it is characterized in that, the Chemical Composition of this boron nitride pottery side seal board is by mass percentage: hexagonal boron nitride 20～75%, aluminum nitride powder 10～55%, magnesium-aluminium spinel 5～40%, mullite 5～20% and additive 0.5～15%, wherein, additive is MgAlON, AlON, CaAl
4o
7, CaZrO
3and CaTiO
3in one or more combination.
2. boron nitride pottery side seal board for thin strap continuous casting according to claim 1, is characterized in that: the weight percent that described hexagonal boron nitride accounts for described boron nitride pottery side seal board is 20～70%.
3. boron nitride pottery side seal board for thin strap continuous casting according to claim 1, is characterized in that: described additive is MgAlON, AlON and CaAl
4o
7, the weight percent that described MgAlON accounts for described boron nitride pottery side seal board is that the weight percent that 5%, AlON accounts for described boron nitride pottery side seal board is 3%, CaAl
4o
7the weight percent that accounts for described boron nitride pottery side seal board is 2%.
4. boron nitride pottery side seal board for thin strap continuous casting according to claim 1, is characterized in that: described additive is MgAlON, CaZrO
3and CaTiO
3, the weight percent that described MgAlON accounts for described boron nitride pottery side seal board is 2%, described CaZrO
3the weight percent that accounts for described boron nitride pottery side seal board is 2%, described CaTiO
3the weight percent that accounts for described boron nitride pottery side seal board is 1%.
5. boron nitride pottery side seal board for thin strap continuous casting according to claim 1, is characterized in that: described additive is AlON, CaAl
4o
7, CaZrO
3and CaTiO
3, the weight percent that described AlON accounts for described boron nitride pottery side seal board is 5%, CaAl
4o
7the weight percent that accounts for described boron nitride pottery side seal board is 2%, CaZrO
3the weight percent that accounts for described boron nitride pottery side seal board is 2%, CaTiO
3the weight percent that accounts for described boron nitride pottery side seal board is 1%.
6. boron nitride pottery side seal board for thin strap continuous casting according to claim 1, is characterized in that: described additive is MgAlON, AlON, CaZrO
3and CaTiO
3, the weight percent that the weight percent that described MgAlON accounts for described boron nitride pottery side seal board is 1%, AlON accounts for described boron nitride pottery side seal board is 1%, CaZrO
3the weight percent that accounts for described boron nitride pottery side seal board is 2%, CaTiO
3the weight percent that accounts for described boron nitride pottery side seal board is 1%.
7. a preparation method for boron nitride pottery side seal board for thin strap continuous casting, is characterized in that, it comprises the steps:
Step 1: by hexagonal boron nitride powder, aluminum nitride powder, magnesium aluminium spinel powder, mullite powder and additive adopt wet ball grinding method to carry out ball-milling processing at least 12 hours with ball mill respectively, form respectively hexagonal boron nitride slurry, aluminium nitride slurry, magnesium-aluminium spinel slurry, mullite slurry and additive slurry, ball milling solvent in ball-milling processing process is that dehydrated alcohol or acetone or purity are more than 95% industrial spirit, in this ball-milling processing process, control hexagonal boron nitride slurry, aluminium nitride slurry, magnesium-aluminium spinel slurry, in mullite slurry and additive slurry, solid particulate granularity is 0.5～8 μ m, and then by hexagonal boron nitride slurry, aluminium nitride slurry, magnesium-aluminium spinel slurry, mullite slurry and additive slurry are dried respectively and are formed hexagonal boron nitride powder, aluminium nitride powder, magnesium-aluminium spinel powder, porzite powder and additive powder, described additive is MgAlON, AlON, CaAl
4o
7, CaZrO
3and CaTiO
3in one or more combination,
Step 2: be by mass percentage: hexagonal boron nitride 20～75%, aluminum nitride powder 10～55%, magnesium-aluminium spinel 5～40%, powder in mullite 5～20% and additive 0.5～15% selecting step 1 after drying and processing, and by ball mill by above-mentioned hexagonal boron nitride powder, aluminium nitride powder, magnesium-aluminium spinel powder, porzite powder and additive powder carry out wet ball grinding combination treatment, the ball milling solvent adopting in wet ball grinding combination treatment is that dehydrated alcohol or acetone or purity are more than 95% industrial spirit, wet ball grinding combination treatment is until hexagonal boron nitride powder, aluminium nitride powder, magnesium-aluminium spinel powder, porzite powder and additive powder mix, without layering, occur, it is form mixed slurry,
Step 3: mixed slurry is carried out to drying treatment, form mixed powder, recycling nodulizer carries out granulation processing to the mixed powder forming after dry, in granulation treating processes, control mixed powder particle size range and account for 10～20% below 0.5mm, particle size range accounts for 30～50% 0.5～1mm's, particle size range accounts for 10～35% 1.0～2.0mm's, and what particle size range was greater than 2mm accounts for 5～20%;
Step 4: all mixed powders that above-mentioned granulation is processed to resulting different-grain diameter are put into mixer and evenly mixed, and obtain coordinating powder;
Step 5: above-mentioned cooperation powder is put into graphite jig, adopt discharge plasma sintering process sintering to prepare side seal board base substrate, final sintering temperature in discharge plasma sintering process is 1400～2000 ℃, and in discharge plasma sintering process, corresponding atmosphere pressures is 5～50MPa during final sintering;
Step 6: adopt lathe to carry out processing treatment the side seal board base substrate after above-mentioned sintering, obtain boron nitride pottery side seal board for thin strap continuous casting.
8. the preparation method of boron nitride pottery side seal board for thin strap continuous casting according to claim 7, is characterized in that: in step 1, the purity of hexagonal boron nitride powder, aluminum nitride powder, magnesium aluminium spinel powder, mullite powder and additive all will reach analytical pure rank.
9. the preparation method of boron nitride pottery side seal board for thin strap continuous casting according to claim 7, is characterized in that: the Ball-milling Time of the wet ball grinding combination treatment of described step 2 is 12～48 hours.
10. the preparation method of boron nitride pottery side seal board for thin strap continuous casting according to claim 7, is characterized in that: the drying treatment of described step 3 is vacuum freeze-drying method or micro-wave drying method.
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