KR20160136766A - Zirconia refractory materials for superhigh temperature using nano-powder - Google Patents
Zirconia refractory materials for superhigh temperature using nano-powder Download PDFInfo
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
- C04B35/481—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates containing silicon, e.g. zircon
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
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- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3418—Silicon oxide, silicic acids, or oxide forming salts thereof, e.g. silica sol, fused silica, silica fume, cristobalite, quartz or flint
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Abstract
The present invention relates to a zirconia refractory material for high temperature using a nano-powder, zirconia (ZrO 2) of silicon oxide relative to 100 parts by weight of (SiO 2) 1 ~ 2 parts by weight of particles containing size 325mesh (0.043㎜) the following raw material powder 70 (ZrO 2 ) nano powder having a particle size of 10 to 1,000 nm in a range of 0.1 to 30% by weight with respect to 99.9 wt% to 99.9 wt% of the raw material powder, and the raw material powder has a cubic zirconia (Cubic-ZrO 2 ) , And the zirconia refractory material is sintered at a density of about 3.2 to 4.0 g / cm 3.
The ultra-high temperature zirconia refractory material using the nano powder of the present invention can be obtained by forming and sintering various shapes of refractory materials by using zirconia nano powder having an interfacial energy insecure as a binder in a zirconia powder having a particle size of less than 325 mesh (0.043 mm) Low thermal conductivity, excellent heat resistance, fire resistance and light weight.
Further, since the organic or inorganic binder which is sintered in liquid phase at the time of refractory material fabrication and zirconia nano powder which does not contain a carbon component and is the same component as the mother phase plays a role of binding the parent phase, There is an advantage that the problem of acting as a pollution source in the furnace can be prevented originally.
Description
The present invention relates to an ultra-high temperature zirconia refractory material using nanopowder, and more particularly, to a zirconia refractory material having a particle size of less than 325 mesh (0.043 mm) and a zirconia nano powder having insufficient interfacial energy as a binder. And more particularly to a zirconia refractory for ultra-high temperature using nanopowder having low thermal conductivity, excellent heat resistance, fire resistance and light weight even at an ultra-high temperature of 2,000 DEG C or higher.
Refractory inorganic oxide raw materials such as alumina, magnesia, zirconia and the like or carbonaceous bond such as graphite are formed have poor wettability to slag and excellent corrosion resistance But it is excellent in thermal shock resistance because of low thermal conductivity and modulus of elasticity. Particularly, since the refractory material containing the fixed carbon raw material such as graphite as the base particles is more remarkable in its characteristics, it is widely used as a refractory material for the interior of equipment such as a crosstrain, a converter, a ladle, In recent years, as the conditions of use of refractories become too severe, higher strength and thermal shock resistance are required.
The refractory material containing the refractory inorganic oxide material or the fixed carbon is mainly used as a refractory brick material in the steelmaking and casting process of steelworks because it is directly or indirectly contacted with molten steel at about 1,600 ° C to be exposed to periodic thermal shock, Heat resistance, corrosion resistance, and anti-scratch resistance to slag or slag are required.
Accordingly, in order to impart properties such as corrosion resistance and anti-spalling property to the refractory material containing fixed carbon, impression graphite has been mainly used as a carbon raw material. However, in order to use graphite as a refractory for refractory bricks, And an expensive antioxidant must be added.
In addition, carbon has a property that it is not easily wetted by melts such as slugs, and a refractory material containing carbon is widely used as a refractory material that is recently installed in various molten metal containers because of its excellent durability. For example, when the magnesia is used as the refractory aggregate, the refractory material is applied to the inside of the molten metal vessel due to the characteristics of the carbon and the corrosion resistance of the magnesia to the molten metal, thereby exhibiting excellent corrosion resistance and heat resistance.
However, as the use of carbon-containing refractories increases, the carbon in the refractories leaks into molten metal, so-called carbon pick-up. Particularly, in recent years, the demand for high-quality steel is more strict, and the demand for a refractory material having a smaller carbon content is increasing. Further, low heat conductive refractory materials are inevitably required in terms of environmental protection such as suppression of heat radiation from heat resistant facilities and energy conservation, and research and development of low carbon content refractory materials is steadily being carried out.
In general, the refractory has a very wide variety of particle distributions ranging from a granulation of about 5 mm to a finer particle size of 1 탆 or less, and aggregates of a so-called matrix, which fills the gaps of relatively large particles, There are many pores or voids in the matrix portion, which affects the strength of the refractory, permeability to melts such as slugs, and relaxation of thermal shock.
As regards the prior art related to zirconia refractories similar to the present invention, Korean Patent Laid-Open No. 10-2009-0091696 (Ebonik Degussa GmbH, Germany) comprises at least one granular refractory component and at least one binder, wherein , The particulate refractory component has an average particle diameter > 0.3 mu m, the binder has a mean particle diameter of 10 nm to 0.3 mu m, and contains 0.05 to 50 wt% of aluminum oxide, titanium dioxide, zirconium dioxide, and / 0 to 20% by weight of a hydraulic binder, 0 to 15% by weight of an organic silicon-free binder, 0 to 35% by weight of an organosilicon coupling agent, Wherein the ratio of the particulate refractory component is 100 and the ratio of the additional material in the formulation is less than or equal to the granular component The refractory material is sintered in a liquid phase during the production of a sintered body by using an inorganic binder, and thus the refractory material produced in this way is an inorganic binder in which the inorganic binder is volatilized at a high temperature, It is recognized that there is a problem that it acts as a pollution source in a furnace.
In addition, in Korean Patent Registration No. 10-1012106 (Korea Research Institute of Standards and Science), zirconium chloride and yttrium nitrate solution are prepared; The solution is mixed and heated to form a pale yellow gel; Firing the pale yellow gel to form amorphous zirconia; Wet-milling the zirconia and then drying at 50 to 70 ° C to form amorphous zirconia powder; And heating the amorphous zirconia powder to form crystalline yttrium oxide stabilized square zirconia polycrystals (3Y-TZP).
On the other hand, in the present invention, a nano-scale (not more than 1 탆) zirconia powder having substantially the same composition as the zirconia raw material powder is contained, which is mixed with crude raw material powders so that the nanoparticles act as a binder, The present invention has been accomplished by developing a zirconia refractory material for ultra-high temperature having low thermal conductivity, excellent heat resistance, fire resistance and light weight even at an ultra-high temperature of 2,000 DEG C or more.
It is an object of the present invention to provide a zirconia powder having a particle size of 325 mesh (0.043 mm) or less and a zirconia nano powder having an interfacial energy unstable in place of an inorganic binder as a binder to form and sinter various shapes of refractory materials, And to provide an ultra-high temperature zirconia refractory using nano powder having excellent heat resistance, fire resistance and light weight.
The zirconia refractory material for ultra-high temperature using the nano powder according to the present invention is characterized by containing raw material powder having a particle size of 325 mesh (0.043 mm) or less containing 1 to 2 parts by weight of silicon oxide (SiO 2 ) relative to 100 parts by weight of zirconia (ZrO 2 ) (ZrO 2 ) nano powder having a particle size of 10 to 1,000 nm in an amount of 0.1 to 30% by weight based on the weight%.
Also, the raw material powder is made of cubic zirconia (ZrO 2 ), and the zirconia refractory material is sintered to a density of about 3.2 to 4.0 g / cm 3.
The ultra-high temperature zirconia refractory material using the nano powder of the present invention can be obtained by forming and sintering various shapes of refractory materials using zirconia nano powder having insufficient interfacial energy as a binder in a zirconia powder having a particle size of less than 325 mesh (0.043 mm) Low thermal conductivity, excellent heat resistance, fire resistance and light weight.
Further, since the organic or inorganic binder which is sintered in liquid phase at the time of refractory material fabrication and zirconia nano powder which does not contain a carbon component and is the same component as the mother phase plays a role of binding the parent phase, There is an advantage that the problem of acting as a pollution source in the furnace can be prevented originally.
The zirconia refractory material for ultra-high temperature using the nano powder according to the present invention is characterized by containing raw material powder having a particle size of 325 mesh (0.043 mm) or less containing 1 to 2 parts by weight of silicon oxide (SiO 2 ) relative to 100 parts by weight of zirconia (ZrO 2 ) (ZrO 2 ) nano powder having a particle size of 10 to 1,000 nm in the range of 0.1 to 30% by weight based on the weight%.
Hereinafter, a zirconia refractory material for ultra-high temperature using the nanopowder according to the present invention will be described. It is to be appreciated that those skilled in the art will readily understand the present invention, It is not intended to limit the technical spirit and scope of the present invention.
Zirconia (ZrO 2 ) is a heat resistant material having a high melting temperature (2,700 ° C) of a molecular weight of 123.22, and is excellent in low thermal conductivity, chemical resistance, low thermal expansion, abrasion resistance, high strength, high hardness, excellent fracture toughness and ionic conductivity Material. However, since pure zirconia has a property of changing its crystal shape from tetragomal to monoclinic at a temperature of 1,170 ° C, it is easily broken due to volume change. Therefore, conventionally pure yttria (Y 2 O 3 ) To stabilize zirconia to improve strength and fracture toughness.
In the present invention, by using a raw material powder containing 1 to 2 parts by weight of silicon oxide (SiO 2 ) relative to 100 parts by weight of zirconia (ZrO 2 ), zirconia is formed in cubic zirconia (Cubic-ZrO 2 ) And the vinegar powder state is maintained.
When the content of silicon oxide (SiO 2 ) is less than 1 part by weight with respect to 100 parts by weight of zirconia (ZrO 2 ), the zirconia crystal may spontaneously deform from a square to a monotone shape, Can lead to fatal problems in the physical and mechanical properties of zirconia refractory materials. When the content of silicon oxide (SiO 2 ) is more than 2 parts by weight, the high temperature stability of the refractory material, that is, the heat resistance and the refractoriness, is lowered due to fusion welding of silicon oxide (SiO 2 ) having a relatively low melting point.
In addition, since the zirconia raw material powder can be manufactured using a sintered body having a particle size of 325 mesh (0.043 mm) or less, the final product combined with the zirconia nano powder, that is, the sintered body having a zirconia refractory material of about 3.2 to 4.0 g / It is possible to appropriately maintain low heat conductivity, excellent heat resistance and fire resistance even at light temperature and ultra-high temperature of 2,000 DEG C or more.
In order to achieve the above-described characteristics, the present invention includes zirconia (ZrO 2 ) nano powder having a particle size of 10 to 1,000 nm in an amount of 0.1 to 30 wt% based on 70 to 99.9 wt% of the raw material powder, The refractory material is formed and sintered. The zirconia nanopowder may be produced by a hydrothermal synthesis method, a sol-gel synthesis method, a gas phase synthesis method, or the like. Recently, a zirconium salt solution is heated to form a gel, which is then fired to form amorphous zirconia. The amorphous zirconia powder is then wet-milled and dried to form amorphous zirconia powder, which is then heated to form crystalline zirconia- A zirconia nano powder to be formed may be used.
On the other hand, various kinds of additives and auxiliaries are used in the production of refractory raw materials, and a binder is very important here. For example, as a conventional organic binder, cellulose derivatives, sulfite steels, tar, pitch, resins and the like have increased sensitivity to porosity and corrosion as they are decomposed or volatilized at temperatures exceeding about 250 ° C, It has strength.
Further, when an inorganic binder such as an aqueous solution of phosphoric acid or a salt thereof, water glass and silica sol or the like is used, the steel produced in contact with the refractory material may cause undesired contamination of the product produced by melting or firing. Further, Thermal and mechanical properties may be deteriorated. In the case of refractory cements based on hydraulic binders such as cement, especially calcium aluminate and hydrated alumina, there is a disadvantage in that it is decomposed in a temperature range of 1,000 ° C. or lower. Even when a sub ingredient such as CaO is introduced into the refractory cement, Resulting in deterioration of thermal and mechanical properties.
In order to solve the problems of the conventional binder as described above, in the present invention, the zirconia nano powder is mixed between the coarse zirconia powders in the process of mixing the refractory material and serves as a binder for the zirconia raw material powder through the forming and sintering processes do.
Since the nano-state zirconia has the same chemical composition as that of the zirconia-based raw material powder, it has no reactivity and is good in kneading property. Therefore, the sintered body containing the zirconia has low density and hydrophobicity, The product is uniform, has excellent water resistance, oil resistance and durability, and does not cause swelling due to moisture penetration.
The zirconia nano powder has a matrix in which a gap between the raw powder powders having a particle size of 325 mesh (0.043 mm) or less is very large, and a large number of pores are present in the matrix portion, and the strength, And mitigating action of heat shock. It is generally known that the particle size of the matrix of the refractory material is about 44 탆 or less. However, the inventors of the present invention have found the fact that the behavior of ultrafine particles having a size of 10 탆 to 1 탆, Respectively.
In other words, the reduction of the refractory porosity leads to the improvement of the corrosion resistance, and the shape control and the refinement of the pores contribute to the improvement of the thermal shock resistance. In the present invention, by controlling the pore structure, the heat resistance of the refractory material is improved, In addition to its oxidative properties, it aims to improve low thermal conductivity, excellent heat resistance, fire resistance and light weight.
The present inventors have paid attention to the size and the ratio of the pores existing in the structure of the refractory material in the high zirconia region. The presence of these pores leads to an increase in the contact area between the zirconia material powders present in the refractory material, and the zirconia nano- The zirconia (ZrO 2 ) nano powder having a particle size of 10 to 1,000 nm in an amount of not less than 0.1% by weight and not more than 30% by weight based on 70 to 99.9% by weight of the raw material powder having a particle size of not more than 325 mesh (0.043 mm) % In the range of < RTI ID = 0.0 >
On the other hand, unlike the above zirconia nano powder, carbon black is known as a carbonaceous raw material that is a nano-grade fine particle. It is possible to control a certain degree of pore structure by controlling the particle size thereof, but a refractory material using carbon black as a matrix material Corrosion resistance and oxidation resistance are not sufficient. In the past, when a sintered body was manufactured using an organic or inorganic binder for bonding raw material powders, the binder was sintered in liquid phase to bond the mother phase. In the present invention, The use of the nano powder as a matrix prevents the components such as the binder contained in the refractory material from volatilizing at a high temperature and acting as a contamination source in the furnace as in the prior art.
The zirconia refractory material for ultra-high temperature according to the present invention is compressed into axial or equilibrium at a very high press pressure, for example, in a press mold, molded into a medium density of about 3.2 to 4.0 g / cm 3, dried and sintered, And the refractory material using the nano powder of the same composition as that of the present invention as a binder has good product stability, good drying and sintering properties.
Accordingly, the zirconia refractory material for ultra-high temperature using the nanopowder manufactured according to the present invention can be variously substituted, modified and changed without departing from the technical idea of the present invention, and it has a low thermal conductivity and excellent heat resistance even at an ultra- Fire resistance and light weight, as well as refractory materials that can be used for steel and non-ferrous industries and ceramics manufacturing facilities requiring the above-mentioned characteristics.
Claims (3)
And a zirconia (ZrO 2 ) nano powder having a particle size of 10 to 1,000 nm in a range of 0.1 to 30 wt%.
Wherein the raw material powder is in the cubic zirconia (Cubic-ZrO 2 ) state.
Wherein the zirconia refractory material is sintered at a density of about 3.2 to 4.0 g / cm < 3 >.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108285350A (en) * | 2018-01-31 | 2018-07-17 | 景德镇陶瓷大学 | A kind of tri compound SiC based refractories and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108285350A (en) * | 2018-01-31 | 2018-07-17 | 景德镇陶瓷大学 | A kind of tri compound SiC based refractories and preparation method thereof |
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