CN115321996A - Iron runner castable containing submicron composite antioxidant and preparation method thereof - Google Patents
Iron runner castable containing submicron composite antioxidant and preparation method thereof Download PDFInfo
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Abstract
The invention discloses an iron runner castable containing a submicron composite antioxidant and a preparation method thereof. The castable comprises plate-shaped corundum fine powder and active alpha-Al 2 O 3 Micro powder, silicon carbide, calcium aluminate cement, a carbon source, a submicron composite antioxidant, explosion-proof fibers, metal aluminum powder, a polycarboxylate dispersant and brown corundum particles; wherein the submicron composite antioxidant comprises B 4 C、ZrB 2 Elemental Si and MoSi 2 Four kinds of micron powder. The castable is prepared by mixing the raw materials to obtain a premix, adding water, stirring to obtain a wet mixed material, and pouring and vibration forming the wet mixed material. The iron runner castable realizes the anti-oxidation effect in the full temperature range, obviously improves the slag corrosion resistance and the scouring resistance of the material, prolongs the service life, and has wide application prospect.
Description
Technical Field
The invention belongs to the technical field of casting materials, and particularly relates to an iron runner casting material containing a submicron composite antioxidant and a preparation method thereof.
Background
The iron tap channel is the guarantee of smooth tapping of the blast furnace, and Al 2 O 3 the-SiC-C iron runner castable is the most mature material system applied at present, and must meet the harsh service conditions of physical scouring, chemical erosion, oxidation, thermal shock spalling caused by intermittent periodic tapping and the like on a tapping site. In fact, the oxidation resistance of the material system is one of the decisive factors of the service comprehensive performance of the material, and the oxidation of carbon/silicon carbide in the matrix causes the structure to be loose, thereby not only influencing the mechanical property and the thermal shock resistance of the castable, but also causing the corrosion and the penetration of the slag to the material to be more serious at high temperature. Generally, there are two main approaches to improving the oxidation resistance of carbonaceous materials: one is to introduce an additive to be oxidized in preference to the carbonaceous raw material, so as to reduce the oxygen partial pressure of the material, thereby playing the role of sacrificing self and protecting a carbon source; the other is to form stable oxide filler after oxidation by means of the additive to block air holes, thereby preventing further oxidation of the material. At present, B is generally adopted in iron runner castable 4 C and simple substance Si are used as antioxidant, in the actual use process, because the iron runner working lining can be used (1500 +/-50 ℃) only after being demoulded and baked (the baking temperature is 400-900 ℃), only a small amount of B is added 4 The C and the simple substance Si can not completely meet the anti-oxidation requirement, and the oxidation of the carbon material can influence the formation of an in-situ ceramic phase in a high-temperature service environment, so that the capability of resisting the erosion of the molten metal and the erosion of slag of the castable is obviously deteriorated, and therefore, a novel antioxidant system needs to be designed, the anti-oxidation in the full-temperature range is realized, and the service life of the iron runner castable is prolonged.
Disclosure of Invention
The invention aims to provide an iron runner castable containing a submicron composite antioxidant and a preparation method thereof. The iron runner castable realizes continuous anti-oxidation effect in the full temperature range, obviously improves the slag corrosion resistance and scouring resistance of the material, prolongs the service life, and has wide application prospect.
In order to solve the technical problems, the invention adopts the following technical scheme:
the iron runner castable containing the submicron composite antioxidant comprises the following components in percentage by mass:
5-12wt% of plate-like corundum fine powder and 4-7wt% of active alpha-Al 2 O 3 Micro powder, 2-5wt% of silicon micro powder, 10-20wt% of silicon carbide, 1-3wt% of calcium aluminate cement, 2-4wt% of carbon source, 2-4wt% of submicron composite antioxidant, 0.1-0.3wt% of explosion-proof fiber, 0.1-0.15wt% of metal aluminum powder, 0.1-0.2wt% of polycarboxylate dispersant and the balance of brown corundum particles; wherein:
the submicron composite antioxidant comprises B 4 C、ZrB 2 Elemental Si and MoSi 2 Four kinds of micron powder.
According to the scheme, in the submicron composite antioxidant, B 4 C、ZrB 2 Elemental Si and MoSi 2 The mass ratio of (1) to (0.5-2) to (3-4) to (0.5-2).
According to the scheme, the particle size of the submicron composite antioxidant is 100-200nm.
According to the scheme, B 4 C micro powder B 4 Content of C>99wt％，B 4 The granularity of the C micro powder is less than 45 mu m.
According to the scheme, the ZrB 2 ZrB in micropowder 2 In an amount of>99wt％，ZrB 2 Particle size of the fine powder<45μm。
According to the scheme, the content of Si in the simple substance Si powder is more than 98wt%, and the granularity of the simple substance Si powder is less than 45 mu m.
According to the scheme, the MoSi 2 MoSi in micro powder 2 In an amount of>99wt％，MoSi 2 The granularity of the micro powder is less than 45 mu m.
According to the scheme, al in the tabular corundum fine powder 2 O 3 In an amount of>99wt% of tabular corundum fine powder particle size<45μm。
According to the scheme, the active alpha-Al 2 O 3 Al in micro powder 2 O 3 In a content of>99wt%, active alpha-Al 2 O 3 Particle size of the fine powder<5μm。
According to the scheme, siO in the silicon micropowder 2 In a content of>95wt% of fine silica powder<2μm。
According to the scheme, the silicon carbide comprises silicon carbide fine powder and silicon carbide particles, the content of SiC is more than 98wt%, the particle size of the SiC particles is 1-0.1mm, and the particle size of the SiC micro powder is less than 75 mu m.
According to the scheme, al in the calcium aluminate cement 2 O 3 In an amount of>70wt% of calcium aluminate cement particle size<75μm。
According to the scheme, the carbon source is at least one of carbon black, spherical asphalt or graphite electrode powder.
Preferably, the carbon black is a submicron carbon black.
Preferably, the particle size of the spherical asphalt is less than or equal to 1mm.
Preferably, the particle size of the graphite electrode powder is less than or equal to 1mm.
According to the scheme, the granularity of the metal aluminum powder is less than 45 mu m.
According to the scheme, the explosion-proof fiber is common organic fiber.
According to the scheme, al in the brown corundum particles 2 O 3 In a content of>95wt%, the grain diameter of the brown corundum grains comprises 1-0.1mm,3-1mm,5-3mm and 8-5mm.
According to the scheme, the submicron composite antioxidant is prepared by the following steps:
b is to be 4 C、ZrB 2 Elemental Si and MoSi 2 Adding the four micron powders into a mechanical alloying high-energy ball mill, wherein the rotating speed of a main disc is 300-350r/min, the relative rotating speed of a ball milling tank is 625-675r/min, and the ball milling time is 18-22h, thus preparing the submicron composite antioxidant.
Preferably, the mass ratio of the ball material is 20.
The preparation method of the iron runner castable material containing the submicron composite antioxidant comprises the following steps:
1) Weighing plate-shaped corundum fine powder and activityα-Al 2 O 3 Uniformly mixing micro powder, silicon carbide, calcium aluminate cement, a carbon source, a submicron composite antioxidant, a polycarboxylate dispersant, explosion-proof fibers, metal aluminum powder and brown corundum particles to obtain a premix;
2) Adding water accounting for 3-6wt% of the premix obtained in the step 1) into the premix, uniformly mixing to obtain a wet mixed material, and pouring and vibration forming the wet mixed material to obtain the iron runner castable containing the submicron composite antioxidant.
The invention provides an iron runner castable containing a submicron composite antioxidant, wherein the submicron composite antioxidant comprises B 4 C、ZrB 2 Elemental Si and MoSi 2 The specific working mechanism of the four powders is as follows:
firstly, the composite antioxidant is in submicron order, the submicron-sized antioxidant has larger specific surface area, the oxidation temperature is advanced, the protection effect of the carbon component is further advanced, the preferential oxidation of the carbon component is realized, and the effect of protecting a carbon source is more favorably realized.
Secondly, the invention selects the antioxidant combination covered in the whole temperature range from low temperature to high temperature, fully exerts the sectional oxidation characteristics of each component and realizes the purpose of whole temperature range oxidation resistance. Wherein: b is 4 The temperature of C is about 500 ℃, and a few antioxidants which can be oxidized in priority to the carbon source generate a liquid phase B after oxidation 2 O 3 Can block the air holes, B along with the rise of the temperature 2 O 3 Can be mixed with SiO 2 Reaction to form borosilicate, and Al 2 O 3 Reacting to generate aluminum borate; zrB 2 The temperature for starting oxidation is about 800 ℃ compared with B 4 C, oxidation not only produces B 2 O 3 Also, stable oxides ZrO may be formed 2 The gas holes are filled to improve the density, and the gas holes can react with a matrix at high temperature (over 1200 ℃) to generate stable zirconite (zirconium silicate) and the like to improve the stability of an oxide layer; the simple substance Si starts to be oxidized at about 900 ℃, and can generate SiO under the condition of higher oxygen partial pressure 2 When the oxygen partial pressure is low, it will generateSiO vapor is generated and meets the air to generate SiO when the SiO vapor overflows to the surface 2 The air is prevented from entering, and the SiO is also beneficial to the growth of the silicon carbide crystal whisker; in fact, the SiC introduced in the material starts to oxidize at about 1100 ℃, the oxidation of which favours the formation of SiO at the interface 2 A protective layer; moSi 2 Oxidation to Mo at 1300 deg.C 3 O 5 And SiO 2 MoSi compared to elemental Si and SiC 2 The oxidation further promotes the stability of the silicate (borosilicate, zirconium silicate, etc.) protective layer.
Finally, the composite antioxidant is introduced, so that the oxygen partial pressure in the material is remarkably reduced, the growth of ceramic whiskers such as silicon carbide and the like is promoted by a gas-solid or gas-gas growth mechanism of a carbon component, the scouring resistance and the thermal shock resistance of the material are improved, and the problem of poor service efficiency caused by less formation of the ceramic whiskers in the material due to poor antioxidant effect, large oxidation of elemental silicon and the carbon component in the traditional channel castable is effectively solved.
The invention has the following beneficial effects:
the invention provides an iron runner castable material containing a submicron composite antioxidant, which is characterized in that a submicron composite antioxidant powder is obtained by reasonably matching several antioxidants with different oxidation temperature ranges, so that the temperature range of carbon material oxidation of the iron runner castable material is fully covered, and the antioxidant effect in the full temperature range is realized; meanwhile, the in-situ formation of a ceramic whisker reinforcement is promoted, and the condition of loose structure caused by oxidation of the castable is improved, so that the slag corrosion resistance and the scouring resistance of the material are obviously improved.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in detail by the following examples. The specific embodiments described herein are merely illustrative of the invention and are not intended to be limiting.
In order to avoid repetition, the materials related to the specific embodiment are uniformly described as follows, and are not described in the embodiment again:
B 4 c micro powder B 4 Content of C>99wt％，B 4 The granularity of the C micro powder is less than 45 mu m.
ZrB 2 ZrB in micropowder 2 In a content of>99wt％，ZrB 2 Particle size of the fine powder<45μm。
The content of Si in the simple substance Si powder is more than 98wt%, and the granularity of the simple substance Si powder is less than 45 mu m.
MoSi 2 MoSi in micro powder 2 In a content of>99wt％，MoSi 2 The granularity of the micro powder is less than 45 mu m.
Al in plate-like corundum fine powder 2 O 3 In an amount of>99wt% of tabular corundum fine powder particle size<45μm。
Active alpha-Al 2 O 3 Al in micro powder 2 O 3 In an amount of>99wt% active alpha-Al 2 O 3 Particle size of the fine powder<5μm。
SiO in silicon micropowder 2 In a content of>95wt% of fine silica powder<2μm。
The content of SiC in the silicon carbide fine powder and the SiC particles is more than 98wt%, the grain diameter of the SiC particles is 1-0.1mm, and the grain diameter of the SiC micro powder is less than 75 mu m.
Al in calcium aluminate cement 2 O 3 In an amount of>70wt% of calcium aluminate cement particle size<75μm。
The carbon source comprises carbon black, spherical asphalt and graphite electrode powder, wherein the carbon black is submicron carbon black, the particle size of the spherical asphalt is less than or equal to 1mm, and the particle size of the artificial graphite is less than or equal to 1mm.
The granularity of the metal aluminum powder is less than 45 mu m.
The explosion-proof fiber is common organic fiber.
Al in brown corundum 2 O 3 In an amount of>95wt%, the grain diameter of the brown corundum grain is 1-0.1mm,3-1mm,5-3mm and 8-5mm.
Example 1
The preparation method of the iron runner castable containing the submicron composite antioxidant comprises the following steps:
1) Preparation of submicron composite antioxidant powder
B is to be 4 C、ZrB 2 Elemental Si and MoSi 2 Four kinds of micro rice flourAdding the body (according to the weight ratio of 1.
2) Weighing the following raw materials:
weighing 7.12wt% of plate-shaped corundum fine powder and 4wt% of active alpha-Al 2 O 3 The raw materials of the composite antioxidant comprise micropowder, 3wt% of silica micropowder, 16wt% of silicon carbide micropowder and particles (the ratio of the micropowder to the particles is 9:7), 2wt% of calcium aluminate cement, 3.5wt% of a carbon source (the ratio of carbon black, spherical asphalt and graphite electrode powder is 2;
3) Uniformly mixing the raw materials weighed in the step 2) to obtain a premix;
4) Adding 4.2wt% of water into the premix obtained in the step 3), uniformly mixing to obtain a wet mixed material, and pouring and vibration-forming the wet mixed material to obtain the iron runner castable.
Sequentially carrying out maintenance, drying and heat treatment on the molded castable, and carrying out performance test; wherein:
1) The maintenance process comprises the following steps: curing for 24h at 25 ℃ and 75% humidity.
2) The drying process comprises the following steps: drying at 110 deg.C for 24h.
3) The heat treatment process comprises the following steps: preserving the heat for 3 hours at 1100 ℃; preserving the heat for 3 hours at 1450 ℃; preserving heat at 1450 ℃ for 3h, then placing the sample in a muffle furnace, heating to 900 ℃, preserving heat for 30min, then quickly taking out and placing in flowing tap water for water quenching experiment; and directly carrying out high-temperature breaking strength test after heat preservation for 0.5h at 1450 ℃.
4) The castable obtained in example 1 was subjected to strength tests after heat treatment at different temperatures:
(1) and in the heat treatment stage, the flexural strength of the castable is 10MPa and the compressive strength is 62MPa when the castable is subjected to heat treatment at 1100 ℃ for 3 hours.
(2) In the heat treatment stage, the rupture strength of the casting material is 12.6MPa and the compressive strength is 84MPa when the casting material is at 1450 ℃ for 3 hours; after the castable is quenched at 900 ℃ and tested, the breaking strength retention rate is 63%, and the compressive strength retention rate is 95%.
(3) And in the heat treatment stage, the high-temperature breaking strength of the casting material is 3.5MPa at 1450 ℃ for 0.5 h.
5) The castable obtained in example 1 was subjected to oxidation area test after heat treatment at different temperatures:
(1) after heat treatment at 1100 ℃ for 3h, the oxidation area of the sample accounts for 34%.
(2) After the heat treatment at 1450 ℃ for 3h, the oxidation area of the sample accounts for 20 percent.
Example 2
The preparation method of the iron runner castable containing the submicron composite antioxidant comprises the following steps:
1) Preparation of submicron composite antioxidant powder
B is to be 4 C、ZrB 2 Elemental Si and MoSi 2 Adding four kinds of micron powder (according to the weight ratio of 1.
2) Weighing the following raw materials:
weighing 7.12wt% of tabular corundum fine powder and 4wt% of active alpha-Al 2 O 3 The raw materials of the composite antioxidant comprise micropowder, 3wt% of silica micropowder, 16wt% of silicon carbide micropowder and particles (the ratio of the fine powder particles is 9:7), 2wt% of calcium aluminate cement, 3.5wt% of carbon source (the ratio of carbon black, spherical asphalt and graphite electrode powder is 2;
3) Uniformly mixing the raw materials weighed in the step 2) to obtain a premix;
4) Adding 4.2wt% of water into the premix obtained in the step 3), uniformly mixing to obtain a wet mixed material, and pouring and vibration-forming the wet mixed material to obtain a pouring material;
sequentially carrying out maintenance, drying and heat treatment on the molded castable, and carrying out performance test; wherein:
1) The maintenance process comprises the following steps: curing for 24h at 25 ℃ and 75% humidity.
2) The drying process comprises the following steps: drying at 110 deg.C for 24h.
3) The heat treatment process comprises the following steps: preserving the heat for 3 hours at 1100 ℃; preserving the heat for 3 hours at 1450 ℃; preserving heat at 1450 ℃ for 3h, then placing the sample in a muffle furnace, heating to 900 ℃, preserving heat for 30min, then quickly taking out and placing in flowing tap water for water quenching experiment; and directly carrying out high-temperature breaking strength test after heat preservation is carried out for 0.5h at 1450 ℃.
4) The strength of the casting material obtained in example 2 was tested after heat treatment at different temperatures:
(1) and in the heat treatment stage, the rupture strength of the castable is 12MPa and the compressive strength is 70MPa at 1100 ℃ for 3 h.
(2) In the heat treatment stage, the rupture strength of the castable is 13MPa and the compressive strength is 90MPa when the temperature is 1450 ℃ for 3 hours; after the casting material is quenched at 900 ℃ and tested, the breaking strength retention rate of the casting material is 69%, and the compressive strength retention rate of the casting material is 94%.
(3) And in the heat treatment stage, the high-temperature rupture strength of the castable is 4MPa at 1450 ℃ for 0.5 h.
5) The castable obtained in example 2 was subjected to heat treatment at different temperatures and then subjected to oxidation area test:
(1) after heat treatment at 1100 ℃ for 3h, the oxidation area of the sample accounts for 30%.
(2) After the heat treatment at 1450 ℃ for 3h, the oxidation area of the sample accounts for 17 percent.
Comparative example 1
The preparation method of the iron runner castable containing the common antioxidant comprises the following steps:
1) Weighing the following raw materials:
weighing 7.12wt% of tabular corundum fine powder4wt% of active alpha-Al 2 O 3 Fine powder, 3wt% of fine silica powder, 16wt% of fine silicon carbide powder and particles (fine powder particle ratio of 9:7), 2wt% of calcium aluminate cement, 3.5wt% of carbon source (carbon black, spherical pitch and graphite electrode powder ratio of 2 4 The proportion of C and simple substance Si is 1:5), 0.1wt% of explosion-proof fiber, 0.13wt% of metal aluminum powder, 0.15wt% of polycarboxylate dispersant and 61wt% of brown corundum particles are taken as raw materials;
2) Uniformly mixing the raw materials weighed in the step 1) to obtain a premix;
3) Adding 4.2wt% of water into the premix obtained in the step 2), uniformly mixing to obtain a wet mixed material, and pouring and vibration-forming the wet mixed material to obtain the castable.
Sequentially carrying out maintenance, drying and heat treatment on the molded castable, and carrying out performance test; wherein:
1) The maintenance process comprises the following steps: curing for 24h at 25 ℃ and 75% humidity.
2) The drying process comprises the following steps: drying at 110 deg.C for 24h.
3) The heat treatment process comprises the following steps: preserving the heat for 3 hours at 1100 ℃; preserving the heat for 3 hours at 1450 ℃; preserving heat at 1450 ℃ for 3h, then placing the sample in a muffle furnace, heating to 900 ℃, preserving heat for 30min, then quickly taking out and placing in flowing tap water for water quenching experiment; and directly carrying out high-temperature breaking strength test after heat preservation for 0.5h at 1450 ℃.
4) And (3) carrying out strength test on the castable obtained by the comparison ratio after heat treatment at different temperatures:
(1) and in the heat treatment stage, the rupture strength of the castable is 8.7MPa and the compressive strength is 58MPa at 1100 ℃ for 3 hours.
(2) In the heat treatment stage, the rupture strength of the castable is 11MPa and the compressive strength is 75MPa when the temperature is 1450 ℃ for 3 hours; after the casting material is quenched at 900 ℃ and tested, the breaking strength retention rate of the casting material is 59%, and the compressive strength retention rate of the casting material is 91%.
(3) And in the heat treatment stage, the high-temperature breaking strength of the casting material is 3.3MPa at 1450 ℃ for 0.5 h.
5) And (3) carrying out oxidation area test on the castable obtained by comparison after heat treatment at different temperatures:
(1) after heat treatment at 1100 ℃ for 3h, the oxidation area of the sample accounts for 44%.
(2) After the heat treatment at 1450 ℃ for 3h, the oxidation area of the sample accounts for 26 percent.
Claims (10)
1. The iron runner castable containing the submicron composite antioxidant is characterized by comprising the following components in percentage by mass:
5-12wt% of plate-like corundum fine powder and 4-7wt% of active alpha-Al 2 O 3 Micro powder, 2-5wt% of silicon micro powder, 10-20wt% of silicon carbide, 1-3wt% of calcium aluminate cement, 2-4wt% of carbon source, 2-4wt% of submicron composite antioxidant, 0.1-0.3wt% of explosion-proof fiber, 0.1-0.15wt% of metal aluminum powder, 0.1-0.2wt% of polycarboxylate dispersant and the balance brown corundum particles; wherein:
the submicron composite antioxidant comprises B 4 C、ZrB 2 Elemental Si and MoSi 2 Four kinds of micron powder.
2. The castable for iron runners according to claim 1, wherein in the submicron composite antioxidant, B 4 C、ZrB 2 Elemental Si and MoSi 2 The mass ratio of (1) to (0.5-2) to (3-4) to (0.5-2).
3. The castable for iron runners according to claim 1, wherein the particle size of the submicron composite antioxidant is 100-200nm.
4. The iron runner casting material of claim 1, wherein B is the same as B 4 The granularity of the C micro powder is less than 45 mu m; zrB 2 Particle size of the fine powder<45 μm; the granularity of the simple substance Si powder is less than 45 mu m; moSi 2 The granularity of the micro powder is less than 45 mu m.
5. The castable iron runner of claim 1, wherein the tabular corundum fines are included in the corundum finesAl 2 O 3 In an amount of>99wt% of tabular corundum fine powder particle size<45 μm; the active alpha-Al 2 O 3 Particle size of the micropowder<5 μm; the particle size of the silicon micropowder<2 μm; the silicon carbide comprises silicon carbide fine powder and silicon carbide particles, the particle size of the SiC particles is 1-0.1mm, the particle size of the SiC micropowder is<75μm。
6. The iron runner casting material of claim 1, wherein the carbon source is at least one of carbon black, spherical pitch, or graphite electrode powder.
7. The iron runner castable material of claim 1, wherein the metal aluminum powder has a particle size of < 45 μm; the explosion-proof fiber is common organic fiber.
8. The iron runner casting material of claim 1, wherein the calcium aluminate cement comprises Al 2 O 3 In an amount of>70wt% of calcium aluminate cement particle size<75 μm; in the brown corundum particles, al 2 O 3 In an amount of>95wt%, the grain diameter of the brown corundum grain is 1-0.1mm,3-1mm,5-3mm and 8-5mm.
9. The iron runner casting material of claim 1, wherein the submicron composite antioxidant is prepared by the following steps:
b is to be 4 C、ZrB 2 Elemental Si and MoSi 2 Adding the four micron powders into a mechanical alloying high-energy ball mill, wherein the rotating speed of a main disc is 300-350r/min, the relative rotating speed of a ball milling tank is 625-675r/min, and the ball milling time is 18-22h, thus preparing the submicron composite antioxidant.
10. A method for preparing the iron runner castable containing the submicron composite antioxidant as set forth in any one of claims 1-9, which is characterized by comprising the following steps:
1) Weighing plate-shaped corundum fine powder and active alpha-Al 2 O 3 Fine powder, fine silicon powder, and silicon carbideUniformly mixing calcium aluminate cement, a carbon source, a submicron composite antioxidant, a polycarboxylate dispersant, explosion-proof fibers, metal aluminum powder and brown corundum particles to obtain a premix;
2) Adding water accounting for 3-6wt% of the premix obtained in the step 1) into the premix, uniformly mixing to obtain a wet mixed material, and pouring and vibration forming the wet mixed material to obtain the iron runner castable containing the submicron composite antioxidant.
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