Carbonization of Ni-doped Phenol Resin Under Various Conditions

Ni-doped phenol resin was prepared with 1∶100 mass ratio of Ni（ NO_3）_2·6H_2O to thermosetting phenol resin to optimize the structure and properties of pyrolytic carbon derived from phenol resin and increase its carbon yield. The specimens were cured at 200 ℃ and carbonized under different atmospheres（ carbon-embedded atmosphere and Ar atmosphere） and at different temperatures（ 600,800,1000 and 1200 ℃） for3 h,respectively. The carbon yield was measured. Thermal decomposition characteristics of Ni-doped phenol resin,and the oxidation resistance,phase composition and microstructure of pyrolytic carbon were characterized by differential scanning calorimetry,X-ray diffraction,energy dispersive spectroscopy, scanning electron microscopy and transmission electron microscopy. The results show that the carbon yield of Ni-doped phenol resin carbonized at800 or 1 000 ℃ is increased significantly,compared with that without any dopants. The graphitization degree of pyrolytic carbon structure derived from Ni-doped phenol resin increases with the increase of carbonization temperature. The massive multi-wall carbon nanotubes of 50-100 nm in diameter and of micrometre scale in length are generated at 1000 ℃. Compared with the carbonembedded atmosphere,carbon nanotubes can be more easily generated in Ar atmosphere,resulting in higher carbon yield and degree of crystallinity of the pyrolyticcarbon derived from Ni-doped phenol resin. The oxidation resistance of the pyrolytic carbon derived from Ni-doped phenol resin at 1200 ℃ is improved significantly and its highest oxidation temperature is increased by about 84℃,compared with that from Ni free phenol resin.

Preparation and Performance of Zirconia Ceramic Ring for Slide Plate

The zirconia ceramic ring was prepared using fused monoclinic zirconia as main starting material, adopting composite stabilizer of magnesia, yttria and calcium nitrate, and applying recombination technology of traditional refractories and ceramics. Effect of the preparation process on material properties was comparatively studied, and the microstructure and phase composition were analyzed. The results show that adopting the high-speed mixing granulation process and the appropriate heat treatment can realize the control on the phase composition and microstructure, the zirconia ceramic ring with good thermal shock resitance and mechanical properties can be prepared.

Effect of Spherical Ni Powder on Microstructure of Secondary Carbon in MgO-C Refractories Matrix

In order to tackle the shortcomings of high brittleness,hard graphitization,and poor oxidation resistance resulted from carbonization of phenolic resin of Mg O- C refractories, effects of 2 mass% spherical Ni, and2 mass% spherical Ni plus 7. 5 mass% Al composite powder on microstructure of the secondary carbon in Mg O- C refractories matrix were investigated. The results show that a large number of carbon whiskers form after the carbonization of phenolic resin with Ni powder;in the Mg O- C refractories matrix with only Ni powder,the carbon microspheres form at all treatment temperatures and change slightly with the temperature rising;the carbon whiskers begin to generate in the specimens with composite powder at 1 000 ℃,the diameter of the carbon whiskers is about 0. 4- 0. 5 μm,and the length is about 3- 4 μm,and the formed carbon whiskers increase gradually with the temperature rising.

Preparation,Performance and Slag Resistant Mechanism of Low Thermal Conductivity Microporous Corundum

The microporous corundum material was prepared using alumina micro-powder as the main raw material, alumina sol and starch as binders by a wet process, achieving the bulk density of 3.05 g · cm^-3, the apparent porosity of 9. 1%, the closed porosity of 12.3%, the median pore diameter of 0. 43 μm, and the thermal conductivity of 6. 5 W· m^-1· K^-1 at 800 ℃ which is 41.6% lower than that of common corundum. The slag resistance of the microporous corundum material was studied by immersion and compared with that of the common corundum aggregate, and the slag resistant mechanism of microporous corundum material was revealed. The results show that the slag resistance of the microporous corundum material is superior to that of the common corundum aggregate, the SEM and EDX show that on the reaction interface between microporous corundum and molten, slag, a continuous isolation layer with a large quantity of CA2 and CA6 columnar crystals is formed; while the common corundum aggregate reacts with the molten slag interface to form a discontinuous isolation layer of columnar crystals, through which a lot of molten slag corrodes or permeates into the aggregate. The mechanism is mainly that the microporous structure is more advantageous to nucleation and growth of CA2 and CA6 columnar crystals; in the reaction with the aggregate, the molten slag gets saturated and the critical solution thickness of the microporous corundum and the common corundum is 0. 16 μm and 0. 34 μm, respectively, this is caused by the smaller microporous corundum aggregate pores; and the smaller pores also increase the second phase ripening rate of microporous corundum, which is 9. 7 times of that of the common corundum.

Preparation of Microporous Corundum and Its Effect on Properties of Al_2O_3-MgO Castables

Based on the pore size design of microporous aggregate by numerical simulation applying porous media model,α-Al2O3 micropowder,industrial Al2 O3fine powder,α-Al2O3 micropowder ＋ CaCO3 fine powder were used as starting materials,respectively,to prepare three microporous corundum aggregates specimens,named as A1,A2 and A3.Two lightweight Al2O3-MgO castables were prepared by selecting A1 or A3 as aggregate with O.6 μm of average pore size,then performances of castables with microporous corundum aggregates and castables with tabular corundum aggregates were compared.The results show that：（1） the microporous corundum aggregates with bulk density of 3.1-3.5 g · cm-3,apparent porosity of 5％,closed porosity of 8％-13％,and smaller thermal conductivity at 800 ℃ than tabular corundum,can be prepared by sintering at above 1 800 ℃ ; （2） compared to normal Al2 O3-MgO castables,the two lightweight Al2O3-MgO castables have lower bulk density and higher apparent porosity;lower change rate in dimensions and higher strength firing at 1 500 ℃ ; and lower thermal conductivity at 600 and 800 ℃ ; （3） compared to normal Al2O3-MgO castables,Al2O3-MgO castable with A1 has higher penetration index,and that with A3 has higher corrosion index and lower penetration index.

Effect of One/Two-dimensional Bonding Phases on Strength and Toughness of Carbon-containing Refractories

Gaseous phases of carbon-containing and metastable oxides will be resulted from the carbonization of phenolic resin binders and the reduced reactions between C and oxides at high temperatures in carbon-containing refractories. With the in-situ catalysis technique, these gaseous phases can be transformed to one-or two-dimensional bonding phases by deposition,which is favorable for the improvement on strength and toughness of carboncontaining refractories,especially low carbon refractories. The research results reveal that：（ 1） the amorphous carbon resulted from phenolic resin can be transformed to carbon nanotubes,thus,the oxidation peak temperature is raised from 506 to 664. 6 ℃;（ 2） onedimensional whiskers of MgO or Mg Al2 O4 can be in-situ formed in MgO-C refractories, and their CMOR,CCS,rupture displacement and residual CCS（ two water quenching cycles,1 100 ℃） are increased by 66%,47%,13% and 26%,respectively;（ 3） two-dimensional array structure of flake β-SiAlON can be in-situ formed in Al2 O3-C refractories,which improves the material strength by 60% and decreases the residual strength after thermal shock by only 4. 5 MPa. It is believed that the in-situ formation of one-or two-dimensional bonding phases at high temperatures can improvethe comprehensive thermal physical properties of carboncontaining refractories,and will be the developing trend of the strengthening and toughening of low carbon-containing refractories.

Influences of Binders on Properties of Highalumina Repairing Mix for Medium-frequency Induction Furnace

Three kinds of high-alumina repairing mixes for medium-frequency induction furnace were prepared by ramming method with sodium silicate, phosphoric acid and aluminium dihydrogen phosphate as binder, respectively. Physical properties of the specimens heat treated at different temperatures were tested and compared. The results show that the specimen bonded by sodium silicate behaves much higher strength after fired at 1 600 ℃ compared with the specimen, bonded by phosphoric acid or aluminium dihydrogen phosphate. Due to more liquid phase formation the properties of specimen bonded by sodium silicate are poor with a low strength and a large volume shrinkage at high temperatures. Meanwhile. the speeimen bonded by phosphoric acid and aluminium dihydrogen phosphate, respectively, show relatively high strengths and slight volume expansions at high temperatures because of in-situ mullite formation.

Effect of Pyrophyllite Particle Size on Properties of AI_2O_3-SiC-C Bricks for Iron Ladles

The Al2O3 -SiC-C bricks for iron ladles were pre-pared asing bauxite, fused corundum,pyrophyllite, SiC powder and flake graphite as main starting materials, and phenolic resin as binder. The effect of pyroph,yllite particle size on permanent change in dimensions, cold crushing strength, oxidation resistance, and corrosion resistance of Al2O3 - SiC - C bricks was investigated. The results show that with the decrease of the pyrophyllite particle size, the permanent change in dimensions of Al2O3 - SiC - C bricks decreases, cold crushing strength increases, the oxidation resistance at 1400 ℃ increases, and the corrosion resistance at 1500℃ decreases.

Effect of SiO2 Micropowder Addition on Properties of Alumina-magnesia Based Wet Gunning Mix for Working Layer

The magnesia - alumina based wet gunning mix was prepared using tabular corundum aggregates,fused mag- nesia aggregates, tabular corundum micropowder, silica mieropowder and pure calcium ahuninate cement as the main starting materials. Effects of silica micropowder ad- ditions （0, 0. 2% , 0. 5% , 1.0% , 1.5% , 2. 0% , and 2.5%, by mass, the same hewinafier） on properties oJ the gunning mix were researched. The results show that when ttze silica micropowder addition is i. 0% -2. 0% , the gunning mix has good .flou,ability and pumpability. Adding 2.5% silica micropowder, the nepheline forms at 1 600 ℃, which will reduce the high. temperature proper- ties of ntagnesia -ahtmina wet gunning mix. The intro- duction qf silica micropowder has obvious effects on cold mechanical properties of the gunning mix. For the speci- tnens dried at 110 ℃ , the strength increases slightly with the silica micropowder addition increasing. For the specimens heat-treated at 1 600 ℃ for 3 h, the strength in- creases nutrkedlv with the silica micropowder addition in- creasing. When keeping the water addition and particle size di, stribution constant, the residual linear expansion rate qf the specimen with 1.5% of silica micropowder is the lowest, ltot modulus tf rupture at 1 450 ℃ .for 0. 5 h oJ the specimens decreases gradually with the increase of silica fame addition. A small amount of silica micropow- der is beneficial for the slag penetration resistance.

Application Research of Dense Sintered Alumina in Iron Runner Castables

Three different kinds of corundum aggregates-tabular sintered alumina, dense sintered alumina, and fused dense corundum-were introduced into the silica fume .free or silica fume containing Al2O3 -SiC - C iron runner castables to investigate their influences on the flow ability, linear change on heating, bulk density, apparent porosity, cold strength, hot modulus of rupture, therm, al shock resistance, slag resistance, oxidation resistance as well as wear resistance of Al2O3 - SiC - C iron runner castables. The results show that （ 1 ） compared with the specimens with fused dense corundum, the specimens with dense sintered alumina have equivalent installation property, slag resistance and oxidation resistance, equivalent or even higher cold modulus of rupture, cold crushing strength and hot modulus of rupture, exhibiting better thermal shock resistance and cold wear resistance ; （2） adopting bimodal alumina micropowder LISAL22RABL as well as water reducers ZX2 and ZD2 can well reduce the water requirement of silica fume free castables, solving the problem of deteriorated flow ability resulted from the lack of silica fume; since the lack of silica fume avoids the formation of low melting point liquid, the hot modulus of rupture and the thermal shock resistance of the silica fume free castables are both better than those of the silica fume containing castables ; （3） the density of the castable specimens with dense sintered alumina is 4% -6% lower than that of the castable specimens with Jhsed dense corundum so the refractories consumption of one iron runner reduces by 5% by using the tastable with dense sintered alumina, which obviously reduces the cost of refractories.

Development and Application of Carbon-free Al_(2)O_(3)-MgO Dense Bricks for Steel Ladles

Carbon-free Al_(2)O_(3)-MgO dense bricks were produced by the pressing method,using tabular alumina,white fused alumina,alumina micro-powder as main raw materials,and inorganic powder as the binder.The comprehensive properties and performance in steel ladle side wall were made a comparison between Al_(2)O_(3)-MgO dense bricks and precast blocks.The results show that Al_(2)O_(3)-MgO dense bricks exhibit high dense structure and strength,as well as superior thermal shock resistance and better penetration and corrosion resistance to slag than precast blocks.While replacing precast blocks with dense bricks in 250 t steel ladle side wall in some domestic steel mills,the thickness of the metamorphic layer from slag penetration and the corrosion rate decrease evidently.The damage of dense bricks during service is mainly caused by the corrosion from molten steel and slag,and the structure spalling of the metamorphic layer also plays an important role.

Effect of Various Alumina Powders on Properties of Castables

To satisfy the requirements of alumina castables in specific environment and enhance their properties,alumina castables were prepared using tabular alumina,various alumina powders(07RAL,15RA,22RABL,40CA,99-20um,and 99-325mesh),and calcium aluminate cement as main raw materials,and heat treating at 110,1000,1600℃,respectively.Their flowability and physical properties were tested,and the morphology was researched.The results show that compared with calcined alumina and tabular alumina powders,reactive alumina has higher specific surface area and better filling performance leading to lower water demand and higher viscosity,and the castables prepared with reactive alumina have higher CCS and CMOR after heat treating at 110,1000 and 1600℃as well as lower PLC than those with calcined alumina and tabular alumina powders.

Effects of Four Kinds of Alumina Micropowder on Properties of Al_(2)O_(3)-C Refractories

In order to further improve the strength and the thermal shock resistance of Al_(2)O_(3)-C materials for steel ladle slide gates,the effects of four kinds of alumina micropowders(unimodal activated alumina micropowder 07RAL,unimodal activated alumina micropowder 15RA,bimodal activated alumina micropowder 22RABL,and calcined alumina micropowder 40CA)on the density,the strength and the thermal shock resistance of Al_(2)O_(3)-C materials were studied.The results show that the density,the strength and the thermal shock resistance of Al_(2)O_(3)-C materials can be improved with the introduction of activated alumina micropowders.Among them,the specimen with bimodal activated alumina micropowder shows the best comprehensive performance,especially the hot modulus of rupture.Its actual application results in steel mills show that the average service life of the Al_(2)O_(3)-C slide plates prolongs,and the problems of cast hole reaming,plate oxidation,roughening and cracking during the use of slide plates are obviously improved.

Thickness monitoring and discontinuous degradation mechanism of wear lining refractories for refining ladle

As a functional metallurgical container for molten steel,refining ladle has a great influence on the smelting safety and quality of steel.The online monitoring of the residual thickness for ladle lining was applied to increase the smelting efficiency and safety.It is found that the ladle refractories show obvious discontinuous degradation characteristics through the monitoring data.Moreover,the degradation of low-carbon magnesia–carbon brick at slag line and corundum-based castable at steel bath was calculated according to the established corrosion model and crack propagation model,respectively.The discontinuous degradation mechanism of the ladle refractories is illustrated,which is of great significance to the optimal configuration of the ladle lining refractories.