CN104844216A - Sialon-MgAl2O4-SiC complex phase wear-resistant ceramic material and preparation method therefor - Google Patents
Sialon-MgAl2O4-SiC complex phase wear-resistant ceramic material and preparation method therefor Download PDFInfo
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- CN104844216A CN104844216A CN201510152474.2A CN201510152474A CN104844216A CN 104844216 A CN104844216 A CN 104844216A CN 201510152474 A CN201510152474 A CN 201510152474A CN 104844216 A CN104844216 A CN 104844216A
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- sialon
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- magnesite
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- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 229910010293 ceramic material Inorganic materials 0.000 title abstract description 6
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 68
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 64
- 239000000843 powder Substances 0.000 claims abstract description 56
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 claims abstract description 36
- 229910000021 magnesium carbonate Inorganic materials 0.000 claims abstract description 36
- 239000001095 magnesium carbonate Substances 0.000 claims abstract description 36
- 235000014380 magnesium carbonate Nutrition 0.000 claims abstract description 36
- 239000002245 particle Substances 0.000 claims abstract description 28
- 239000007767 bonding agent Substances 0.000 claims abstract description 26
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000010453 quartz Substances 0.000 claims abstract description 18
- 238000000498 ball milling Methods 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 12
- 239000004375 Dextrin Substances 0.000 claims abstract description 11
- 229920001353 Dextrin Polymers 0.000 claims abstract description 11
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 11
- 235000019425 dextrin Nutrition 0.000 claims abstract description 11
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 11
- 229920001131 Pulp (paper) Polymers 0.000 claims abstract description 3
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 86
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 64
- 239000004411 aluminium Substances 0.000 claims description 53
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 52
- 239000000758 substrate Substances 0.000 claims description 47
- 229910020068 MgAl Inorganic materials 0.000 claims description 37
- 229910052757 nitrogen Inorganic materials 0.000 claims description 26
- 238000009413 insulation Methods 0.000 claims description 16
- 238000002156 mixing Methods 0.000 claims description 16
- 239000000203 mixture Substances 0.000 claims description 16
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 13
- 238000003825 pressing Methods 0.000 claims description 13
- 229920005551 calcium lignosulfonate Polymers 0.000 claims description 9
- RYAGRZNBULDMBW-UHFFFAOYSA-L calcium;3-(2-hydroxy-3-methoxyphenyl)-2-[2-methoxy-4-(3-sulfonatopropyl)phenoxy]propane-1-sulfonate Chemical compound [Ca+2].COC1=CC=CC(CC(CS([O-])(=O)=O)OC=2C(=CC(CCCS([O-])(=O)=O)=CC=2)OC)=C1O RYAGRZNBULDMBW-UHFFFAOYSA-L 0.000 claims description 9
- 239000000126 substance Substances 0.000 claims description 9
- 238000002203 pretreatment Methods 0.000 claims description 8
- 229910052742 iron Inorganic materials 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 4
- 229910021418 black silicon Inorganic materials 0.000 claims description 3
- 238000005868 electrolysis reaction Methods 0.000 claims description 3
- 229910003465 moissanite Inorganic materials 0.000 claims description 3
- 239000002994 raw material Substances 0.000 abstract description 18
- 238000005245 sintering Methods 0.000 abstract description 18
- 238000001035 drying Methods 0.000 abstract description 9
- 239000000654 additive Substances 0.000 abstract 1
- 230000000996 additive effect Effects 0.000 abstract 1
- 238000000462 isostatic pressing Methods 0.000 abstract 1
- 239000012299 nitrogen atmosphere Substances 0.000 abstract 1
- 239000002585 base Substances 0.000 description 42
- 239000002956 ash Substances 0.000 description 36
- 235000012239 silicon dioxide Nutrition 0.000 description 15
- 239000000919 ceramic Substances 0.000 description 12
- 239000000463 material Substances 0.000 description 10
- 230000003628 erosive effect Effects 0.000 description 9
- 238000006243 chemical reaction Methods 0.000 description 8
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 6
- 206010013786 Dry skin Diseases 0.000 description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- -1 Sialon Inorganic materials 0.000 description 5
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 5
- 239000003082 abrasive agent Substances 0.000 description 5
- 239000011449 brick Substances 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 238000007493 shaping process Methods 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- 229910010413 TiO 2 Inorganic materials 0.000 description 4
- 230000007797 corrosion Effects 0.000 description 4
- 238000005260 corrosion Methods 0.000 description 4
- 238000004064 recycling Methods 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 239000002893 slag Substances 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 229910052581 Si3N4 Inorganic materials 0.000 description 3
- 229910001037 White iron Inorganic materials 0.000 description 3
- 239000000956 alloy Substances 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 230000035939 shock Effects 0.000 description 3
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 3
- 238000013459 approach Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 235000010755 mineral Nutrition 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 239000002910 solid waste Substances 0.000 description 2
- 230000003245 working effect Effects 0.000 description 2
- 229910001018 Cast iron Inorganic materials 0.000 description 1
- 229910000599 Cr alloy Inorganic materials 0.000 description 1
- 229910000617 Mangalloy Inorganic materials 0.000 description 1
- 235000014676 Phragmites communis Nutrition 0.000 description 1
- GANNOFFDYMSBSZ-UHFFFAOYSA-N [AlH3].[Mg] Chemical compound [AlH3].[Mg] GANNOFFDYMSBSZ-UHFFFAOYSA-N 0.000 description 1
- 239000006061 abrasive grain Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 229910001563 bainite Inorganic materials 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 229910052728 basic metal Inorganic materials 0.000 description 1
- 150000003818 basic metals Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 244000309464 bull Species 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 239000000788 chromium alloy Substances 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005553 drilling Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 238000001513 hot isostatic pressing Methods 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 238000007373 indentation Methods 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 235000000396 iron Nutrition 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 229960001866 silicon dioxide Drugs 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 230000035882 stress Effects 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
- 239000003832 thermite Substances 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
Abstract
The present invention discloses a Sialon-MgAl2O4-SiC complex phase ceramic material and a preparation method therefor. As aluminum ash, magnesite and SiC are taken as raw materials, natural quartz powder services as an additive, and paper pulp dry powder, industrial dextrin or polyvinyl alcohol are taken as a bonding agent, the preparation method comprises the specific steps: firstly, the aluminum ash and the magnesite are subjected to ball milling to form mixed fine powder; secondly, SiC particles and fine powder are added into the mixed fine powder and uniformly agitated; a proper amount of the bonding agent is added and pressed into a blank; and the blank body is subjected to isostatic pressing treatment and drying, and is sintered in a high-temperature kiln under a nitrogen atmosphere so as to obtain the product. The Sialon-MgAl2O4-Sic complex phase wear resistant ceramic material prepared by adopting the method not only solves the problem of difficulty in sintering the SiC wear resistant ceramic material and low cost, but also provides an important technical way for zero emission resource utilization of the aluminum ash and the high-efficiency utilization of the magnesite.
Description
Technical field
The present invention relates to one utilizes industrial solid castoff aluminium ash, magnesite and silicon carbide to prepare Sialon-MgAl
2o
4-SiC multi-phase wear-resistant stupalith, belongs to high-abrasive material technical field.
Background technology
All the time, the research of erosion resistance mill material is caused to the extensive attention of Chinese scholars, and carried out intensive research work.From the developmental stage of wear-resisting erosion material, experienced by from evolutions such as ordinary white cast iron and manganese steel → ni-hard cast iron → high-chromium white cast iron → bainite ball cast irons.But, these metal and alloy materials under liquid-fixed double phase flow erosive wear and some Special Corrosion synergy conditions, due to its Anti-erosion abradability and chemical resistance poor, actual production requirement can not be met well.As the flow passage part in mining and mill run technique and scraper plate, industrial Pulp pump, Yellow River Channel dredging, variously stand the failure procedure that synergy that the corrosion resistant pump housing of erosion and flow passage part etc. be subjected to erosive wear and corrosion accelerates component.
Compared with industrial conventional metal and hard alloy wear resistance material, advanced ceramics material (aluminum oxide, zirconium white, aluminum oxide and zirconium oxide composite material, silicon nitride, silicon carbide ceramics etc.) has high intensity, hardness, the excellent properties such as high temperature resistant and corrosion-resistant, wear-resisting spare part uses and has shown excellent erosive resistance.Such as: the slurry pump ceramic cylinder jacket of Reed company of U.S. development reaches 2500h(current high-chromium alloy white cast iron drilling mud pump liner and be only 200 ~ 600h its work-ing life work-ing life), but price is very expensive.At present, such as the units such as Zhejiang University, Xi'an Communications University, University Of Tianjin, University of Science & Technology, Beijing of domestic minority universities and colleges have also carried out the research of relevant wear-resistant ceramic.Because the thermal conductivity of alumina-ceramic and zirconia ceramics is lower, their exist an outstanding technical problem is that its goods local temperature raises and easily forms thermal stresses under special operation condition condition, cause pottery easily cracking, impact is normal to be used, and alumina-ceramic and zirconia ceramics production cost higher, easily be out of shape during sintering, the problems such as yield rate is low constitute higher price, limit it and produce on a large scale and apply.Silicon nitride belongs to the compound of covalent bonds, although silicon nitride ceramics sintering character prepared by the method such as hot pressing, hot isostatic pressing is good, its facility investment is large, and product size is restricted, yielding poorly causes its production cost higher and limit its large-scale application.Silicon carbide has strong covalent linkage, and its crystal boundary energy is very high with the ratio of surface energy, and not easily obtain enough energy and form crystal boundary, therefore silicon carbide is difficult to sintering.In addition, velocity of diffusion during sintering is very low, and its surface is normal forms SiO2 film, and this layer of oxide film also plays diffusion barrier affects its sintering character further.Research shows that the mean sizes with SiC particle increases, and the wear rate of material reduces.This is due to when silicon-carbide particle size is larger than the depth of indentation of abrasive grain (or erosion particle), and silicon carbide has thrust inhibition to abrasive material, thus can improve wear resistance.Therefore often adopt SiC particle to be that raw material sintering prepares as high-abrasive material SiC ceramic, but between particle and particle, be difficult to sintering.
Along with the day by day exhaustion of natural high aluminum mineral resource, start to study around the solid waste of high aluminium content to carry out at searching high aluminum mineral surrogate and the work reduced in heat resistant and wear resistant material cost.Aluminium ash is the solid waste of slag after cooling processing produced in electrolytic aluminum or cast aluminum-molykote composite material production technique.Aluminium slag contains the metallic aluminium of 50% ~ 70% usually, and after the recycling of routine, the metallic aluminium still containing 15 ~ 30% in remaining aluminium scrap ash, discards because of the lower general extraction aluminium no longer further of grade.Also there is the Al2O3 of 10 ~ the 25% and AlN of 5 ~ 20% in aluminium ash simultaneously, contain comparatively high basic metal (Na, K etc.) and heavy metal (Zn, Cu etc.) compound in addition, do not add the waste utilizing and will cause resource, also bring the pollution of environment simultaneously.Realize the high efficiente callback of aluminium slag and the recycling of aluminium ash, it is important for effectively reducing the meaning of the impact that ecotope causes.
Magnesium-aluminium spinel has good thermal shock resistance, chemistry-resistant characteristic and wear resisting property and makes it be widely used in the every field such as refractory materials, high-abrasive material, fine ceramics.Al
2o
3, MgO and MgAl
2o
4three's thermal expansivity (mean thermal expansion coefficients between 20 ~ 1000K/DEG C
-1) be respectively 8.8 × 10
-6, 13.5 × 10
-6, 7.6 × 10
-6, by contrast, the thermal shock resistance of MgO is not as good as Al
2o
3, Al
2o
3anti-slag alkali erosiveness can be inferior to MgO, MgAl
2o
4thermal expansivity is minimum, and therefore thermal shock resistance is better.When synthetic MgAl spinal, with the volumetric expansion of 5% ~ 8%, the effect that stress plays activeness and quietness can be produced in the material.Sialon and MgAl
2o
4phase compound as SiC in conjunction with phase, in conjunction with both advantages, the NEW TYPE OF COMPOSITE Sialon-MgAl of excellent property can be prepared
2o
4in conjunction with SiC wear-resistant ceramic material.
Summary of the invention
The technical problem to be solved in the present invention be at present as high-abrasive material metal and alloy materials due to distinct issues such as starting material are expensive and erosive resistance difference and advanced wear-resistant ceramic material sintering difficulty under special conditions, production cost be high, provide the control of the raw materials such as a kind of high alumina industrial solid castoff aluminium of industrial easy acquisition ash, magnesite and SiC by design of components and thermite reduction nitrogenizing reaction sintering to prepare low-cost and high-performance New Si alon-MgAl for this reason
2o
4-SiC multi-phase wear-resistant stupalith.
Technical scheme of the present invention is: a kind of Sialon-MgAl
2o
4-SiC multi-phase wear-resistant stupalith, is characterized in that it comprises aluminium ash, magnesite, SiC, natural quartz powder and bonding agent, and described bonding agent is paper pulp dry powder, industrial dextrin or polyvinyl alcohol solution at least one wherein.
Optionally, the ash of aluminium described in such scheme is that the aluminium aluminium that is grey or founding generation that electrolysis produces is grey, and the chemical constitution of described aluminium ash is counted in mass ratio: Al
2o
35% ~ 40%, AlN0% ~ 20%, Al10% ~ 40%, MgO 5% ~ 20%, SiO
25% ~ 35%, Fe
2o
3≤ 4.0%, Na
2o≤3.0%, described aluminium ash accounts for 15 ~ 30% of total batching massfraction; Described magnesite accounts for 5 ~ 30% of total batching massfraction; Described natural quartz powder accounts for 0 ~ 20% of total batching massfraction; SiC is green silicon carbide or black silicon carbide, accounts for 40 ~ 70% of total batching massfraction, and described bonding agent accounts for 3% ~ 10% of total batching massfraction.
Optionally, MgCO in magnesite described in such scheme
3mass content be greater than 90%.
Optionally, in such scheme, the grain composition ratio of SiC is: the small-particle 10 ~ 30% of the middle particle 10 ~ 40%, 0 ~ 0.15mm of the macrobead 30 ~ 50%, 1 ~ 0mm of 3 ~ 1mm, is less than the fine powder 0 ~ 15% of 0.074mm; Described grain composition ratio is for accounting for the massfraction of the total add-on of SiC.
Optionally, in such scheme, bonding agent is selected from least one in the polyvinyl alcohol solution of the industrial dextrin of concentration 30%, the calcium lignosulfonate solution of concentration 30% and concentration 10%.
Sialon-MgAl
2o
4the preparation method of-SiC multi-phase wear-resistant stupalith, first with levigate equipment, magnesite and aluminium ash are carried out levigate pre-treatment, make its granularity≤0.074mm, again in mass ratio the ratio of 5 ~ 30:15 ~ 30:40 ~ 70 by magnesite, aluminium ash and natural quartz powder carry out sufficient ball milling and are mixed to form mixing fine powders, mixing fine powders and SiC are prepared burden, be uniformly mixed by stirrer, add the bonding agent accounting for base substrate total mass 3% ~ 10% and be pressed into base substrate, by base substrate through the process of 100MPa ~ 300MPa isostatic cool pressing, then by base substrate at 50 DEG C of dry 4h, dry 4h at 100 DEG C, base substrate is placed in high temperature nitrogen steam stove and is incubated 1 ~ 3h prior to 1100 ~ 1200 DEG C under flowing nitrogen protection, again in 1350 ~ 1450 DEG C of insulation 1 ~ 5h, it sinters inferior to 1550 DEG C ~ 1750 DEG C insulation 2 ~ 10h, finally naturally cooling to room temperature with stove under nitrogen protection can obtain this Sialon-MgAl
2o
4-SiC multi-phase wear-resistant stupalith.
Optionally, in such scheme, the temperature increasing schedule of high temperature nitrogen steam stove is: during from room temperature to 1000 DEG C, temperature rise rate is 5 ~ 8 DEG C/min; When more than 1000 DEG C, temperature rise rate 2 ~ 5 DEG C/min.
A kind of Sialon-MgAl
2o
4preparation technology's flow process of-SiC multi-phase wear-resistant stupalith is:
Raw material → raw materials pretreatment (pulverizing and jevigating sieves) → first batching → dry ball milling → add SiC second batch → be uniformly mixed → add bonding agent to make base substrate → isostatic pressed process → drying → nitrogenizing reaction sintering → processing → use
The invention has the beneficial effects as follows the Sialon-MgAl of preparation
2o
4-SiC multi-phase wear-resistant stupalith effectively can not only reduce the cost of wear-resistant ceramic, and the efficiency utilization of the zero release recycling and magnesite that can be high alumina industrial solid castoff aluminium ash provides important technological approaches, the multi-phase wear-resistant stupalith use properties of preparation is excellent.Sialon and MgAl of this System forming
2o
4in conjunction with the problem solving SiC mutually and be difficult to sinter, the sintering temperature of SiC can be reduced simultaneously.The silicon-dioxide oxide film of surface of SiC can be formed Si by the metallic aluminium reduction nitridation in aluminium ash
3n
4/ Sialon, can strengthen the combination of SiC particle and particle and SiC particle and matrix further.The Sialon-MgAl of this System forming
2o
4in conjunction with SiC material, there is excellent Erosive Properties.The present invention can be the playing a role in promoting of high-performance abrasion-proof ceramic complex phase material cost degradation technology, and can be widely used in being used as in the industry such as cement, electric power, mine the material of the wearing pieces such as wear-resistant ball, abrasion-proof pipe, nozzle, bull ring are complete, impeller.
Embodiment
Below in conjunction with embodiment, the present invention will be further described.
The present invention adopt composition of raw materials and proportioning be respectively: aluminium ash (can be electrolysis produce aluminium ash also can be founding produce aluminium ash, its chemical constitution (
w): Al
2o
35% ~ 20%, AlN0% ~ 10%, Al10% ~ 20%, MgO 5% ~ 15%, SiO
25% ~ 15%, Fe
2o
3≤ 4.0%, Na
2o≤3.0%) account for 15 ~ 30% of total batching massfraction; Magnesite (MgCO
3content general requirement is greater than 90%) account for 10 ~ 30% of total batching massfraction; Natural quartz powder (SiO
2content is generally greater than 88%, and granular size is≤0.074mm) account for 0 ~ 20% of total batching massfraction; SiC(can be green silicon carbide also can be black silicon carbide) particle and fine powder account for 40 ~ 70% of total batching massfraction, its grain composition is the macrobead 30 ~ 50% of (massfraction accounting for the total add-on of SiC): 3 ~ 1mm, the middle particle 10 ~ 40% of 1 ~ 0mm, the small-particle 10 ~ 30% of 0 ~ 0.15mm, is less than the fine powder 0 ~ 15% of 0.074mm; Bonding agent can adopt that concentration is about 30% industrial dextrin, concentration be about 30% calcium lignosulfonate solution or concentration be about 10% polyvinyl alcohol solution wherein a kind of, also can be wherein two kinds be combined as bonding agent, or concentration be about 30% industrial dextrin, concentration be about 30% calcium lignosulfonate solution and concentration be the polyvinyl alcohol solution of about 10% as bonding agent, bonding agent accounts for 3% ~ 10% of total batching massfraction.
First with vibration mill or other fine powder levigate equipment, magnesite and aluminium ash are carried out levigate pre-treatment (making granularity≤0.074mm), again in required ratio by magnesite, aluminium ash and natural quartz powder carry out sufficient ball milling and are mixed to form mixing fine powders, then by magnesite, aluminium ash and the mixing fine powders of natural quartz powder and the SiC particle of different-grain diameter and fine powder are prepared burden according to the above ratio, be uniformly mixed by stirrer, adding the interim bonding agent accounting for base substrate total mass 3% ~ 10% (generally can adopt concentration to be about 30% industrial dextrin, concentration be about 30% calcium lignosulfonate solution or concentration be the polyvinyl alcohol solution of about 10%) be pressed into base substrate, by base substrate through the process of 100MPa ~ 300MPa isostatic cool pressing, then by base substrate 50 DEG C of dryings 4 hours, dry 4h at 100 DEG C, base substrate is placed in high temperature nitrogen steam stove and is incubated 1 ~ 3h prior to 1100 ~ 1200 DEG C under flowing nitrogen protection, again in 1350 ~ 1450 DEG C of insulation 1 ~ 5h, finally in 1550 DEG C ~ 1750 DEG C insulation 2 ~ 10h(temperature increasing schedules: from room temperature to 1000 DEG C of temperature rise rates, 5 ~ 8 DEG C/min, more than 1000 DEG C, 2 ~ 5 DEG C/min) sinter, finally naturally cooling to room temperature with stove under nitrogen protection can obtain this Sialon-MgAl
2o
4-SiC multi-phase wear-resistant stupalith.
A kind of Sialon-MgAl
2o
4preparation technology's flow process of-SiC multi-phase wear-resistant stupalith is:
Raw material → raw materials pretreatment (pulverizing and jevigating sieves) → first batching → dry ball milling → add SiC second batch → be uniformly mixed → add bonding agent to make base substrate → isostatic pressed process → drying → nitrogenizing reaction sintering → processing → use
The present invention prepares Sialon-MgAl
2o
4-SiC multi-phase wear-resistant stupalith effectively can not only reduce the cost of wear-resistant ceramic, and the efficiency utilization of the zero release recycling and magnesite that can be high alumina industrial solid castoff aluminium ash provides important technological approaches, the multi-phase wear-resistant stupalith use properties of preparation is excellent.
embodiment 1
Raw material:
The aluminium ash that electrolytic aluminum produces, its chemical constitution (
w): Al
2o
318.02%, AlN 14.13%, Al 18.62%, MgO 7.1%, SiO
25.9%, Fe
2o
34.0%, CaO 2.8%, Na
2o 2.6%, TiO
21.6%, loss on ignition 12.8%, other 12.43%, account for 20% of total batching massfraction;
Magnesite (MgCO
3content 92.4%) account for 12% of total batching massfraction;
Natural quartz powder (SiO
2content 90.6%, granular size is≤0.074mm) account for 5% of total batching massfraction;
SiC(green silicon carbide) account for 63% of total batching massfraction, its grain composition is (massfraction accounting for the total add-on of SiC): particle 30% in 3 ~ 1mm macrobead, 45%, 1 ~ 0mm, and 0 ~ 0.15mm small-particle 15%, is less than 0.074mm fine powder 10%;
Bonding agent can adopt concentration to be about 30% industrial dextrin, accounts for 3% of total batching massfraction.
Raw materials pretreatment:
First with vibration mill or other fine powder levigate equipment, magnesite and aluminium ash are carried out levigate pre-treatment, cross 200 mesh sieves.
First batching and ball milling:
According to the above ratio magnesite, aluminium ash and natural quartz powder are carried out batching and ball milling 4h, form mixing fine powders.
Again prepare burden and mix:
Then the SiC of mixing fine powders and different-grain diameter is prepared burden according to the above ratio, stir 2h by stirrer, batching is mixed.
Shaping:
Be that about 30% industrial dextrin joins in batching by the above-mentioned concentration accounting for base substrate total mass 3%, be suppressed into sample base substrate by brick pressing machine, specimen size is 10 × 10 × 80mm, forming pressure 50MPa.Sample base substrate is closely knit through isostatic cool pressing pressurization, pressure 200MPa pressurize 1min.
Dry:
Then by base substrate 50 DEG C of dryings 4 hours, dry 4h at 100 DEG C, after dry, the moisture of sample base substrate should control be less than 0.1%.
Nitrogenizing reaction sinters:
Base substrate is placed in high temperature nitrogen steam stove and is incubated 2h prior to 1200 DEG C under flowing nitrogen protection; again in 1350 DEG C of insulation 2h; it is inferior to 1600 DEG C of insulation 4h(temperature increasing schedules: from room temperature to 1000 DEG C of temperature rise rates, 5 DEG C/min; more than 1000 DEG C; 2 DEG C/min) sinter, finally naturally cool to room temperature with stove under nitrogen protection and can obtain this Sialon-MgAl
2o
4-SiC multi-phase wear-resistant stupalith.
The physicochemical property of sample is: XRD result shows that its crystalline phase is SiC, Sialon, MgAl
2o
4; After sintering, the apparent porosity of sample is 7.0%, and volume density is 3.15g/cm
3, strength at normal temperature is 192.2MPa; Dimension formula hardness is 15.2GPa, and wear resisting property is good.
embodiment 2
Raw material:
The aluminium ash that electrolytic aluminum produces, its chemical constitution (
w): Al
2o
318.02%, AlN 14.13%, Al 18.62%, MgO 7.1%, SiO
25.9%, Fe
2o
34.0%, CaO 2.8%, Na
2o 2.6%, TiO
21.6%, loss on ignition 12.8%, other 12.43%, account for 25% of total batching massfraction;
Magnesite (MgCO
3content 92.4%) account for 10% of total batching massfraction;
Natural quartz powder (SiO
2content 90.6%, granular size is≤0.074mm) account for 8% of total batching massfraction;
SiC(green silicon carbide) account for 52% of total batching massfraction, its grain composition is (massfraction accounting for the total add-on of SiC): particle 30% in 3 ~ 1mm macrobead, 45%, 1 ~ 0mm, and 0 ~ 0.15mm small-particle 15%, is less than 0.074mm fine powder 10%;
Bonding agent can adopt concentration be about 10% polyvinyl alcohol solution, account for 5% of total batching massfraction.
Raw materials pretreatment:
First with vibration mill or other fine powder levigate equipment, magnesite and aluminium ash are carried out levigate pre-treatment, cross 200 mesh sieves.
First batching and ball milling:
According to the above ratio magnesite, aluminium ash and natural quartz powder are carried out batching and ball milling 4h, form mixing fine powders.
Again prepare burden and mix:
Then the SiC of mixing fine powders and different-grain diameter is prepared burden according to the above ratio, stir 5h by stirrer, batching is mixed.
Shaping:
The polyvinyl alcohol solution being about 10% by the above-mentioned concentration accounting for base substrate total mass 5% joins in batching, is suppressed into sample base substrate by brick pressing machine, and specimen size is 10 × 10 × 80mm, forming pressure 50MPa.Sample base substrate is closely knit through isostatic cool pressing pressurization, pressure 200MPa pressurize 1min.
Dry:
Then by base substrate 50 DEG C of dryings 4 hours, dry 4h at 100 DEG C, after dry, the moisture of sample base substrate should control be less than 0.1%.
Nitrogenizing reaction sinters:
Base substrate is placed in high temperature nitrogen steam stove and is incubated 1h prior to 1200 DEG C under flowing nitrogen protection; again in 1350 DEG C of insulation 3h; it is inferior to 1550 DEG C of insulation 6h(temperature increasing schedules: from room temperature to 1000 DEG C of temperature rise rates, 5 DEG C/min; more than 1000 DEG C; 2 DEG C/min) sinter, finally naturally cool to room temperature with stove under nitrogen protection and can obtain this Sialon-MgAl
2o
4-SiC multi-phase wear-resistant stupalith.
The physicochemical property of sample is: XRD result shows that its crystalline phase is SiC, Sialon, MgAl
2o
4; After sintering, the apparent porosity of sample is 8.5%, and volume density is 3.10g/cm
3, strength at normal temperature is 184.8MPa; Dimension formula hardness is 15.0GPa, and wear resisting property is good.
embodiment 3
Raw material:
The aluminium ash that electrolytic aluminum produces, its chemical constitution (
w): Al
2o
318.02%, AlN 14.13%, Al18.62%, MgO 7.1%, SiO
25.9%, Fe
2o
34.0%, CaO 2.8%, Na
2o 2.6%, TiO
21.6%, loss on ignition 12.8%, other 12.43%, account for 15% of total batching massfraction;
Magnesite (MgCO
3content 92.4%) account for 10% of total batching massfraction;
Natural quartz powder (SiO
2content 90.6%, granular size is≤0.074mm) account for 5% of total batching massfraction;
SiC(green silicon carbide) account for 70% of total batching massfraction, its grain composition is (massfraction accounting for the total add-on of SiC): particle 30% in 3 ~ 1mm macrobead, 45%, 1 ~ 0mm, and 0 ~ 0.15mm small-particle 15%, is less than 0.074mm fine powder 10%;
Bonding agent can adopt concentration be about 30% calcium lignosulfonate solution, account for 3% of total batching massfraction.
Raw materials pretreatment:
First with vibration mill or other fine powder levigate equipment, magnesite and aluminium ash are carried out levigate pre-treatment, cross 200 mesh sieves.
First batching and ball milling:
According to the above ratio magnesite, aluminium ash and natural quartz powder are carried out batching and ball milling 6h, form mixing fine powders.
Again prepare burden and mix:
Then the SiC of mixing fine powders and different-grain diameter is prepared burden according to the above ratio, stir 5h by stirrer, batching is mixed.
Shaping:
The calcium lignosulfonate solution being about 30% by the above-mentioned concentration accounting for base substrate total mass 3% joins in batching, is suppressed into sample base substrate by brick pressing machine, and specimen size is 10 × 10 × 80mm, forming pressure 50MPa.Sample base substrate is closely knit through isostatic cool pressing pressurization, pressure 200MPa pressurize 1min.
Dry:
Then by base substrate 50 DEG C of dryings 4 hours, dry 4h at 100 DEG C, after dry, the moisture of sample base substrate should control be less than 0.1%.
Nitrogenizing reaction sinters:
Base substrate is placed in high temperature nitrogen steam stove and is incubated 2h prior to 1200 DEG C under flowing nitrogen protection; again in 1350 DEG C of insulation 2h; it is inferior to 1650 DEG C of insulation 4h(temperature increasing schedules: from room temperature to 1000 DEG C of temperature rise rates, 5 DEG C/min; more than 1000 DEG C; 2 DEG C/min) sinter, finally naturally cool to room temperature with stove under nitrogen protection and can obtain this Sialon-MgAl
2o
4-SiC multi-phase wear-resistant stupalith.
The physicochemical property of sample is: XRD result shows that its crystalline phase is SiC, Sialon, MgAl
2o
4; After sintering, the apparent porosity of sample is 6.2%, and volume density is 3.19g/cm
3, strength at normal temperature is 227.4MPa; Dimension formula hardness is 16.5GPa, and wear resisting property is good.
embodiment 4
Raw material:
The aluminium ash that electrolytic aluminum produces, its chemical constitution (
w): Al
2o
35%, Al 10%, MgO 5%, SiO
25%, Fe
2o
33.0%, CaO 26.77%, Na
2o 2.4%, TiO
27.6%, loss on ignition 12.8%, other 22.43%, account for 30% of total batching massfraction;
Magnesite (MgCO
3content 93.4%) account for 5% of total batching massfraction;
SiC(green silicon carbide) account for 40% of total batching massfraction, its grain composition is (massfraction accounting for the total add-on of SiC): particle 30% in 3 ~ 1mm macrobead, 45%, 1 ~ 0mm, and 0 ~ 0.15mm small-particle 15%, is less than 0.074mm fine powder 10%;
Bonding agent can adopt concentration to be the calcium lignosulfonate solution of about 30% and the industrial dextrin of concentration 30%, accounts for 10% of total batching massfraction.
Raw materials pretreatment:
First with vibration mill or other fine powder levigate equipment, magnesite and aluminium ash are carried out levigate pre-treatment, cross 200 mesh sieves.
First batching and ball milling:
According to the above ratio magnesite and aluminium ash are carried out batching and ball milling 6h, form mixing fine powders.
Again prepare burden and mix:
Then the SiC of mixing fine powders and different-grain diameter is prepared burden according to the above ratio, stir 5h by stirrer, batching is mixed.
Shaping:
Join in batching by the above-mentioned bonding agent accounting for base substrate total mass 10%, be suppressed into sample base substrate by brick pressing machine, specimen size is 10 × 10 × 80mm, forming pressure 50MPa.Sample base substrate is closely knit through isostatic cool pressing pressurization, pressure 200MPa pressurize 1min.
Dry:
Then by base substrate 50 DEG C of dryings 4 hours, dry 4h at 100 DEG C, after dry, the moisture of sample base substrate should control be less than 0.1%.
Nitrogenizing reaction sinters:
Base substrate is placed in high temperature nitrogen steam stove and is incubated 3h prior to 1100 DEG C under flowing nitrogen protection; again in 1450 DEG C of insulation 1h; it is inferior to 1750 DEG C of insulation 2h(temperature increasing schedules: from room temperature to 1000 DEG C of temperature rise rates, 8 DEG C/min; more than 1000 DEG C; 5 DEG C/min) sinter, finally naturally cool to room temperature with stove under nitrogen protection and can obtain this Sialon-MgAl
2o
4-SiC multi-phase wear-resistant stupalith.
The physicochemical property of sample is: XRD result shows that its crystalline phase is SiC, Sialon, MgAl
2o
4; After sintering, the apparent porosity of sample is 6.3%, and volume density is 3.18g/cm
3, strength at normal temperature is 228.4MPa; Dimension formula hardness is 16.7GPa, and wear resisting property is good.
embodiment 5
Raw material:
The aluminium ash that electrolytic aluminum produces, its chemical constitution (
w): Al
2o
320%, AlN10 %, Al 20%, MgO 15%, SiO
215%, loss on ignition 7.57%, other 22.43%, account for 30% of total batching massfraction;
Magnesite (MgCO
3content 94.4%) account for 30% of total batching massfraction;
Natural quartz powder (SiO
2content 90.6%, granular size is≤0.074mm) account for 20% of total batching massfraction;
SiC(green silicon carbide) account for 40% of total batching massfraction, its grain composition is (massfraction accounting for the total add-on of SiC): particle 30% in 3 ~ 1mm macrobead, 45%, 1 ~ 0mm, and 0 ~ 0.15mm small-particle 15%, is less than 0.074mm fine powder 10%;
Bonding agent can adopt concentration to be the calcium lignosulfonate solution of about 30% and the polyvinyl alcohol solution of concentration 10%, accounts for 10% of total batching massfraction.
Raw materials pretreatment:
First with vibration mill or other fine powder levigate equipment, magnesite and aluminium ash are carried out levigate pre-treatment, cross 200 mesh sieves.
First batching and ball milling:
According to the above ratio magnesite and aluminium ash are carried out batching and ball milling 6h, form mixing fine powders.
Again prepare burden and mix:
Then the SiC of mixing fine powders and different-grain diameter is prepared burden according to the above ratio, stir 5h by stirrer, batching is mixed.
Shaping:
Join in batching by the above-mentioned bonding agent accounting for base substrate total mass 10%, be suppressed into sample base substrate by brick pressing machine, specimen size is 10 × 10 × 80mm, forming pressure 50MPa.Sample base substrate is closely knit through isostatic cool pressing pressurization, pressure 200MPa pressurize 1min.
Dry:
Then by base substrate 50 DEG C of dryings 4 hours, dry 4h at 100 DEG C, after dry, the moisture of sample base substrate should control be less than 0.1%.
Nitrogenizing reaction sinters:
Base substrate is placed in high temperature nitrogen steam stove and is incubated 3h prior to 1100 DEG C under flowing nitrogen protection; again in 1450 DEG C of insulation 1h; it is inferior to 1750 DEG C of insulation 2h(temperature increasing schedules: from room temperature to 1000 DEG C of temperature rise rates, 8 DEG C/min; more than 1000 DEG C; 5 DEG C/min) sinter, finally naturally cool to room temperature with stove under nitrogen protection and can obtain this Sialon-MgAl
2o
4-SiC multi-phase wear-resistant stupalith.
The physicochemical property of sample is: XRD result shows that its crystalline phase is SiC, Sialon, MgAl
2o
4; After sintering, the apparent porosity of sample is 6.6%, and volume density is 3.28g/cm
3, strength at normal temperature is 226.4MPa; Dimension formula hardness is 16.9GPa, and wear resisting property is good.
Claims (8)
1. a Sialon-MgAl
2o
4-SiC multi-phase wear-resistant stupalith, is characterized in that it comprises aluminium ash, magnesite, SiC, natural quartz powder and bonding agent, and described bonding agent is paper pulp dry powder, industrial dextrin or polyvinyl alcohol solution at least one wherein.
2. a kind of Sialon-MgAl as claimed in claim 1
2o
4-SiC multi-phase wear-resistant stupalith, is characterized in that: described aluminium ash is that the aluminium aluminium that is grey or founding generation that electrolysis produces is grey, and the chemical constitution of described aluminium ash is counted in mass ratio: Al
2o
35% ~ 20%, AlN0% ~ 10%, Al10% ~ 20%, MgO 5% ~ 15%, SiO
25% ~ 15%, Fe
2o
3≤ 4.0%, Na
2o≤3.0%, described aluminium ash accounts for 15 ~ 30% of total batching massfraction; Described magnesite accounts for 5 ~ 30% of total batching massfraction; Described natural quartz powder accounts for 0 ~ 20% of total batching massfraction; SiC is green silicon carbide or black silicon carbide, accounts for 40 ~ 70% of total batching massfraction, and described bonding agent accounts for 3% ~ 10% of total batching massfraction.
3. a kind of Sialon-MgAl as claimed in claim 1
2o
4-SiC multi-phase wear-resistant stupalith, is characterized in that: MgCO in described magnesite
3mass content be greater than 90%.
4. a kind of Sialon-MgAl as claimed in claim 1
2o
4-SiC multi-phase wear-resistant stupalith, is characterized in that: the SiO in described natural quartz powder
2mass content is greater than 88%, and granular size is≤0.074mm.
5. a kind of Sialon-MgAl as claimed in claim 1
2o
4-SiC multi-phase wear-resistant stupalith, is characterized in that: the grain composition ratio of SiC is: the small-particle 10 ~ 30% of the middle particle 10 ~ 40%, 0 ~ 0.15mm of the macrobead 30 ~ 50%, 1 ~ 0mm of 3 ~ 1mm, is less than the fine powder 0 ~ 15% of 0.074mm; Described grain composition ratio is for accounting for the massfraction of the total add-on of SiC.
6. the Sialon-MgAl as described in any one of claim 1-5
2o
4-SiC multi-phase wear-resistant stupalith, is characterized in that: bonding agent is selected from least one in the polyvinyl alcohol solution of the industrial dextrin of concentration 30%, the calcium lignosulfonate solution of concentration 30% and concentration 10%.
7. the Sialon-MgAl as described in any one of claim 1-6
2o
4the preparation method of-SiC multi-phase wear-resistant stupalith, it is characterized in that: first with levigate equipment, magnesite and aluminium ash are carried out levigate pre-treatment, make its granularity≤0.074mm, again in mass ratio the ratio of 5 ~ 30:15 ~ 30:40 ~ 70 by magnesite, aluminium ash and natural quartz powder carry out sufficient ball milling and are mixed to form mixing fine powders, mixing fine powders and SiC are prepared burden, be uniformly mixed by stirrer, add the bonding agent accounting for base substrate total mass 3% ~ 10% and be pressed into base substrate, by base substrate through the process of 100MPa ~ 300MPa isostatic cool pressing, then by base substrate at 50 DEG C of dry 4h, dry 4h at 100 DEG C, base substrate is placed in high temperature nitrogen steam stove and is incubated 1 ~ 3h prior to 1100 ~ 1200 DEG C under flowing nitrogen protection, again in 1350 ~ 1450 DEG C of insulation 1 ~ 5h, it sinters inferior to 1550 DEG C ~ 1750 DEG C insulation 2 ~ 10h, finally naturally cooling to room temperature with stove under nitrogen protection can obtain this Sialon-MgAl
2o
4-SiC multi-phase wear-resistant stupalith.
8. Sialon-MgAl as claimed in claim 7
2o
4the preparation method of-SiC multi-phase wear-resistant stupalith, is characterized in that: the temperature increasing schedule of high temperature nitrogen steam stove is: during from room temperature to 1000 DEG C, temperature rise rate is 5 ~ 8 DEG C/min; When more than 1000 DEG C, temperature rise rate 2 ~ 5 DEG C/min.
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