CN101456740B - Method for in-situ synthesis of MgAlON/beta-sialon composite ceramic material - Google Patents
Method for in-situ synthesis of MgAlON/beta-sialon composite ceramic material Download PDFInfo
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- CN101456740B CN101456740B CN2009100760600A CN200910076060A CN101456740B CN 101456740 B CN101456740 B CN 101456740B CN 2009100760600 A CN2009100760600 A CN 2009100760600A CN 200910076060 A CN200910076060 A CN 200910076060A CN 101456740 B CN101456740 B CN 101456740B
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- 238000000034 method Methods 0.000 title claims abstract description 14
- 230000015572 biosynthetic process Effects 0.000 title claims abstract description 9
- 238000003786 synthesis reaction Methods 0.000 title claims abstract description 8
- 239000002131 composite material Substances 0.000 title claims description 20
- 229910010293 ceramic material Inorganic materials 0.000 title abstract description 9
- 238000011065 in-situ storage Methods 0.000 title abstract 2
- 239000000463 material Substances 0.000 claims abstract description 41
- 239000002994 raw material Substances 0.000 claims abstract description 32
- 239000000919 ceramic Substances 0.000 claims abstract description 25
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 15
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 10
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 32
- 229910052749 magnesium Inorganic materials 0.000 claims description 32
- 239000011777 magnesium Substances 0.000 claims description 32
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 24
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 claims description 18
- 239000004411 aluminium Substances 0.000 claims description 13
- 239000000843 powder Substances 0.000 claims description 13
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 12
- 235000013312 flour Nutrition 0.000 claims description 10
- 239000000377 silicon dioxide Substances 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 6
- 238000000498 ball milling Methods 0.000 claims description 4
- 238000005245 sintering Methods 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 238000013461 design Methods 0.000 claims description 3
- 239000012895 dilution Substances 0.000 claims description 3
- 238000010790 dilution Methods 0.000 claims description 3
- 239000004677 Nylon Substances 0.000 claims description 2
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 claims description 2
- 229920003123 carboxymethyl cellulose sodium Polymers 0.000 claims description 2
- 229940063834 carboxymethylcellulose sodium Drugs 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 229920001778 nylon Polymers 0.000 claims description 2
- 238000003825 pressing Methods 0.000 claims description 2
- 238000002791 soaking Methods 0.000 claims description 2
- 239000000243 solution Substances 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- 239000002893 slag Substances 0.000 abstract description 6
- 239000011819 refractory material Substances 0.000 abstract description 3
- 238000001308 synthesis method Methods 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 abstract description 2
- 230000003628 erosive effect Effects 0.000 abstract description 2
- 238000002360 preparation method Methods 0.000 abstract description 2
- 230000035939 shock Effects 0.000 abstract description 2
- 229910052710 silicon Inorganic materials 0.000 abstract description 2
- 239000010703 silicon Substances 0.000 abstract description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 abstract 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract 2
- 240000002871 Tectona grandis Species 0.000 abstract 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract 1
- 239000003638 chemical reducing agent Substances 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 abstract 1
- 239000000395 magnesium oxide Substances 0.000 abstract 1
- 239000011863 silicon-based powder Substances 0.000 abstract 1
- 230000002194 synthesizing effect Effects 0.000 abstract 1
- 238000006243 chemical reaction Methods 0.000 description 8
- 229910052581 Si3N4 Inorganic materials 0.000 description 6
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 230000007797 corrosion Effects 0.000 description 4
- 238000005260 corrosion Methods 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- GANNOFFDYMSBSZ-UHFFFAOYSA-N [AlH3].[Mg] Chemical compound [AlH3].[Mg] GANNOFFDYMSBSZ-UHFFFAOYSA-N 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 229910052596 spinel Inorganic materials 0.000 description 3
- 239000011029 spinel Substances 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 238000001778 solid-state sintering Methods 0.000 description 2
- 229910018516 Al—O Inorganic materials 0.000 description 1
- 229910007991 Si-N Inorganic materials 0.000 description 1
- 229910003564 SiAlON Inorganic materials 0.000 description 1
- 229910006294 Si—N Inorganic materials 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000000156 glass melt Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910052752 metalloid Inorganic materials 0.000 description 1
- 150000002738 metalloids Chemical class 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 230000002829 reductive effect Effects 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
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Abstract
The invention discloses an MgAlON/beta-Sialon diphase ceramic material obtained by in-situ synthesis by a reducing nitridation method, which belongs to the technical field of structural ceramics and refractory materials. The used raw materials by mass percentage comprise 2 to 30 percent of silicon powder, 2 to 10 percent of aluminum powder, 40 to 85 percent of alumina, and 3 to 15 percent of magnesia; the MgAlON/beta-Sialon diphase material comprises 40 to 95 percent of MgAlON and 5 to 60 percent of beta-Sialon; and the material is subjected to one-step synthesis by adopting a high-temperature reduction nitridation synthesis method. The requirement of preparation technology for synthesizing the MgAlON/beta-Sialon diphase ceramic material comprises: nitrogen is introduced during the high-temperature heat treatment, the atmosphere pressure is 0.1Mpa, the temperature is between 1,500 and 1,800 DEG C, and the holding time is between 2 and 8 hours. The invention teaks silicon and aluminum as a reducing agent to synthesize the MgAlON/beta-Sialon diphase ceramic material through reducing nitridation, has the advantages of a single-phase MgAlON material or a beta-Sialon material respectively, and has the characteristics of high strength, good toughness, good slag erosion resistance, and excellent thermal shock resistance.
Description
Technical field
The invention belongs to structural ceramics and fire resisting material field, relate to a kind of diphase ceramic material, material has mechanical property preferably, and synthetic controllability is strong.
Background technology
Magnesium-aluminium spinel has identical crystalline structure and close lattice parameter with A Long, and at high temperature they can form far-ranging sosoloid magnesium A Long.Magnesium A Long material has excellent optics, mechanics, dielectric properties; The high-temperature thermal stability performance is good, resistance to slag corrosion is good; Wettability to glass melt and molten iron is little, in fields such as optical window material and refractory materials, have broad application prospects, but heat-shock resistance is relatively poor relatively.Magnesium A Long material generally can adopt solid state sintering, the metallic reducing nitrogenize is synthetic and carbothermal reduction-nitridation is synthetic; The metallic reducing nitrogenize is to be the direct nitrogenizing reaction synthesis method of raw material with Natural manganese dioxide or magnesium-aluminium spinel and metallic aluminium powder; Metallic aluminium is a transition plasticity phase in the building-up process; It is nitrided into AlN in building-up process, and active attitude and the Natural manganese dioxide (magnesium-aluminium spinel) with new life is combined to magnesium A Long then, and metal can be brought into play plasticity and act on mutually in moulding and sintering process; Be of value to the raising of material property, its reduction-nitridation is following:
Al+MgO+Al
2O
3+N
2→MgAlON
β-Sai Long is that z Si-N key in the beta-silicon nitride replaced formation by z Al-O key, advances Al and O atom in the mid-transsexual ground solid solution of the lattice of beta-silicon nitride, is formed with distored beta-silicon nitride lattice.β-Sai Long is a crystalline phase the most stable in the sialon material, and being considered to best also is high temperature resistant sialon material the most likely.β-Sai Long has lower thermal expansivity, higher intensity and toughness, and its thermal expansivity is littler than beta-silicon nitride, so heat-shock resistance is superior to beta-silicon nitride, the oxidation-resistance of β-Sai Long obviously is superior to beta-silicon nitride simultaneously, and close with silit.β-Sai Long has very high anti-molten metal attack and blast-furnace slag erosive ability, so β-Sailong and silicon carbide combined material is widely used at special dimensions such as metallurgy high furnaces.With magnesium A Long material similar be that β-sialon material generally also adopts solid state sintering, metallic reducing nitrogenize synthetic and carbothermal reduction-nitridation is synthetic; The metallic reducing nitrogenize is to be the direct nitrogenizing reaction synthesis method of raw material with aluminum oxide, silica flour and aluminium powder; Same metal is brought into play plasticity and is acted on mutually in moulding and sintering process, improved the performance of material.Its reduction-nitridation is following:
Al+Si+Al
2O
3+N
2→β-SiAlON
The research of advanced ceramics was once once trending towards high-purity one-component ceramic, but because of its limitation on preparation and performance, made it can't satisfy development in Hi-Tech making excessive demands material.Material desirable more, comprehensive, excellent combination property for developing, enlarge the purposes application new with development of advanced ceramics, current research begins to trend towards the research of heterogeneous composite structural ceramic again.Complex phase ceramic can keep the main characteristic of former composition, and obtains the performance that stock blend does not possess through complex effect, can make the performance complement of each component also associated with each other through the material design again, thereby obtain new high-performance.
Summary of the invention
The objective of the invention is to utilize two-way reduction-nitridation original position to synthesize magnesium A Long/β-composite ceramics material, the diphase ceramic material that obtained performance is good.
The characteristics of pottery or refractory materials are high temperature resistant, anti-erosion, HS etc., but it also need have higher heat-shock resistance and toughness.Single-phase magnesium A Long has excellent properties such as intensity height, resistance to slag corrosion are good, good in oxidation resistance, and single-phase β-Sai Long has excellent properties such as good thermal shock, toughness height, and the two all has advantage high temperature resistant, that high high-temp stability is good.The synthetic comparatively condition of strictness that all needs of magnesium A Long and β-Sai Long; Research shows that the synthetic single-phase magnesium A Long of reduction nitridation or β-Sai Long have similar atmosphere mode, through introducing the synthetic diphase ceramic material of silica flour, aluminium powder two-way reduction nitridation original position under appropriate atmosphere, can utilize silica flour; The aluminium powder reaction makes material have the plasticity of metalloid; Thereby improve toughness, improve density, reduce apparent porosity; With making material have intensity height, good toughness, resistance to slag corrosion is good, heat-shock resistance is excellent characteristics, be expected to become new type high temperature structural ceramics of new generation and high performance refractory.
A kind of original position is synthesized the method for magnesium A Long/β-composite ceramics material, it is characterized in that using the mass percent of raw material to be: silica flour, 2～30%; Aluminium powder, 2～10%; Aluminum oxide, 57.5～85%; Natural manganese dioxide, 3～15%.The percentage composition of magnesium A Long is 40～95% in magnesium A Long/β-composite ceramics material, and the percentage composition of β-Sai Long is 5～60%.Use high temperature reduction nitrification established law one-step synthesis, the synthesis technique flow process is as shown in Figure 1.
(1) according to prescription difference weighing design proportion raw material;
(2) with load weighted prepared using water dilution (raw material powder and water weight ratio=1: 3～6), diameter be the agate ball (at the bottom of the cloth canful) of 1cm as ball-milling medium, after the raw material of dilution and agate ball put into the nylon jar and seal, ball milling 6h in planetary ball mill;
(3) mixed raw materials is put into 100 ℃ in loft drier, 10h drying;
(4) the exsiccant raw material is added a spot of carboxymethylcellulose sodium solution (0.5mL/10g), mechanical pressing under the pressure of 40MPa;
(5) feed ordinary nitrogen (purity is 99.5%), nitrogen pressure is 0.1Mpa, and temperature is 1500-1800 ℃, and soaking time is a sintering appearance base under the condition of 2-8h; Synthesize magnesium A Long/β-composite ceramics material.
The present invention is that the synthetic magnesium A Long/β of reductive agent reduction nitridation-composite ceramics material has the advantage of single-phase magnesium A Long material or β-sialon material respectively with silicon, aluminium; Have intensity height, good toughness, resistance to slag corrosion is good, heat-shock resistance is excellent characteristics, be expected to become new type high temperature structural ceramics of new generation and high performance refractory.
Description of drawings
Fig. 1 is a synthesis process flow diagram of the present invention
Fig. 2 and Fig. 3 are the X ray diffracting spectrum of synthetic magnesium A Long/β-composite ceramics material
Fig. 4 and Fig. 5 are the SEM photo of synthetic magnesium A Long/β-composite ceramics material
Embodiment
Embodiment 1,
The silica flour that raw material is, aluminium powder, Natural manganese dioxide and aluminum oxide, its proportioning raw materials (sample 1) as shown in table 1.Normal pressure following feeding ordinary nitrogen (purity is 99.5%) is incubated 4h under 1650 ℃ of temperature synthetic.
Embodiment 2,
The silica flour that raw material is, aluminium powder, Natural manganese dioxide and aluminum oxide, its proportioning raw materials (sample 2) as shown in table 2.Normal pressure following feeding ordinary nitrogen (purity is 99.5%) is incubated 5h under 1600 ℃ of temperature synthetic.Synthetic sample 2 is carried out X-ray diffraction analysis; The result is as shown in Figure 2, X-ray diffraction analysis show the staple of the synthetic sample of experiment be magnesium A Long, β-Sai Long and aluminum oxide mutually, folding strength is 52MPa; The content of magnesium A Long phase is about 46% in the diphase ceramic material; The content of β-Sai Long phase is about 42%, and the aluminum oxide phase content is about 12%, and there are good corresponding relationship in synthetic phase composite and proportioning raw materials.Fig. 4 is the SEM fracture photo of sample 2, can find out that the crystal grain of synthetic sample is grown better, and the β of column-Sai Long content is higher, grows in the space mostly.
Embodiment 3,
The silica flour that raw material is, aluminium powder, Natural manganese dioxide and aluminum oxide, its proportioning raw materials (sample 3) as shown in table 3.Normal pressure following feeding ordinary nitrogen (purity is 99.5%) is incubated 2h under 1700 ℃ of temperature synthetic.
Embodiment 4,
The silica flour that raw material is, aluminium powder, Natural manganese dioxide and aluminum oxide, its proportioning raw materials (sample 4) as shown in table 4.Normal pressure following feeding ordinary nitrogen (purity is 99.5%) is incubated 5h under 1600 ℃ of temperature synthetic.Synthetic sample 4 is carried out X-ray diffraction analysis; The result is as shown in Figure 3; X-ray diffraction analysis show the staple of the synthetic sample of experiment be magnesium A Long, β-Sai Long and aluminum oxide mutually, the content of magnesium A Long phase is about 73% in the diphase ceramic material, the content of β-Sai Long phase is about 19%; The content of aluminum oxide phase is about 9%, and there is good corresponding relationship in the same and proportioning raw materials of synthetic phase composite.Fig. 5 is the SEM fracture photo of sample 4, can find out that there is the significantly brilliant fracture in edge in its fracture mode, and have transgranular fracture; Its folding strength is determined as 85MPa, and is obviously higher than sample 1, has mechanical property preferably; The void content of comparing sample 4 with sample 2 is obviously lower, and grain-size is big and the intergranule combination is comparatively fine and close, the staggered growth of the β-Sai Long of oarse-grained magnesium A Long crystal and column; Not only help improving the intensity of material, also help the toughness that improves material.
Embodiment 5,
The silica flour that raw material is, aluminium powder, Natural manganese dioxide and aluminum oxide, its proportioning raw materials (sample 5) as shown in table 5.Normal pressure following feeding ordinary nitrogen (purity is 99.5%) is incubated 4h under 1650 ℃ of temperature synthetic.
Table 1 reduction nitridation reaction synthesizes the proportioning raw materials of magnesium A Long/β-composite ceramics material
Table 2 reduction nitridation reaction synthesizes the proportioning raw materials of magnesium A Long/β-composite ceramics material
Table 3 reduction nitridation reaction synthesizes the proportioning raw materials of magnesium A Long/β-composite ceramics material
Table 4 reduction nitridation reaction synthesizes the proportioning raw materials of magnesium A Long/β-composite ceramics material
Table 5 reduction nitridation reaction synthesizes the proportioning raw materials of magnesium A Long/β-composite ceramics material
Claims (1)
1. the method for the synthetic magnesium A Long/β of original position-composite ceramics material is characterized in that using the mass percent of raw material to be: silica flour, 2～30%; Aluminium powder, 2～10%; Aluminum oxide, 57.5～85%; Natural manganese dioxide, 3～15%; The percentage composition of magnesium A Long is 40～95% in magnesium A Long/β-composite ceramics material, and the percentage composition of β-Sai Long is 5～60%; Adopt high temperature reduction nitrification established law one-step synthesis, the synthesis technique flow process is:
(1) according to prescription difference weighing design proportion raw material;
(2) with the dilution of load weighted prepared using water, raw material powder and water weight ratio=1: 3～6, with agate ball as ball-milling medium, after the raw material that dilutes and agate ball put into the nylon jar and seal, ball milling 6h in planetary ball mill;
(3) mixed raw materials is put into 100 ℃ in loft drier, 10h drying;
(4) the exsiccant raw material is added the carboxymethylcellulose sodium solution of 0.5mL/10g, mechanical pressing under the pressure of 40MPa;
(5) feeding purity is 99.5% ordinary nitrogen, and nitrogen pressure is 0.1MPa, and temperature is 1500-1800 ℃, and soaking time is a sintering appearance base under the condition of 2-8h; Synthesize magnesium A Long/β-composite ceramics material.
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|---|---|---|---|
| CN2009100760600A CN101456740B (en) | 2009-01-04 | 2009-01-04 | Method for in-situ synthesis of MgAlON/beta-sialon composite ceramic material |
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| CN2009100760600A CN101456740B (en) | 2009-01-04 | 2009-01-04 | Method for in-situ synthesis of MgAlON/beta-sialon composite ceramic material |
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| CN111875398B (en) * | 2020-08-13 | 2022-02-15 | 中钢集团洛阳耐火材料研究院有限公司 | Nitride-silicon carbide-magnesia-alumina spinel complex phase refractory material product and preparation method thereof |
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| Title |
|---|
| 罗星源 等.新一代β-Sialon复合MgAlON耐火材料抗渣及抗钢水性能.《耐火材料》.2000,第34卷(第3期),147-150. * |
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