CN102086125A - Method for synthesizing mullite whisker toughened corundum-mullite in situ - Google Patents
Method for synthesizing mullite whisker toughened corundum-mullite in situ Download PDFInfo
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- CN102086125A CN102086125A CN201010553262.2A CN201010553262A CN102086125A CN 102086125 A CN102086125 A CN 102086125A CN 201010553262 A CN201010553262 A CN 201010553262A CN 102086125 A CN102086125 A CN 102086125A
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- 229910052863 mullite Inorganic materials 0.000 title claims abstract description 30
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 238000000034 method Methods 0.000 title claims abstract description 17
- 230000002194 synthesizing effect Effects 0.000 title claims abstract description 11
- 238000011065 in-situ storage Methods 0.000 title abstract description 6
- 239000002994 raw material Substances 0.000 claims abstract description 21
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 claims abstract description 18
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 14
- IRPGOXJVTQTAAN-UHFFFAOYSA-N 2,2,3,3,3-pentafluoropropanal Chemical compound FC(F)(F)C(F)(F)C=O IRPGOXJVTQTAAN-UHFFFAOYSA-N 0.000 claims abstract description 9
- KLZUFWVZNOTSEM-UHFFFAOYSA-K Aluminum fluoride Inorganic materials F[Al](F)F KLZUFWVZNOTSEM-UHFFFAOYSA-K 0.000 claims abstract description 9
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims abstract description 7
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 7
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 6
- 230000032683 aging Effects 0.000 claims abstract description 5
- 238000000498 ball milling Methods 0.000 claims abstract description 3
- 239000011819 refractory material Substances 0.000 claims description 35
- 239000000203 mixture Substances 0.000 claims description 15
- 239000000843 powder Substances 0.000 claims description 15
- 239000013078 crystal Substances 0.000 claims description 11
- 229910021502 aluminium hydroxide Inorganic materials 0.000 claims description 6
- 229960001866 silicon dioxide Drugs 0.000 claims description 6
- 239000011230 binding agent Substances 0.000 claims description 4
- 229910052799 carbon Inorganic materials 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 4
- 238000009413 insulation Methods 0.000 claims description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims 1
- 229910002804 graphite Inorganic materials 0.000 claims 1
- 239000010439 graphite Substances 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 9
- 230000000694 effects Effects 0.000 abstract description 7
- 238000010438 heat treatment Methods 0.000 abstract description 5
- 239000003054 catalyst Substances 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 description 9
- 230000003014 reinforcing effect Effects 0.000 description 9
- 238000005452 bending Methods 0.000 description 8
- 230000007246 mechanism Effects 0.000 description 8
- 239000000835 fiber Substances 0.000 description 7
- 230000008569 process Effects 0.000 description 7
- 230000008901 benefit Effects 0.000 description 3
- 239000000306 component Substances 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000010310 metallurgical process Methods 0.000 description 2
- 230000035939 shock Effects 0.000 description 2
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 2
- 229910010271 silicon carbide Inorganic materials 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000006557 surface reaction Methods 0.000 description 2
- 229910016569 AlF 3 Inorganic materials 0.000 description 1
- 208000037656 Respiratory Sounds Diseases 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 206010042209 Stress Diseases 0.000 description 1
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 1
- 239000011358 absorbing material Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000000748 compression moulding Methods 0.000 description 1
- 239000008358 core component Substances 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 239000010431 corundum Substances 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 230000002542 deteriorative effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 230000035882 stress Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000003245 working effect Effects 0.000 description 1
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Abstract
The invention provides a method for synthesizing mullite whisker toughened corundum-mullite in situ, which comprises the following steps of: proportioning industrial aluminum hydroxide and silicon dioxide serving as raw materials and aluminum fluoride and vanadium pentoxide serving as catalysts, performing ball milling by using ethanol as a medium, adding polyvinyl alcohol, mixing and ageing; tabletting; heating to the temperature of between 900 and 1,000 DEG C at the heating rate of 3 to 5 DEG C/min from room temperature, and preserving heat for 1 to 2 hours; heating to the temperature of between 1,350 and 1,450 DEG C at the heating rate of 5 to 10 DEG C/min, and preserving heat for 2 to 3 hours; and cooling to obtain the required corundum-mullite fireproof material. By the method, the fireproof material is toughened in a mode of synthesizing mullite whiskers in situ, and the whiskers are uniformly distributed and have high length-to-diameter ratio and a good toughening effect.
Description
Technical field
The present invention relates to the method for the crystal whisker toughened corundum-mullite refractory materials of a kind of original position mullite synthesizing, this refractory materials is mainly used in microwave metallurgical pyroreaction device, the invention belongs to the metallurgical material preparing technical field.
Background technology
Compare with known metallurgical method, microwave metallurgical has that selectivity adds thermal material, temperature rise rate is fast, heating efficiency is high, chemical reaction is had katalysis, is easy to significant advantage such as control automatically, so microwave metallurgical is expected to one of effective way that becomes the metallurgical industry cleaner production.Core component as the microwave metallurgical reaction unit, microwave metallurgical with refractory materials except that should possessing the basic physical and chemical performance that common refractory has, also should satisfy following particular requirement: 1. heat resisting temperature height, can stand various structural stresss, physics, chemistry and mechanical effect etc. being higher than under 1000 ℃ the temperature; 2. microwave penetrating is strong, specific absorption is low, and promptly refractory materials should have less specific inductivity and low dielectric loss; 3. good heat-shock resistance and opposing thermal shocking ability can stand heating-cooling process rapidly repeatedly and cracking destruction not occur.
Above-mentioned complicated harsh requirement makes the refractory materials of general one-component be difficult to satisfy the service requirements of microwave metallurgical process, thereby the refractory materials that needs to have different advantages usually carries out compound and then develops the plural components refractory materials of excellent performance.The refractory body that is hopeful most at present to use as microwave metallurgical pyroreaction device is a corundum-mullite base refractory materials, it has the two excellent properties of corundum and mullite simultaneously concurrently, be a kind of high temperature resistant, anti-erosion, anti-ly wash away, physical strength height, wave penetrate capability high-quality refractory material preferably.But the greatest problem that this refractory materials exists cracking destruction occurs under the serious thermal shocking effect exactly easily in the microwave metallurgical process, heat-shock resistance is poor, work-ing life is short.Therefore, adopt suitable Toughening Measures to improve toughness, the heat-shock resistance of refractory materials and the ability of resisting thermal shocking becomes the key issue that present solution microwave metallurgical uses with refractory materials.
Theoretically, known ceramic toughening mechanism as phase toughness, particle malleableize, microstructure malleableize, plus fiber or whisker malleableize etc., all can be used for corundum-mullite is carried out patent.But consider the singularity of microwave metallurgical, in the selection of Toughening Mechanism, also should be taken into account the influence of toughening mechanisms, thereby the selection of toughness reinforcing mode has been produced considerable restraint the refractory materials wave penetrate capability with the refractory materials environment for use.For example: 1. for phase toughness, because the partially stabilized ZrO that adds
2Be a kind of suction ripple material when high temperature, its adding must improve the specific inductivity and the dielectric loss of refractory materials, causes the decline of wave energy power; 2. for the microstructure malleableize, owing to size, the form of crystal grain, pore and tiny crack, be distributed in and can change after long-time high temperature uses, thereby toughening effect can deterioration occur with prolonging duration of service; 3. for the particle malleableize, toughness reinforcing particle such as zirconium white, silicon carbide etc. commonly used at high temperature are absorbing material, thereby have limited the application of this toughening mechanisms; 4. and in plus fiber (or whisker) malleableize process, the too high sintering temperature of stupalith will certainly produce deteriorating effect to fiber (or whisker), and make between the fiber and to produce surface reaction and cause strong interface combination, cause the toughening mechanisms such as bridging of the extracting of fiber, crackle to lose efficacy.Adopt superfine powder can reduce the sintering temperature of refractory materials, by prepare the generation that coating can be avoided surface reaction between the fiber at fiber surface, but the direct result of above-mentioned measure is that the cost of product is increased substantially, and makes the preparation technology of refractory materials further complicated.
Aspect mullite crystal whisker in-situ flexible stupalith, also only be confined in present document and the patented technology carry out toughness reinforcing to material systems such as aluminum oxide, Y-TZP and SiC, also very limited to whisker synthesis technique approach, process of growth, toughening effect and Study on Mechanism concrete under this particular surroundings of other materials system, particularly microwave metallurgical.The present invention is by introducing the microwave metallurgical fire resisting material field with the crystal whisker toughened refractory materials mechanism of original position mullite synthesizing, adopt low-cost industrial level raw material original position mullite synthesizing whisker and refractory materials is carried out toughness reinforcing processing, not only preparation technology is simple, cost is low, and the expection toughening effect is remarkable.
Summary of the invention
For solving problems such as prior art cost height, complex process, technical problem to be solved by this invention is: with technical grade Al (OH)
3And SiO
2Be main raw material, add certain quantity of additive AlF
3And V
2O
5, original position synthesizes mullite crystal whisker and realizes the in-situ flexible of microwave metallurgical with the corundum-mullite refractory materials.
In order to achieve the above object, the present invention is achieved through the following technical solutions:
1. used starting material composition of the present invention and mass percent are as follows
The present invention with technical grade aluminium hydroxide and silicon-dioxide as raw material, adopt aluminum fluoride and Vanadium Pentoxide as catalyzer, wherein the quality percentage composition of technical grade aluminium hydroxide is 75.5-85.5%, the quality percentage composition of technical grade silicon-dioxide is 14.5-24.5%, the add-on of aluminum fluoride is the 3-5% of raw material weight, and the add-on of Vanadium Pentoxide is the 3-8% of raw material weight.
2. technological process is as follows
With above-mentioned raw materials and catalyzer is ball-milling medium with ethanol, carries out wet ball grinding, obtains the powder mix, and the granularity of powder is 75-100 μ m, and the 3-5% polyvinyl alcohol (PVA) that this powder is added raw material weight mixes and ageing as binding agent; Carry out compressing tablet afterwards, compressing tablet pressure is 15-30MPa, is pressed into the sheet of 36 * 4 * 3mm; The above-mentioned sample that presses is raised to 900 ℃-1000 ℃ with the temperature rise rate of 3 ℃ of-5 ℃/min from room temperature, behind the insulation 1-2h; Be raised to 1350 ℃-1450 ℃ and be incubated 2-3h with the temperature rise rate of 5 ℃ of-10 ℃/min again; Furnace cooling promptly obtains required corundum-mullite refractory materials afterwards.
Thereby the present invention generates bar-shaped crystal whisker materials by original position in the ceramic post sintering process makes pottery obtain malleableize, and promptly so-called in-situ flexible mechanism is the toughness reinforcing mode of a kind of ideal.The present invention selects original position mullite synthesizing whisker as the toughness reinforcing phase of toughness reinforcing microwave metallurgical with the corundum-mullite refractory materials, because it has identical component with matrix, therefore has good coupling aspect thermal expansivity and the chemical compatibility; In addition, the wave penetrate capability of mullite crystal whisker is better, can the wave penetrate capability of refractory materials not had a negative impact.
Realize original position mullite synthesizing whisker and microwave metallurgical is carried out toughness reinforcing advantage with the corundum-mullite refractory materials being with above-mentioned technology: 1. need not the adding and the complicated dispersion process thereof of expensive whisker, preparation process is simple, cost reduces; 2. the mode by original position mullite synthesizing whisker realizes the toughness reinforcing of refractory materials, and whisker is uniformly dispersed, length-to-diameter ratio height, toughening effect are good.
Description of drawings
Fig. 1 is embodiment 1 technology synthetic refractory materials and whisker morphology figure; Fig. 2 is that embodiment 1 adds 3% AIF
3And V
2O
5For catalyzer with do not add the comparison diagram of the bending resistance degree of catalyst samples; Fig. 3 is embodiment 2 technology synthetic refractory materialss and whisker morphology figure; Fig. 4 is that embodiment 2 adds 3% AIF
3And V
2O
5For catalyzer with do not add the comparison diagram of the bending resistance degree of catalyst samples.
Embodiment
Embodiment 1:
With the quality percentage composition is that 75.5% industrial aluminium hydroxide and quality percentage composition are that 24.5% silicon-dioxide is main raw material, 3% the Vanadium Pentoxide in FLAKES that adds 3% aluminum fluoride of raw material weight and raw material weight is as catalyzer, adopt planetary ball mill to carry out wet ball grinding, the powder that acquisition mixes, granularity 75-100 μ m; The PVA that this powder is added raw material weight 3% mixes and ageing afterwards as binding agent again; Adopt powder compressing machine to be pressed into the sheet of 36 * 4 * 3mm in above-mentioned powder, forming pressure is 15MPa; Afterwards above-mentioned compressing tablet gained sample is raised to 900 ℃ with the temperature rise rate of 3 ℃/min from room temperature, behind the insulation 2h, is raised to 1350 ℃ and be incubated 3h with the temperature rise rate of 5 ℃/min again, furnace cooling promptly obtains the product of wanting afterwards.Scanning electron microscope analysis is the result show, with the good dispersion of above-mentioned technology original position synthetic mullite crystal whisker in refractory material matrix, whisker length is between 30 μ m-40 μ m, and diameter is about about 5 μ m, and the pattern of the synthetic whisker of original position as shown in Figure 1.
Said sample (promptly adding the quality percentage composition and be 3% aluminum fluoride and quality percentage composition and be 3% the Vanadium Pentoxide in FLAKES sample as catalyzer) and its bending strength contrast of sample of not adding catalyzer are as shown in Figure 2.With respect to the sample that does not add catalyzer, to add after the above-mentioned catalyzer, the bending strength of refractory materials has improved 200%, and tension set has improved 60%.With the refractory materials sample that adds above-mentioned content catalyzer and do not add catalyzer be heated to 1000 ℃ be incubated 2 hours after water-cooled rapidly, after above-mentioned 10 thermal shocks circulation, the sample that the bending strength rate of loss of the refractory materials sample behind the interpolation catalyzer is not added catalyzer has relatively reduced 50%.
Embodiment 2:
With the quality percentage composition is that 80.5% industrial aluminium hydroxide and quality percentage composition are that 19.5% silicon-dioxide is main raw material, 8% the Vanadium Pentoxide in FLAKES that adds 5% aluminum fluoride of raw material weight and raw material weight is as catalyzer, adopt planetary ball mill to carry out wet ball grinding, obtain the powder that mixes; The PVA that this powder is added raw material weight 5% mixes and ageing afterwards as binding agent again; Above-mentioned powder is adopted powder compressing machine compression moulding, and forming pressure is 25MPa; Afterwards above-mentioned compressing tablet gained sample is raised to 1000 ℃ with the temperature rise rate of 5 ℃/min from room temperature, after the insulation 1, is raised to 1450 ℃ and be incubated 2h with the temperature rise rate of 8 ℃/min again, furnace cooling promptly obtains the product of wanting afterwards.Scanning electron microscope analysis is the result show, with the good dispersion of above-mentioned technology original position synthetic mullite crystal whisker in refractory material matrix, whisker length is between 30 μ m-40 μ m, and diameter is about about 4 μ m, and the pattern of the synthetic whisker of original position as shown in Figure 3.
Said sample (promptly adding the quality percentage composition and be 5% aluminum fluoride and quality percentage composition and be 8% the Vanadium Pentoxide in FLAKES sample as catalyzer) and its bending strength contrast of sample of not adding catalyzer are as shown in Figure 4.With respect to the sample that does not add catalyzer, to add after the above-mentioned catalyzer, the bending strength of refractory materials has improved 500%, and tension set has improved 70%.With the refractory materials sample that adds above-mentioned content catalyzer and do not add catalyzer be heated to 1000 ℃ be incubated 2 hours after water-cooled rapidly, after above-mentioned 10 thermal shocks circulation, the sample that the bending strength rate of loss of the refractory materials sample behind the interpolation catalyzer is not added catalyzer has relatively reduced 60%.
Claims (3)
1. the method for the crystal whisker toughened corundum-mullite of original position mullite synthesizing is characterized in that: implements according to the following steps,
(1) with technical grade aluminium hydroxide and silicon-dioxide as raw material, adopt aluminum fluoride and Vanadium Pentoxide as catalyzer, wherein the quality percentage composition of technical grade aluminium hydroxide is 75.5%-85.5%, the quality percentage composition of technical grade silicon-dioxide is 14.5%-24.5%, the add-on of aluminum fluoride is the 3%-5% of raw material weight, and the add-on of Vanadium Pentoxide is the 3%-8% of raw material weight;
(2) be ball-milling medium with ethanol with above-mentioned raw materials and catalyzer, carry out wet ball grinding, obtain the powder mix, the polyvinyl alcohol that this powder is added raw material weight 3%-5% mixes and ageing as binding agent; Carry out compressing tablet afterwards, compressing tablet pressure is 15-30MPa; The above-mentioned sample that presses is raised to 900 ℃-1000 ℃ with the temperature rise rate of 3 ℃ of-5 ℃/min from room temperature, behind the insulation 1-2h; Be raised to 1350 ℃-1450 ℃ and be incubated 2-3h with the temperature rise rate of 5 ℃ of-10 ℃/min more afterwards; Furnace cooling promptly obtains required corundum-mullite refractory materials afterwards.
2. method according to claim 1 is characterized in that: the granularity of spheroidal graphite gained powder is 75-100 μ m in the step (2).
3. method according to claim 1 is characterized in that: during compressing tablet, be pressed into the sheet of 36 * 4 * 3mm in the step (2).
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Cited By (14)
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|---|---|---|---|---|
| CN103614808A (en) * | 2013-10-24 | 2014-03-05 | 西安交通大学 | Mullite fiber with villous whisker and preparation method thereof |
| CN104843795A (en) * | 2015-04-30 | 2015-08-19 | 昆明理工大学 | Microwave-assisted method for preparing manganite crystal whiskers |
| CN104876273A (en) * | 2015-04-30 | 2015-09-02 | 昆明理工大学 | Preparation method of manganese oxide whiskers |
| CN105036720A (en) * | 2015-07-28 | 2015-11-11 | 景德镇陶瓷学院 | Preparation method for synthesizing mullite whiskers through adopting borides as additives |
| CN105272288A (en) * | 2015-10-16 | 2016-01-27 | 河南东普热能科技有限公司 | Special thermal-insulation refractory material for microwave high temperature and preparation method of special thermal-insulation refractory material |
| CN106167413A (en) * | 2016-07-06 | 2016-11-30 | 江西省工业陶瓷工程技术研究中心 | A kind of toughness reinforcing 90 aluminium oxide ceramics of On In-situ Synthesis of Mullite Whisker and preparation method |
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| CN103614808A (en) * | 2013-10-24 | 2014-03-05 | 西安交通大学 | Mullite fiber with villous whisker and preparation method thereof |
| CN104843795A (en) * | 2015-04-30 | 2015-08-19 | 昆明理工大学 | Microwave-assisted method for preparing manganite crystal whiskers |
| CN104876273A (en) * | 2015-04-30 | 2015-09-02 | 昆明理工大学 | Preparation method of manganese oxide whiskers |
| CN105036720A (en) * | 2015-07-28 | 2015-11-11 | 景德镇陶瓷学院 | Preparation method for synthesizing mullite whiskers through adopting borides as additives |
| CN105036720B (en) * | 2015-07-28 | 2017-03-08 | 景德镇陶瓷大学 | A kind of preparation method by the use of boride as additive mullite synthesizing whisker |
| CN105272288A (en) * | 2015-10-16 | 2016-01-27 | 河南东普热能科技有限公司 | Special thermal-insulation refractory material for microwave high temperature and preparation method of special thermal-insulation refractory material |
| CN106167413B (en) * | 2016-07-06 | 2018-09-28 | 江西省工业陶瓷工程技术研究中心 | A kind of 90 aluminium oxide ceramics of On In-situ Synthesis of Mullite Whisker toughening and preparation method |
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Application publication date: 20110608 |