CN105016735A - SiC ceramic preparation method - Google Patents
SiC ceramic preparation method Download PDFInfo
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- CN105016735A CN105016735A CN201510436636.5A CN201510436636A CN105016735A CN 105016735 A CN105016735 A CN 105016735A CN 201510436636 A CN201510436636 A CN 201510436636A CN 105016735 A CN105016735 A CN 105016735A
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Abstract
The present invention discloses a SiC ceramic preparation method including raw material selection ratio, mixing, compression moulding forming, and firing for production of SiC ceramic. The preparation method is simple in preparation process, and low in cost of raw materials, and the resulting SiC ceramic has good heat resistance, acid and alkaline corrosion resistance, high mechanical strength, good thermal shock resistance, high temperature stability and other advantages, and is widely used in refractories.
Description
Technical field
The present invention relates to a kind of preparation method of SiC ceramic, belong to technical field of ceramic material.
Background technology
Rotary kiln is in operational process, refractory materials can be subject to various thermal stresses, mechanical stress effect (as between fragment of brick because of the extruding that the extruding of the limited generation of thermal expansion, simplified distortion produce brick, and brick and kiln simplified between produce friction) be damaged.The chemical reaction that kiln lining hot end surface occurs can cause the change of refractory materials physicals, especially reacts the change of position thermal expansivity, exacerbates the generation of pinch spalling and thermal spalling.Refractory materials in present stage rotary kiln mainly adopts indefinite form refractory castable, it be a kind of without calcining, stir without being shaped, adding water after there is the refractory materials of better mobility.But it easily peels off, thermal shock resistance is poor, and alkaline resistance properties is better, and acid resistance is poor.
Summary of the invention
For solving the deficiencies in the prior art, the object of the present invention is to provide the preparation method of the SiC ceramic that a kind of preparation method is simple, with low cost, performance is good.
In order to realize above-mentioned target, the present invention adopts following technical scheme:
A preparation method for SiC ceramic, is characterized in that, comprises the following steps:
(1) batch mixing: described raw material comprises following component, and the mass percentage of each component is respectively: SiC:60-70wt%; Mullite: 1-15wt%; Trichroite: 3-8 wt%; Al
2o
3: 5-15wt%; SiO
2: 0-10wt%; MgO:0-5wt%, first SiC is joined in polyvinyl alcohol water solution and mix, described SiC and the mass ratio of polyvinyl alcohol water solution are (4-16): 1, and then add trichroite, mullite mixing according to the mass percentage of each component, finally add Al
2o
3, SiO
2and MgO, again mix, obtain mixed powder;
(2) compression molding: step (1) mixed powder is carried out single way stempressing, is shaped to base substrate;
(3) burn till: after the body drying that step (2) is suppressed, sinter under the air atmosphere of 1200-1400 DEG C, obtain SiC ceramic.
Further, the particle diameter of above-mentioned SiC comprises coarse grain footpath, middle particle diameter and fine grain size, and described coarse grain footpath is 250 ~ 500 μm, content is 30%-60%, and middle particle diameter is 100 ~ 250 μm, and content is 10%-40%, fine grain size is 5 ~ 100 μm, and content is 30%-60%, and the content of SiC is greater than 95%.
The particle diameter of described mullite is 5-250 μm.The particle diameter of trichroite is 5-250 μm.Described Al
2o
3particle diameter be 5-70 μm, and Al
2o
3content be greater than 99.9%, and Al
2o
3for α-Al
2o
3.Described SiO
2particle diameter be 5-100 μm, and SiO
2content be greater than 99.9%.The particle diameter of described MgO is 5-70 μm, and the content of MgO is greater than 99.9%.
Further, in the batch mixing process of step (1), all adopt ball mill mixing, and be ball-milling medium with SiC, rotating speed during ball mill mixing need at 50-100 rev/min, and Ball-milling Time is 10-12h, and material ball ratio is 1:(1-3).
Beneficial effect of the present invention is: preparation method preparation technology of the present invention is simple, raw materials cost is low, and the SiC ceramic obtained has resistance toheat is good, acid-alkali-corrosive-resisting performance is good, physical strength is high, thermal shock resistance is good, high-temperature stability is good advantage, be widely used in refractory materials.
Embodiment
Below in conjunction with specific embodiment, concrete introduction is done to the present invention.
Should be understood that these embodiments just in order to demonstrate the invention, but not limit the scope of the invention by any way.Below in an example, the various process do not described in detail and method are ordinary methods as known in the art.Source, the trade(brand)name of component used and be necessary to list its moiety person, all indicate when occurring first, identical reagent used if no special instructions thereafter, all identical with the content indicated first.
In following examples, the particle diameter of described SiC comprises coarse grain footpath, middle particle diameter and fine grain size, and described coarse grain footpath is 250 ~ 500 μm, and middle particle diameter is 100 ~ 250 μm, and fine grain size is 5 ~ 100 μm, and the content of SiC is greater than 95%.And the particle diameter of described mullite is 5-250 μm.The particle diameter of trichroite is 5-250 μm.Described Al
2o
3particle diameter be 5-70 μm, and Al
2o
3for α-Al
2o
3.Described SiO
2particle diameter be the particle diameter of 5-100 μm, MgO be 5-70 μm, and the content of raw material SiC is greater than 95%, Al
2o
3, SiO
2, MgO content be all greater than 99.9%.
embodiment 1:
Getting mass ratio is: the SiC of 60:20:4:8:6:2, mullite, trichroite, Al
2o
3, SiO
2, MgO, in SiC, the ratio of carse, medium and small particle diameter is: 55:10:35, first SiC is joined in polyvinyl alcohol water solution and mix, described SiC and the mass ratio of polyvinyl alcohol water solution are 10:1, and then add trichroite, mullite mixing according to the mass percentage of each component, finally add Al
2o
3, SiO
2and MgO, again mix, obtain mixed powder, in batch mixing process, all adopt ball mill mixing, and be ball-milling medium with SiC, rotating speed during ball mill mixing need at 80 revs/min, and Ball-milling Time is 10h, and material ball ratio is 1:1; Then single way stempressing is carried out to mixed powder, be shaped to base substrate, then by after the body drying that suppresses, sinter under the air atmosphere of 1200 DEG C, obtain SiC ceramic sample.After measured, the bending strength of SiC ceramic sample is 32MPa, and ultimate compression strength is 96MPa, and volume density is 2.7g/cm
3, thermal expansivity is at 3-8*10
-6k
-1between, be placed on by goods in the high-temperature cabinet of 800 DEG C and be incubated 30 minutes, then put into rapidly the cold water of 25 DEG C, so circulate, do not ftracture for 42 times, be placed on by sample in the sodium hydroxide solution of 1wt%, 50 DEG C of standing 72h, the weightlessness of porous ceramics is 0.2%.
embodiment 2:
Getting mass ratio is: the SiC of 60:20:4:8:6:2, mullite, trichroite, Al
2o
3, SiO
2, MgO, in SiC, the ratio of carse, medium and small particle diameter is: 55:10:35, first SiC is joined in polyvinyl alcohol water solution and mix, described SiC and the mass ratio of polyvinyl alcohol water solution are 10:1, and then add trichroite, mullite mixing according to the mass percentage of each component, finally add Al
2o
3, SiO
2and MgO, again mix, obtain mixed powder, in batch mixing process, all adopt ball mill mixing, and be ball-milling medium with SiC, rotating speed during ball mill mixing need at 100 revs/min, and Ball-milling Time is 12h, and material ball ratio is 1:1; Then single way stempressing is carried out to mixed powder, be shaped to base substrate, then by after the body drying that suppresses, sinter under the air atmosphere of 1300 DEG C, obtain SiC ceramic sample.After measured, the bending strength of SiC ceramic sample is 28MPa, and ultimate compression strength is 86MPa, and volume density is 2.5g/cm
3, thermal expansivity exists, 3-8*10
-6k
-1between, goods are placed on the soak 30 minutes at 800 DEG C, then put into rapidly the cold water of 25 DEG C, so circulate, do not ftracture for 36 times, be placed on by sample in the sodium hydroxide solution of 1wt%, 50 DEG C of standing 72h, the weightlessness of porous ceramics is 0.4%.
embodiment 3:
Getting mass ratio is: the SiC of 60:20:4:8:6:2, mullite, trichroite, Al
2o
3, SiO
2, MgO, in SiC, the ratio of carse, medium and small particle diameter is: 55:10:35, first SiC is joined in polyvinyl alcohol water solution and mix, described SiC and the mass ratio of polyvinyl alcohol water solution are 10:1, and then add trichroite, mullite mixing according to the mass percentage of each component, finally add Al
2o
3, SiO
2and MgO, again mix, obtain mixed powder, in batch mixing process, all adopt ball mill mixing, and be ball-milling medium with SiC, rotating speed during ball mill mixing need at 80 revs/min, and Ball-milling Time is 10h, and material ball ratio is 1:2; Then single way stempressing is carried out to mixed powder, be shaped to base substrate, then by after the body drying that suppresses, sinter under the air atmosphere of 1400 DEG C, obtain SiC ceramic sample.After measured, the bending strength of SiC ceramic sample is 28MPa, and ultimate compression strength is 86MPa, and volume density is 2.5g/cm
3, thermal expansivity exists, 3-8*10
-6k
-1between, goods are placed on the soak 30 minutes at 800 DEG C, then put into rapidly the cold water of 25 DEG C, so circulate, do not ftracture for 36 times, be placed on by sample in the sodium hydroxide solution of 1wt%, 50 DEG C of standing 72h, the weightlessness of porous ceramics is 0.4%.
embodiment 4:
Getting mass ratio is: the SiC of 70:15:3:6:4:2, mullite, trichroite, Al
2o
3, SiO
2, MgO, in SiC, the ratio of carse, medium and small particle diameter is: 55:10:35, first SiC is joined in polyvinyl alcohol water solution and mix, described SiC and the mass ratio of polyvinyl alcohol water solution are 10:1, and then add trichroite, mullite mixing according to the mass percentage of each component, finally add Al
2o
3, SiO
2and MgO, again mix, obtain mixed powder, in batch mixing process, all adopt ball mill mixing, and be ball-milling medium with SiC, rotating speed during ball mill mixing need at 100 revs/min, and Ball-milling Time is 10h, and material ball ratio is 1:1; Then single way stempressing is carried out to mixed powder, be shaped to base substrate, then by after the body drying that suppresses, sinter under the air atmosphere of 1300 DEG C, obtain SiC ceramic sample.After measured, the bending strength of SiC ceramic sample is 36MPa, and ultimate compression strength is 112MPa, and volume density is 2.85g/cm
3, thermal expansivity exists, 3-8*10
-6k
-1between, goods are placed on the soak 30 minutes at 800 DEG C, then put into rapidly the cold water of 25 DEG C, so circulate, do not ftracture for 48 times, be placed on by sample in the sodium hydroxide solution of 1wt%, 50 DEG C of standing 72h, the weightlessness of porous ceramics is 0.1%.
embodiment 5:
Getting mass ratio is: the SiC of 70:15:3:6:4:2, mullite, trichroite, Al
2o
3, SiO
2, MgO, in SiC, the ratio of carse, medium and small particle diameter is: 55:10:35, first SiC is joined in polyvinyl alcohol water solution and mix, described SiC and the mass ratio of polyvinyl alcohol water solution are 8:1, and then add trichroite, mullite mixing according to the mass percentage of each component, finally add Al
2o
3, SiO
2and MgO, again mix, obtain mixed powder, in batch mixing process, all adopt ball mill mixing, and be ball-milling medium with SiC, rotating speed during ball mill mixing need at 100 revs/min, and Ball-milling Time is 10h, and material ball ratio is 1:1; Then single way stempressing is carried out to mixed powder, be shaped to base substrate, then by after the body drying that suppresses, sinter under the air atmosphere of 1300 DEG C, obtain SiC ceramic sample.After measured, the bending strength of SiC ceramic sample is 35MPa, and ultimate compression strength is 105MPa, and volume density is 2.75g/cm
3, thermal expansivity exists, 3-8*10
-6k
-1between, goods are placed on the soak 30 minutes at 800 DEG C, then put into rapidly the cold water of 25 DEG C, so circulate, do not ftracture for 45 times, be placed on by sample in the sodium hydroxide solution of 1wt%, 50 DEG C of standing 72h, the weightlessness of porous ceramics is 0.6%.
embodiment 6:
Getting mass ratio is: the SiC of 70:15:4:5:3:3, mullite, trichroite, Al
2o
3, SiO
2, MgO, in SiC, the ratio of carse, medium and small particle diameter is: 55:10:35, first SiC is joined in polyvinyl alcohol water solution and mix, described SiC and the mass ratio of polyvinyl alcohol water solution are 8:1, and then add trichroite, mullite mixing according to the mass percentage of each component, finally add Al
2o
3, SiO
2and MgO, again mix, obtain mixed powder, in batch mixing process, all adopt ball mill mixing, and be ball-milling medium with SiC, rotating speed during ball mill mixing need at 100 revs/min, and Ball-milling Time is 10h, and material ball ratio is 1:1; Then single way stempressing is carried out to mixed powder, be shaped to base substrate, then by after the body drying that suppresses, sinter under the air atmosphere of 1400 DEG C, obtain SiC ceramic sample.After measured, the bending strength of SiC ceramic sample is 25MPa, and ultimate compression strength is 81MPa, and volume density is 2.4g/cm
3, thermal expansivity exists, 3-8*10
-6k
-1between, goods are placed on the soak 30 minutes at 800 DEG C, then put into rapidly the cold water of 25 DEG C, so circulate, do not ftracture for 32 times, be placed on by sample in the sodium hydroxide solution of 1wt%, 50 DEG C of standing 72h, the weightlessness of porous ceramics is 1.2%.
More than show and describe ultimate principle of the present invention, principal character and advantage.The technician of the industry should understand, and above-described embodiment does not limit the present invention in any form, the technical scheme that the mode that all employings are equal to replacement or equivalent transformation obtains, and all drops in protection scope of the present invention.
Claims (9)
1. a preparation method for SiC ceramic, is characterized in that, comprises the following steps:
(1) batch mixing: described raw material comprises following component, and the mass percentage of each component is respectively: SiC:60-70wt%; Mullite: 1-15wt%; Trichroite: 3-8 wt%; Al
2o
3: 5-15wt%; SiO
2: 0-10wt%; MgO:0-5wt%, first SiC is joined in polyvinyl alcohol water solution and mix, described SiC and the mass ratio of polyvinyl alcohol water solution are (4-16): 1, and then add trichroite, mullite mixing according to the mass percentage of each component, finally add Al
2o
3, SiO
2and MgO, again mix, obtain mixed powder;
(2) compression molding: step (1) mixed powder is carried out single way stempressing, is shaped to base substrate;
(3) burn till: after the body drying that step (2) is suppressed, sinter under the air atmosphere of 1200-1400 DEG C, obtain SiC ceramic.
2. the preparation method of a kind of SiC ceramic according to claim 1, it is characterized in that, the particle diameter of described SiC comprises coarse grain footpath, middle particle diameter and fine grain size, described coarse grain footpath is 250 ~ 500 μm, and content is 30%-60%, and middle particle diameter is 100 ~ 250 μm, content is 10%-40%, fine grain size is 5 ~ 100 μm, and content is 30%-60%, and the content of SiC is greater than 95%.
3. the preparation method of a kind of SiC ceramic according to claim 1, is characterized in that, the particle diameter of described mullite is 5-250 μm.
4. the preparation method of a kind of SiC ceramic according to claim 1, is characterized in that, the particle diameter of described trichroite is 5-250 μm.
5. the preparation method of a kind of SiC ceramic according to claim 1, is characterized in that, described Al
2o
3particle diameter be 5-70 μm, and Al
2o
3content be greater than 99.9%.
6. the preparation method of a kind of SiC ceramic according to claim 1 or 5, is characterized in that, described Al
2o
3for α-Al
2o
3.
7. the preparation method of a kind of SiC ceramic according to claim 1, is characterized in that, described SiO
2particle diameter be 5-100 μm, and SiO
2content be greater than 99.9%.
8. the preparation method of a kind of SiC ceramic according to claim 1, is characterized in that, the particle diameter of described MgO is 5-70 μm, and the content of MgO is greater than 99.9%.
9. the preparation method of a kind of SiC ceramic according to claim 1, it is characterized in that, in the batch mixing process of step (1), all adopt ball mill mixing, and be ball-milling medium with SiC, rotating speed during ball mill mixing need at 50-100 rev/min, and Ball-milling Time is 10-12h, and material ball ratio is 1:(1-3).
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1621125A (en) * | 2004-10-13 | 2005-06-01 | 中国科学院上海硅酸盐研究所 | Low temperature sintering reticular silicon carbide ceramic filtering device with high fire resisting level and its preparation method |
| CN102775163A (en) * | 2012-07-25 | 2012-11-14 | 江苏省陶瓷研究所有限公司 | Silicon carbide-cordierite composite ceramic kiln furniture and preparation method thereof |
| CN103553650A (en) * | 2013-10-11 | 2014-02-05 | 武汉科技大学 | Light mullite-silicon carbide refractory material and preparation method thereof |
| CN104072142A (en) * | 2014-06-30 | 2014-10-01 | 江苏新光环保工程有限公司 | Preparation method of oxide combined SiC porous ceramic |
| CN104446625A (en) * | 2014-11-28 | 2015-03-25 | 中国科学技术大学先进技术研究院 | High-porosity porous ceramic and preparation method thereof |
-
2015
- 2015-07-23 CN CN201510436636.5A patent/CN105016735A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1621125A (en) * | 2004-10-13 | 2005-06-01 | 中国科学院上海硅酸盐研究所 | Low temperature sintering reticular silicon carbide ceramic filtering device with high fire resisting level and its preparation method |
| CN102775163A (en) * | 2012-07-25 | 2012-11-14 | 江苏省陶瓷研究所有限公司 | Silicon carbide-cordierite composite ceramic kiln furniture and preparation method thereof |
| CN103553650A (en) * | 2013-10-11 | 2014-02-05 | 武汉科技大学 | Light mullite-silicon carbide refractory material and preparation method thereof |
| CN104072142A (en) * | 2014-06-30 | 2014-10-01 | 江苏新光环保工程有限公司 | Preparation method of oxide combined SiC porous ceramic |
| CN104446625A (en) * | 2014-11-28 | 2015-03-25 | 中国科学技术大学先进技术研究院 | High-porosity porous ceramic and preparation method thereof |
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Application publication date: 20151104 |
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