CN105152653A - Anticorrosion silicon carbide shelf plate and preparation method thereof - Google Patents
Anticorrosion silicon carbide shelf plate and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to an anticorrosion silicon carbide shelf plate and a preparation method thereof, wherein the anticorrosion silicon carbide shelf plate comprises the following raw materials by mass: silicon carbide particles, silicon carbide coarse powder, silicon carbide fine powder, silicon carbide micro-powder, graphene, a composite antioxidant, a composite binding agent, molybdenum disulfide and a lubricating grease. According to the present invention, the product has characteristics of excellent thermal shock resistance, strong anti-oxidation property, strong slag erosion resistance, strong alkali metal erosion resistance, excellent erosion resistance, excellent thermal insulation and good high temperature volume stability; and the highly uniform dispersion inside the shelf plate can be achieved, the sintering can be promoted, the shelf plate can have the uniform structure, and the strength and the thermal shock resistance of the product can be improved.
Description
Technical field
The present invention relates to a kind of high strength, heat conductivity is good, thermal shock resistance is excellent anticorrosive silicon carbide deck and preparation method thereof.
Background technology
Silicon carbide substrate owing to having the high-temperature behavior of good chemical stability, excellent wear resistance and excellence, therefore is that the refractory slab of matrix have also been obtained and uses widely with silicon carbide, and expanding with heat and contract with cold in silicon carbide deck use procedure, easily cause fracture or crack.
There is following defect in silicon carbide deck: 1) because volume density is inadequate, void content is bigger than normal in sintering procedure, often easily forms minimum eutectic and cause sticky porcelain and surperficial color spot; 2) high temperature break resistant intensity is not high, and under comparatively high temps, larger load condition, refractory slab degree of deformation is large, and the burning both having affected product is made, and substantially reduces again the work-ing life of refractory slab; 3) because heat-shock resistance and high temperature toughness are inadequate, therefore burning till fast, in the kiln of rapid heat cycle, refractory slab easily in break, especially at shrinkage joint position cracking, or the fracture of arm of angle portion.
Geim and Novoselov of Man Chesidun university of Britain in 2004 obtains self-existent two-dimensional graphene (Gra-phene by tape stripping high starch breeding, GN), since crystal, Graphene has become one of extremely concerned study hotspot of material science.In fact Graphene is exactly the graphite of monoatomic layer, and it has unique two-dirnentional structure and excellent mechanics, thermodynamics, optics and electric property.
Graphene is at present the thinnest is in the world the hardest nano material also, and it is almost completely transparent, to the light absorbing 2.3%, thermal conductivity up to 5300W/mk, higher than carbon nanotube and diamond.Graphene is a kind of novel material of the individual layer sheet structure be made up of carbon atom, has intensity high, and specific surface area is large, high chemical reactivity, the feature of high fillibility.
Chinese patent publication No. CN101928117A, date of publication on December 29th, 2010, name is called cast silicon carbide, the main raw material of this application case is black silicon carbide crystal grain, bisphenol A type epoxy resin and additive, through the mixing of vacuum companion heat, vacuum casting, Procuring, the demoulding, solidification, workpiece machining.Its weak point is, because volume density is inadequate, void content is bigger than normal, often easily forms minimum eutectic and causes sticky porcelain and surperficial color spot; High temperature break resistant intensity is not high, and under comparatively high temps, larger load condition, refractory slab degree of deformation is large, and the burning both having affected product is made, and substantially reduces again the work-ing life of refractory slab; Because heat-shock resistance and high temperature toughness are inadequate, therefore burning till fast, in the kiln of rapid heat cycle, refractory slab easily in break, especially at shrinkage joint position cracking, or the fracture of arm of angle portion.
Summary of the invention
The object of the invention is in order to solve existing silicon carbide deck heat-shock resistance and high temperature toughness inadequate, therefore burning till fast, in the kiln of rapid heat cycle, refractory slab is easily in break, especially shrinkage joint position cracking, or the arm of angle portion fracture defect and the anticorrosive silicon carbide deck that a kind of high strength, heat conductivity are good, thermal shock resistance is excellent is provided.
Another object of the present invention is the preparation method in order to provide this anticorrosive silicon carbide deck.
To achieve these goals, the present invention is by the following technical solutions:
A kind of anticorrosive silicon carbide deck, described anticorrosive silicon carbide deck is made up of the raw material of following mass percent: silicon-carbide particle 30-40%, silicon carbide meal 15-20%, carbide fine powder 14-19%, silicon carbide micro-powder 5-10%, Graphene 10-15%, composite antioxidant 2-4%, combined binder 6-8%, lubricating grease 0.2-0.5% and molybdenumdisulphide 0.7-1.5%.In the technical program, Graphene is a kind of novel material of the individual layer sheet structure be made up of carbon atom, has the feature of the high ﹑ specific surface area of strong degree large ﹑ height chemical reaction property ﹑ alive high fillibility; In anticorrosive silicon carbide deck, add Graphene makes anticorrosive silicon carbide deck interior contact more tight, thus because of the stress produced that expands when reducing to burn till, prevents goods from loosening or cracking; The anticorrosive excellent mechanical property that ensure that anticorrosive silicon carbide deck of Graphene, can promote antiacid caustic corrosion performance and the antioxidant property of anticorrosive silicon carbide deck simultaneously.Rosin can increase the elasticity of silicon carbide deck, increases its toughness.
Good in thermal shock, anti-oxidant, slag-resistant, basic metal erosion performance are strong, and resistance to erosion, heat preservation and insulation are excellent, the light silicious brick of high volume good stability; Can be dispersed in refractory slab internal height, acceleration of sintering, and refractory slab is had evenly weave construction, improve the intensity of goods and thermal shock resistance.
Molybdenumdisulphide is the solid powder changing molecular structure by natural concentrated molybdenum ore powder after chemical purification and make.Look black is slightly with silver gray, has metalluster, and that touches has soapy feeling, water insoluble.Product has good dispersity, inadherent advantage, can be added in various grease, forms exhausted inadherent colloidal state, can increase oilness and the extreme pressure property of grease.Also the machine work state of high temperature, high pressure, high rotating speed high loading is applicable to, the extension device life-span.Obtain through chemical purification combined reaction, its pH value is 7-8, shows slightly alkalescence.It covers the surface of friction materials, can protect other materials, prevents them oxidized, especially makes other materials difficult drop-off, and the power that attaches strengthens; Antifriction when molybdenumdisulphide is low temperature for friction materials major function, increase during high temperature and rub, loss on ignition is little, volatile in friction materials.
As preferably, described composite antioxidant is made up of antioxidant 1010, anti-oxidant DLTP and honey, and its mass ratio is 2:2:5.In the technical program, honey itself has oxidation-resistance, and the combination of antioxidant 1010, anti-oxidant DLTP has synergy, and honey serves the effect of lubricant in composite antioxidant, makes antioxidant properties better.
As preferably, described bonding agent is furfuryl resin, mixture with polyacrylamide, furfuryl resin, is 5:2:1 with the mass ratio of polyacrylamide.
As preferably, composite antioxidant is mixed in honey antioxidant 1010, anti-oxidant DLTP, and then at 60-70 DEG C, water bath sonicator dispersion obtains for 2-5 hour.
As preferably, the particle diameter of silicon-carbide particle is 1-3 centimetre, silicon carbide meal 0.5-15 millimeter, carbide fine powder 0.2-12 micron, silicon carbide micro-powder 10-100 nanometer.
As preferably, lubricating grease is high temperature resistant lubricating grease.
A preparation method for anticorrosive silicon carbide deck, described preparation method comprises the following steps:
A) select materials: the particle diameter choosing silicon-carbide particle is 1-3 centimetre, silicon carbide meal 0.5-15 millimeter, carbide fine powder 0.2-12 micron, silicon carbide micro-powder 10-100 nanometer;
B) weigh according to formulation weight per-cent, by silicon-carbide particle, silicon carbide meal, carbide fine powder, silicon carbide micro-powder, Graphene, composite antioxidant, combined binder, lubricating grease mix and blend, obtain mixed powder;
C) mixed powder step b) obtained adopts vibratory compaction pressing machine to be pressed, and obtains silicon carbide biscuit;
D) silicon carbide biscuit step c) obtained dry 1-3 hour at 280-320 DEG C, then continues dry 12-24 hour at 65-85 DEG C;
E) fired in vacuum oven by the silicon carbide biscuit after step d) process, temperature 2100-2300 DEG C, time 5-10 hour, then at 1750-1850 DEG C, be incubated 12-16 hour, cooling obtains silicon carbide deck work in-process;
F) molybdenumdisulphide is sprayed into the half-finished surface of carborundum plate that step e) obtains by use plasma spraying technology, and thickness 0.5-0.8 micron, obtains anticorrosive silicon carbide deck.In the technical program, at silicon carbide deck surface spraying molybdenumdisulphide to form the protective membrane of one deck densification, promote the resistance to fouling of silicon carbide deck further, oxidation-resistance, thermal-shock resistance.
As preferably, the processing parameter of plasma spraying technology is: argon pressure 0.85-0.95Mpa, and nitrogen pressure is 0.45-0.60Mpa, voltage 90-120V, electric current 700-850A, spray distance 160-200 millimeter.
The invention has the beneficial effects as follows: product good in thermal shock of the present invention, anti-oxidant, slag-resistant, basic metal erosion performance are strong, and resistance to erosion, heat preservation and insulation are excellent, the light silicious brick of high volume good stability; Can be dispersed in refractory slab internal height, acceleration of sintering, and refractory slab is had evenly weave construction, improve the intensity of goods and thermal shock resistance.
Embodiment
Below in conjunction with specific embodiment, the present invention is further explained, the restriction not to its protection domain.
The particle diameter of silicon-carbide particle is 1-3 centimetre, silicon carbide meal 0.5-15 millimeter, carbide fine powder 0.2-12 micron, silicon carbide micro-powder 10-100 nanometer.
Lubricating grease is high temperature resistant lubricating grease, purchased from Shanghai Rui Bei petrochemical industry company limited.
Embodiment 1
A preparation method for anticorrosive silicon carbide deck, described preparation method comprises the following steps:
A) select materials: the particle diameter choosing silicon-carbide particle is 1-3 centimetre, silicon carbide meal 0.5-15 millimeter, carbide fine powder 0.2-12 micron, silicon carbide micro-powder 10-100 nanometer;
B) weigh according to formulation weight per-cent, by silicon-carbide particle, silicon carbide meal, carbide fine powder, silicon carbide micro-powder, Graphene, composite antioxidant, combined binder, lubricating grease mix and blend, obtain mixed powder; Described composite antioxidant is made up of antioxidant 1010, anti-oxidant DLTP and honey, and its mass ratio is 2:2:5;
Composite antioxidant is mixed in honey antioxidant 1010, anti-oxidant DLTP, and then at 60 DEG C, water bath sonicator disperses to obtain for 2 hours;
Bonding agent be furfuryl resin, with the mixture of polyacrylamide, furfuryl resin, be 5:2:1 with the mass ratio of polyacrylamide;
C) mixed powder step b) obtained adopts vibratory compaction pressing machine to be pressed, and obtains silicon carbide biscuit;
D) silicon carbide biscuit step c) obtained at 280 DEG C dry 1 hour, then continues dry 12 hours at 65 DEG C;
E) fired in vacuum oven by the silicon carbide biscuit after step d) process, temperature 2100 DEG C, 5 hours time, then at 1750 DEG C, be incubated 12 hours, cooling obtains silicon carbide deck work in-process;
F) molybdenumdisulphide is sprayed into the half-finished surface of carborundum plate that step e) obtains by use plasma spraying technology, and thickness 0.5-0.8 micron, obtains anticorrosive silicon carbide deck; The processing parameter of plasma spraying technology is: argon pressure 0.85Mpa, and nitrogen pressure is 0.45Mpa, voltage 90V, electric current 700A, spray distance 160 millimeters.
Anticorrosive silicon carbide deck is made up of the raw material of following mass percent: silicon-carbide particle 30%, silicon carbide meal 20%, carbide fine powder 14%, silicon carbide micro-powder 10%, Graphene 15%, composite antioxidant 4%, combined binder 6%, lubricating grease 0.2% and molybdenumdisulphide 0.8%.
Embodiment 2
A preparation method for anticorrosive silicon carbide deck, described preparation method comprises the following steps:
A) select materials: the particle diameter choosing silicon-carbide particle is 1-3 centimetre, silicon carbide meal 0.5-15 millimeter, carbide fine powder 0.2-12 micron, silicon carbide micro-powder 10-100 nanometer;
B) weigh according to formulation weight per-cent, by silicon-carbide particle, silicon carbide meal, carbide fine powder, silicon carbide micro-powder, Graphene, composite antioxidant, combined binder, lubricating grease mix and blend, obtain mixed powder; Described composite antioxidant is made up of antioxidant 1010, anti-oxidant DLTP and honey, and its mass ratio is 2:2:5;
Composite antioxidant is mixed in honey antioxidant 1010, anti-oxidant DLTP, and then at 65 DEG C, water bath sonicator disperses to obtain for 3 hours;
Bonding agent be furfuryl resin, with the mixture of polyacrylamide, furfuryl resin, be 5:2:1 with the mass ratio of polyacrylamide;
C) mixed powder step b) obtained adopts vibratory compaction pressing machine to be pressed, and obtains silicon carbide biscuit;
D) silicon carbide biscuit step c) obtained at 300 DEG C dry 2 hours, then continues dry 16 hours at 70 DEG C;
E) fired in vacuum oven by the silicon carbide biscuit after step d) process, temperature 2200 DEG C, 7 hours time, then at 1800 DEG C, be incubated 14 hours, cooling obtains silicon carbide deck work in-process;
F) molybdenumdisulphide is sprayed into the half-finished surface of carborundum plate that step e) obtains by use plasma spraying technology, and thickness 0.5-0.8 micron, obtains anticorrosive silicon carbide deck; The processing parameter of plasma spraying technology is: argon pressure 0.9Mpa, and nitrogen pressure is 0.55Mpa, voltage 100V, electric current 750A, spray distance 180 millimeters.
Anticorrosive silicon carbide deck is made up of the raw material of following mass percent: silicon-carbide particle 35%, silicon carbide meal 18%, carbide fine powder 19%, silicon carbide micro-powder 5%, Graphene 12%, composite antioxidant 3%, combined binder 7%, lubricating grease 0.3% and molybdenumdisulphide 0.7%.
Embodiment 3
A preparation method for anticorrosive silicon carbide deck, described preparation method comprises the following steps:
A) select materials: the particle diameter choosing silicon-carbide particle is 1-3 centimetre, silicon carbide meal 0.5-15 millimeter, carbide fine powder 0.2-12 micron, silicon carbide micro-powder 10-100 nanometer;
B) weigh according to formulation weight per-cent, by silicon-carbide particle, silicon carbide meal, carbide fine powder, silicon carbide micro-powder, Graphene, composite antioxidant, combined binder, lubricating grease mix and blend, obtain mixed powder; Described composite antioxidant is made up of antioxidant 1010, anti-oxidant DLTP and honey, and its mass ratio is 2:2:5;
Composite antioxidant is mixed in honey antioxidant 1010, anti-oxidant DLTP, and then at 70 DEG C, water bath sonicator disperses to obtain for 5 hours;
Bonding agent is the mixture of furfuryl resin, nano-calcium carbonate and polyacrylamide, and the mass ratio of furfuryl resin, nano-calcium carbonate and polyacrylamide is 5:2:1;
C) mixed powder step b) obtained adopts vibratory compaction pressing machine to be pressed, and obtains silicon carbide biscuit;
D) silicon carbide biscuit step c) obtained at 320 DEG C dry 3 hours, then continues dry 24 hours at 85 DEG C;
E) fired in vacuum oven by the silicon carbide biscuit after step d) process, temperature 2300 DEG C, 10 hours time, then at 1850 DEG C, be incubated 16 hours, cooling obtains silicon carbide deck work in-process;
F) molybdenumdisulphide is sprayed into the half-finished surface of carborundum plate that step e) obtains by use plasma spraying technology, and thickness 0.5-0.8 micron, obtains anticorrosive silicon carbide deck; The processing parameter of plasma spraying technology is: argon pressure 0.95Mpa, and nitrogen pressure is 0.60Mpa, voltage 120V, electric current 850A, spray distance 200 millimeters.
Anticorrosive silicon carbide deck is made up of the raw material of following mass percent: silicon-carbide particle 40%, silicon carbide meal 15%, carbide fine powder 15%, silicon carbide micro-powder 8%, Graphene 10%, composite antioxidant 2%, combined binder 8%, lubricating grease 0.5% and molybdenumdisulphide 1.5%.
Comparative example 1, commercially available silicon carbide deck.
Table 1 is the test data of the silicon carbide deck of the anticorrosive silicon carbide deck prepared of embodiment 1-3 and comparative example 1.
Table 1, test data
| There is crack in 1100 DEG C of water-cooled experiment circulating chilled water number of times | Strength at normal temperature (Mpa) | Volume density (g/ cm 3) | |
| Embodiment 1 | 50 | 59 | 2.82 |
| Embodiment 2 | 55 | 62 | 2.85 |
| Embodiment 3 | 60 | 67 | 2.88 |
| Comparative example 1 | 30 | 35 | 2.61 |
Table 1 is visible, the volume density of silicon carbide deck prepared by the present invention is higher than commercially available silicon carbide deck, that is thermal shock resistance is better, just occurs crack, illustrate that silicon carbide deck thermal shock resistance prepared by the present invention is good at 1100 DEG C of water-cooled experiment circulating chilled water number of times 50-60.
Claims (8)
1. an anticorrosive silicon carbide deck, it is characterized in that, described anticorrosive silicon carbide deck is made up of the raw material of following mass percent: silicon-carbide particle 30-40%, silicon carbide meal 15-20%, carbide fine powder 14-19%, silicon carbide micro-powder 5-10%, Graphene 10-15%, composite antioxidant 2-4%, combined binder 6-8%, lubricating grease 0.2-0.5% and molybdenumdisulphide 0.7-1.5%.
2. the anticorrosive silicon carbide deck of one according to claim 1, is characterized in that, described composite antioxidant is made up of antioxidant 1010, anti-oxidant DLTP and honey, and its mass ratio is 2:2:5.
3. the anticorrosive silicon carbide deck of one according to claim 1, is characterized in that, described bonding agent is the mixture of furfuryl resin, nano-calcium carbonate and paraffin, and the mass ratio of furfuryl resin, nano-calcium carbonate and paraffin is 5:2:1.
4. the anticorrosive silicon carbide deck of one according to claim 1 and 2, is characterized in that, composite antioxidant is mixed in honey antioxidant 1010, anti-oxidant DLTP, and then at 60-70 DEG C, water bath sonicator dispersion obtains for 2-5 hour.
5. the anticorrosive silicon carbide deck of one according to claim 1 or 2 or 3, is characterized in that, the particle diameter of silicon-carbide particle is 1-3 centimetre, silicon carbide meal 0.5-15 millimeter, carbide fine powder 0.2-12 micron, silicon carbide micro-powder 10-100 nanometer.
6. the preparation method of a kind of anticorrosive silicon carbide deck according to claim 1 or 2 or 3, is characterized in that, lubricating grease is high temperature resistant lubricating grease.
7. a preparation method for anticorrosive silicon carbide deck as claimed in claim 1, is characterized in that, described preparation method comprises the following steps:
A) select materials: the particle diameter choosing silicon-carbide particle is 1-3 centimetre, silicon carbide meal 0.5-15 millimeter, carbide fine powder 0.2-12 micron, silicon carbide micro-powder 10-100 nanometer;
B) weigh according to formulation weight per-cent, by silicon-carbide particle, silicon carbide meal, carbide fine powder, silicon carbide micro-powder, Graphene, composite antioxidant, combined binder, lubricating grease mix and blend, obtain mixed powder;
C) mixed powder step b) obtained adopts vibratory compaction pressing machine to be pressed, and obtains silicon carbide biscuit;
D) silicon carbide biscuit step c) obtained dry 1-3 hour at 280-320 DEG C, then continues dry 12-24 hour at 65-85 DEG C;
E) fired in vacuum oven by the silicon carbide biscuit after step d) process, temperature 2100-2300 DEG C, time 5-10 hour, then at 1750-1850 DEG C, be incubated 12-16 hour, cooling obtains silicon carbide deck work in-process;
F) molybdenumdisulphide is sprayed into the half-finished surface of carborundum plate that step e) obtains by use plasma spraying technology, and thickness 0.5-0.8 micron, obtains anticorrosive silicon carbide deck.
8. the preparation method of a kind of anticorrosive silicon carbide deck according to claim 7, it is characterized in that, the processing parameter of plasma spraying technology is: argon pressure 0.85-0.95Mpa, nitrogen pressure is 0.45-0.60Mpa, voltage 90-120V, electric current 700-850A, spray distance 160-200 millimeter.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107500782A (en) * | 2017-09-19 | 2017-12-22 | 迟逞 | A kind of preparation method of increasing material manufacturing modified anti-friction wear-resistant nano-ceramic powder material against corrosion |
| CN107602131A (en) * | 2017-09-18 | 2018-01-19 | 山东理工大学 | A kind of carborundum composite-phase ceramic |
| CN107778012A (en) * | 2017-09-18 | 2018-03-09 | 山东理工大学 | A kind of preparation method of carborundum composite-phase ceramic |
| CN117003570A (en) * | 2023-08-17 | 2023-11-07 | 湖南昌诺新材料有限公司 | Ultrathin silicon carbide canopy plate composition and preparation method thereof |
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| EP2280095A2 (en) * | 2009-07-30 | 2011-02-02 | Ewald Dörken Ag | Method for electrochemical coating a workpiece |
| CN103131155A (en) * | 2013-03-06 | 2013-06-05 | 广州千松科技有限公司 | High-thermal conductive plasticized ceramic material and preparation method and application thereof |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2280095A2 (en) * | 2009-07-30 | 2011-02-02 | Ewald Dörken Ag | Method for electrochemical coating a workpiece |
| CN103131155A (en) * | 2013-03-06 | 2013-06-05 | 广州千松科技有限公司 | High-thermal conductive plasticized ceramic material and preparation method and application thereof |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107602131A (en) * | 2017-09-18 | 2018-01-19 | 山东理工大学 | A kind of carborundum composite-phase ceramic |
| CN107778012A (en) * | 2017-09-18 | 2018-03-09 | 山东理工大学 | A kind of preparation method of carborundum composite-phase ceramic |
| CN107500782A (en) * | 2017-09-19 | 2017-12-22 | 迟逞 | A kind of preparation method of increasing material manufacturing modified anti-friction wear-resistant nano-ceramic powder material against corrosion |
| CN107500782B (en) * | 2017-09-19 | 2020-05-05 | 迟逞 | Preparation method of modified antifriction wear-resistant corrosion-resistant nano ceramic powder material for additive manufacturing |
| CN117003570A (en) * | 2023-08-17 | 2023-11-07 | 湖南昌诺新材料有限公司 | Ultrathin silicon carbide canopy plate composition and preparation method thereof |
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