CN1268580C - Method for preparing SIC micro nano ceramic powder via refinery coke salt bath synthesis - Google Patents
Method for preparing SIC micro nano ceramic powder via refinery coke salt bath synthesis Download PDFInfo
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- CN1268580C CN1268580C CN 02159009 CN02159009A CN1268580C CN 1268580 C CN1268580 C CN 1268580C CN 02159009 CN02159009 CN 02159009 CN 02159009 A CN02159009 A CN 02159009A CN 1268580 C CN1268580 C CN 1268580C
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Abstract
The present invention relates to a preparation method of SiC micro-nano ceramic powder, which belongs to the field of ceramic material preparation. The present invention discloses a preparation method of SiC micro-nano ceramic powder through petroleum coke salt bath synthesis, which has the main technological process that Si powder with the particle size of 100 meshes to 200 meshes and petroleum coke are taken to be mixed according to the atomic ratio of Si to C in the petroleum coke of 1:1, NaCl salt accounting for 40 to 60 wt% of the total weight of the powder lot is added, and then the materials are put in a mixing tank to be mixed for 3 to 5 hours and then pressed into billets at the pressure of 3MPas; the billets are put in NaCl molten salt of 1000DEGC for heat preservation for 15 minutes, then cooled and desalted, and the SiC micro-nano ceramic powder with the size of 50 nm to 160 nm is prepared. The present invention has the main characteristics of simple technology, low cost, little investment, mature technology and popularization for use.
Description
The invention belongs to field of ceramic material preparation, relate to the micro-nano ceramic powder material preparation of SiC.
The main method of prior art for preparing SiC powder is: (1) chemical combination method: adopt Si and carbon black to react in carbon tube furnace and make the SiC powder.(2) carbothermic method: by metal oxide or nonmetal oxide and carbon reaction generation carbide; (3) vapour deposition process etc.
The shortcoming of prior art is: preparation temperature height, complex process, cost height generally can not reach micro-nano granularity.In order to overcome the above-mentioned deficiency of prior art, find technological process method simple, with low cost to prepare the SiC ceramic powder, and utilize the low value-added byproduct refinery coke of petroleum industry to prepare the micro-nano ceramic powder material of SiC, special proposition technical solution of the present invention.
Basic design of the present invention is, because the main component of refinery coke is an organic carbon, wherein foreign matter content has only about 10%, and the C in the refinery coke and Si powder chemical reaction at high temperature can take place emit big heat, and the principle of generation SiC.In mechanical milling process, along with the prolongation of time, the powder particle diminishes, specific surface area increases, the active raising; The adding of NaCl salt makes the powder particle fully disperse in mechanical milling process, is easy to form micro-nano size ceramic powder when carrying out chemical reaction in high temp. salt subsequently; High-temperature molten salt not only provides chemical reaction needed initial temperature, also the particle that generates is had good wetting action, has avoided the reunion of micro-nano ceramic powder.
A kind of method of utilizing refinery coke chemistry reaction method manufactured SiC ceramic powder that the present invention is designed, it is characterized in that: getting granularity is 100～200 purpose Si powder and 200 purpose petroleum coke powders, in 1: 1 ratio batch mixes of C atomic ratio in Si and the refinery coke, add the NaCl salt that accounts for powder gross weight 40～60wt% and make base substrate, base substrate put into 1000 ℃ NaCl melting salt, be incubated 15 minutes, chemical reaction takes place in powder in fused salt, through demineralising process, prepare size after the cooling at the micro-nano ceramic powder of the SiC of 50nm～160nm.
A kind of method of utilizing refinery coke chemistry reaction method manufactured SiC ceramic powder that the present invention is designed, it is further characterized in that, the preparation method of base substrate is: add 40～60wt% salt in Si and refinery coke mixed powder after, pack in the mixing tank, the planet gear type drum's speed of rotation is controlled at 150 rev/mins, ratio of grinding media to material is 20: 1, and ball grinder is evacuated to 0.133～1.333Pa and charges into argon gas, and argon pressure is 1.0 * 10
5The scope of Pa, ball milling 4～6 hours is pressed into base substrate under 3MPa pressure; Demineralising process is: the water that the NaCl salt that will be loaded with ceramic powder after will cooling off is put into 5 times of salt weight soaked 10～15 hours, after NaCl salt 100% is soluble in water, filtered out ceramic powder; The control method of micro-nano ceramic powder size is: preparation during less than the ceramic powder of 85nm, adds the NaCl salt that accounts for reactant gross weight 60wt%, ball milling 6 hours more than or equal to 50nm; Preparation during less than the ceramic powder of 120nm, adds the NaCl salt that accounts for reactant gross weight 50wt%, ball milling 5 hours more than or equal to 85nm; Preparation during smaller or equal to the ceramic powder of 160nm, adds the NaCl salt that accounts for reactant gross weight 40wt%, ball milling 4 hours more than or equal to 120nm.
Prior art generally needs at high temperature or synthesizes SiC, cost height with pure Si, C powder.The present invention utilizes the byproduct in the petroleum refining process---and refinery coke prepares the micro-nano ceramic powder of SiC as raw material, and preparation process technology is simple, cost is low, has solved waste disposal problem simultaneously.At present, the utility value of prior art refinery coke is very low, and wherein part is used to make the carbon element product, but most of refinery coke is used for fuel, not only utilizes benefit low, goes back serious environment pollution.
Major advantage of the present invention is: (1) technology is simple, and cost is low, and (2) have improved the refinery coke comprehensive utilization value, and (3) have solved waste disposal problem, helps environment protection simultaneously.
Below in conjunction with specific examples of the present invention, further specify details of the present invention.
Embodiment 1:
Prepare main size-grade distribution more than or equal to 50nm less than the micro-nano ceramic powder of the SiC of 85nm
Raw material is the commercial Si powder of 100 orders～200 purposes, and 200 purpose refinery cokes, refinery coke its content of impurities after measured are 4.0wt%, is 1: 1 batching by the atomic ratio of carbon in Si and the refinery coke, gets Si powder 28 grams, and refinery coke 6.25 restrains, and 34.25g altogether prepares burden; Add NaCl salt 20.55 grams account for gross weight 60wt%, put into mixing tank after the mixing, with mixing tank with seal with elastometic washer after, be evacuated to 0.133～1.333Pa, charge into argon gas, pressure is 1.0 * 10
5Pa, drum's speed of rotation is 150 rev/mins, ratio of grinding media to material is 20: 1 during batch mixing, behind the batch mixing 6h, be pressed into the base substrate of φ 20mm under the pressure with 3MPa in mould, base substrate put into 1000 ℃ NaCl melting salt insulation 15 minutes, the water of the salt that is loaded with the micro-nano ceramic powder of SiC after the reaction cooling being put into 5 times of salt weight soaked 15 hours, after salt 100% incorporates in the water, filter out the micro-nano ceramic powder of SiC, the SiC powder is washed back oven dry repeatedly with deionized water, after measured the micro-nano ceramic powder granularity of SiC more than or equal to 50nm less than 85nm.
Embodiment 2:
Prepare main size-grade distribution more than or equal to 85nm less than the micro-nano ceramic powder of the SiC of 120nm
Raw material is the commercial Si powder of 100 orders～200 purposes, and 200 purpose refinery cokes, refinery coke its content of impurities after measured are 8.5wt%, is 1: 1 batching by the atomic ratio of carbon in Si and the refinery coke, gets Si powder 24 grams, and refinery coke 6.56 restrains, and 34.56g altogether prepares burden; Add NaCl salt 17.33 grams account for gross weight 50wt%, put into mixing tank after the mixing, with mixing tank with seal with elastometic washer after, be evacuated to 0.133～1.333Pa, charge into argon gas, pressure is 1.0 * 10
5Pa, drum's speed of rotation is 150 rev/mins, ratio of grinding media to material is 20: 1 during batch mixing, behind the batch mixing 5h, be pressed into the base substrate of φ 20mm under the pressure with 3MPa in mould, base substrate put into 1000 ℃ NaCl melting salt insulation 15 minutes, the water of the salt that is loaded with the micro-nano ceramic powder of SiC after the reaction cooling being put into 5 times of salt weight soaked 15 hours, after salt 100% incorporates in the water, filter out the micro-nano ceramic powder of SiC, the SiC powder is washed the back oven dry repeatedly with deionized water, and the micro-nano ceramic powder granularity of SiC is less than 120nm more than or equal to 85nm after measured.
Embodiment 3:
Prepare main size-grade distribution more than or equal to 120nm smaller or equal to the micro-nano ceramic powder of the SiC of 160nm
Raw material is the commercial Si powder of 100 orders～200 purposes, and 200 purpose refinery cokes, refinery coke its content of impurities after measured are 12.6wt%, is 1: 1 batching by the atomic ratio of carbon in Si and the refinery coke, gets Si powder 24 grams, and refinery coke 6.86 restrains, and 34.86g altogether prepares burden; Add NaCl salt 13.94 grams account for gross weight 40wt%, put into mixing tank after the mixing, with mixing tank with seal with elastometic washer after, be evacuated to 0.133～1.333Pa, charge into argon gas, pressure is 1.0 * 10
5Pa, drum's speed of rotation is 150 rev/mins, ratio of grinding media to material is 20: 1 during batch mixing, behind the batch mixing 4h, be pressed into the base substrate of φ 20mm under the pressure with 3MPa in mould, base substrate put into 1000 ℃ NaCl melting salt insulation 15 minutes, the water of the salt that is loaded with the micro-nano ceramic powder of SiC after the reaction cooling being put into 5 times of salt weight soaked 15 hours, after salt 100% incorporates in the water, filter out the micro-nano ceramic powder of SiC, the SiC powder is washed the back oven dry repeatedly with deionized water, and the micro-nano ceramic powder granularity of SiC is smaller or equal to 160nm more than or equal to 120nm after measured.
Claims (4)
1, a kind of synthetic method for preparing the micro-nano ceramic powder of SiC of refinery coke salt bath of utilizing, it is characterized in that: getting granularity is 100 orders～200 purpose Si powder and 200 order refinery cokes, in 1: 1 ratio batch mixes of C atomic ratio in Si and the refinery coke, add the NaCl salt that accounts for powder gross weight 40～60wt% and make base substrate, base substrate put into 1000 ℃ NaCl melting salt, be incubated 15 minutes, chemical reaction takes place in powder in fused salt, through demineralising process, prepare size after the cooling at the micro-nano ceramic powder of the SiC of 50nm～160nm.
2, a kind of synthetic method for preparing the micro-nano ceramic powder of SiC of refinery coke salt bath of utilizing according to claim 1, it is characterized in that, the preparation method of base substrate is: add 40～60wt% salt in Si and refinery coke mixed powder after, pack in the mixing tank, the planet gear type drum's speed of rotation is controlled at 150 rev/mins, ratio of grinding media to material is 20: 1, and ball grinder is evacuated to 0.133～1.333Pa and charges into argon gas, and argon pressure is 1.0 * 10
5The scope of Pa, ball milling 4～6 hours is pressed into base substrate under 3MPa pressure.
3, a kind of synthetic method for preparing the micro-nano ceramic powder of SiC of refinery coke salt bath of utilizing according to claim 1, it is characterized in that, demineralising process is: the water that the NaCl salt that will be loaded with ceramic powder after will cooling off is put into 5 times of salt weight soaked 10～15 hours, after NaCl salt 100% is soluble in water, filter out ceramic powder.
4, a kind of method of utilizing refinery coke salt bath synthesis method to prepare the micro-nano ceramic powder of SiC according to claim 1 and 2, it is characterized in that, the control method of micro-nano ceramic powder size is: preparation is more than or equal to 50nm during less than the ceramic powder of 85nm, add the NaCl salt that accounts for reactant gross weight 60wt%, ball milling 6 hours; Preparation during less than the ceramic powder of 120nm, adds the NaCl salt that accounts for reactant gross weight 50wt%, ball milling 5 hours more than or equal to 85nm; Preparation during smaller or equal to the ceramic powder of 160nm, adds the NaCl salt that accounts for reactant gross weight 40wt%, ball milling 4 hours more than or equal to 120nm.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02159009 CN1268580C (en) | 2002-12-27 | 2002-12-27 | Method for preparing SIC micro nano ceramic powder via refinery coke salt bath synthesis |
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| CN 02159009 CN1268580C (en) | 2002-12-27 | 2002-12-27 | Method for preparing SIC micro nano ceramic powder via refinery coke salt bath synthesis |
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| CN1511807A CN1511807A (en) | 2004-07-14 |
| CN1268580C true CN1268580C (en) | 2006-08-09 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103318891B (en) * | 2013-07-08 | 2015-01-28 | 武汉科技大学 | Method for generating one-dimensional silicon carbide nanowires on multiporous charcoal template |
| CN105777128A (en) * | 2016-03-01 | 2016-07-20 | 郑州大学 | Method for synthesizing hafnium carbide ceramic powder at low temperature through assisting of molten salts and magnesiothermic reduction |
| CN105732043A (en) * | 2016-03-01 | 2016-07-06 | 郑州大学 | Method for preparing hafnium carbide ceramic powder body by using fused salt under assistance of carbon thermal reduction |
| CN105732042A (en) * | 2016-03-01 | 2016-07-06 | 郑州大学 | Method for preparing ultrafine tantalum carbide powder by using fused salt under assistance of low temperature |
| DE102017006658A1 (en) * | 2017-07-13 | 2019-01-17 | Forschungszentrum Jülich GmbH | Process for the preparation of non-oxide, ceramic powders |
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