CN1247485C - Method for preparing TiC micro nano ceramic powder via refinery coke salt bath synthesis - Google Patents
Method for preparing TiC micro nano ceramic powder via refinery coke salt bath synthesis Download PDFInfo
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- CN1247485C CN1247485C CN 02159005 CN02159005A CN1247485C CN 1247485 C CN1247485 C CN 1247485C CN 02159005 CN02159005 CN 02159005 CN 02159005 A CN02159005 A CN 02159005A CN 1247485 C CN1247485 C CN 1247485C
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- ceramic powder
- nacl
- powder
- tic
- refinery coke
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Abstract
The present invention relates to a preparation method of TiC micro-nano ceramic powder, which belongs to the field of ceramic material preparation. The present invention discloses a preparation method of TiC micro-nano ceramic powder through petroleum coke salt bath synthesis, and has the main technological steps that Ti powder with the particle size of 100 meshes to 200 meshes and petroleum coke are prepared and mixed according to the atomic ratio of Ti 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 at 900 DEGC for heat preservation for 15 minutes; then the mixture is cooled and desalted, and the TiC micro-nano ceramic powder with the size of 20 nm to 150 nm is prepared. The present invention has the main characteristics of simple technology, low cost, little investment, mature technology and popularization for use.
Description
Technical field
The invention belongs to field of ceramic material preparation, relate to the micro-nano ceramic powder material preparation of TiC.
Background technology
TiC is a kind of face-centered cubic crystal structure stupalith commonly used, has high rigidity, high-melting-point, high conductivity and very high chemical stability, has broad application background in technical fields such as machinery, chemical industry and electronics.
The main method of prior art for preparing TiC ceramic powder is: adopt TiO
2The at high temperature synthetic TiC pottery of powder and graphite C perhaps adopts TiO
2(react among the 1800K～2100K) and make the TiC powder at the carbon tube furnace of logical hydrogen or high frequency vacuum oven with carbon black.
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 deficiencies in the prior art, find technological process method simple, with low cost to prepare the micro-nano ceramic powder of TiC, and utilize the low value-added byproduct refinery coke of petroleum industry to prepare the micro-nano ceramic powder material of TiC, special proposition technical solution of the present invention.
Summary of the 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 Ti powder chemical reaction at high temperature can take place emit a large amount of heat, and the principle of generation TiC.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; The high temperature composite 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 TiC ceramic powder that the present invention is designed, it is characterized in that: getting granularity is 100 orders～200 purpose Ti powder and 200 purpose refinery cokes, press 1: 1 mixed of C atomic ratio in Ti and the refinery coke, add the NaCl that accounts for Ti and petroleum coke powder gross weight 40～60wt%, ball milling, make base substrate, base substrate put into 900 ℃ fusion NaCl, be incubated 15 minutes, chemical reaction takes place in powder in this fused salt, remove NaCl through demineralising process after the cooling, prepare size at the TiC of 20nm～150nm ceramic powder.
A kind of method of utilizing the micro-nano ceramic powder of refinery coke chemistry reaction method manufactured TiC that the present invention is designed, it is further characterized in that, after in Ti and refinery coke mixed powder, adding 40～60wt%NaCl, pack in the ball grinder, the planet gear type drum's speed of rotation is controlled at 100 rev/mins, ratio of grinding media to material is 20: 1, and ball grinder is evacuated to 10
-3～10
-2(0.133～1.333Pa) and charge into argon gas, argon pressure is 1.0atm (1.01 * 10 to torr
5Pa) scope, batch mixing 3～5 hours is pressed into base substrate under 3MPa pressure; Demineralising process is: the NaCl that will be loaded with ceramic powder after will cooling off puts into water and soaked 10～15 hours, and the weight of water is 5 times of this NaCl weight, after NaCl100% is soluble in water, filters out ceramic powder; The control method of ceramic powder size is: when preparing the ceramic powder of 20nm～70nm, add the NaCl that accounts for above-mentioned powder gross weight 60wt%, ball milling 5 hours; When preparing the ceramic powder of 70nm～100nm, add the NaCl that accounts for above-mentioned powder gross weight 50wt%, ball milling 4 hours; When preparing the ceramic powder of 100nm～150nm, add the NaCl that accounts for above-mentioned powder gross weight 40wt%, ball milling 3 hours.
Prior art generally needs at high temperature or synthesizes TiC, cost height with pure Ti, C powder.The present invention utilizes byproduct-refinery coke in the petroleum refining process as raw material, the micro-nano ceramic powder of preparation TiC, and preparation process technology is simple, cost is low, has solved waste disposal problem simultaneously.Under the prior art condition, the utility value of prior art refinery coke is very low at present, 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, and serious environment pollution.
Major advantage of the present invention is: (1) technology is simple, cost is low, preparation temperature is low, and (2) have solved the cheap by product of solid of refining of petroleum industry and handled problems, and help environment protection simultaneously.(3) improved the refinery coke comprehensive utilization value.
Embodiment
Below in conjunction with specific examples of the present invention, further specify details of the present invention.
Embodiment 1:
Prepare main size-grade distribution at the TiC of 20nm～70nm nano-ceramic powder
Raw material is the commercial Ti powder of 100 orders～200 purposes, and 200 purpose refinery cokes, refinery coke content of impurities after measured are 4.0%, is 1: 1 batching by the atomic ratio of carbon in Ti and the refinery coke, gets Ti powder 24 grams, and refinery coke 6.25 restrains, and 30.25g altogether prepares burden; Add NaCl salt 18.15 grams account for gross weight 60wt%, put into mixing tank after the mixing, the planet gear type drum's speed of rotation is set at 100 rev/mins, with mixing tank with seal with elastometic washer after, be evacuated to 10
-3～10
-2Torr (1.333～0.133Pa), charge into argon gas, pressure is 1.0atm (1.01 * 10
5Pa), 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 900 ℃ NaCl melting salt insulation 15 minutes, the salt that is loaded with the micro-nano ceramic powder of TiC after the reaction cooling is put into water soaked 15 hours, the weight of water is 5 times of this NaCl weight.After salt 100% incorporates in the water, filter out the micro-nano ceramic powder of TiC, the TiC powder is washed the back oven dry repeatedly with deionized water, the micro-nano ceramic powder granularity of TiC is 20nm～70nm after measured.
Embodiment 2:
Prepare main size-grade distribution at the TiC of 70nm～100nm nano-ceramic powder
Raw material: the commercial Ti powder of 100 orders～200 purposes, 200 purpose refinery cokes, refinery coke content of impurities after measured are 8.5%, are 1: 1 batching by the atomic ratio of carbon in Ti and the refinery coke, get Ti powder 24 grams, and refinery coke 6.56 restrains, and 30.56g altogether prepares burden; Add the NaCl salt 15.26 gram NaCl salt account for gross weight 50wt%, put into mixing tank after the mixing, the planet gear type drum's speed of rotation is set at 100 rev/mins, with mixing tank with seal with elastometic washer after, be evacuated to 10
-3～10
-2Torr (1.333～0.133Pa), charge into argon gas, pressure is 1.0atm (1.01 * 10
5Pa), 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 900 ℃ NaCl melting salt insulation 15 minutes, the salt that is loaded with the micro-nano ceramic powder of TiC after the reaction cooling is put into water soaked 15 hours, the weight of water is 5 times of this NaCl weight.After salt 100% incorporates in the water, filter out the micro-nano ceramic powder of TiC, the TiC powder is washed the back oven dry repeatedly with deionized water, the micro-nano ceramic powder granularity of TiC is 70nm～100nm after measured.
Embodiment 3:
Prepare main size-grade distribution at the TiC of 100nm～150nm micrometer ceramics powder
Raw material: the commercial Ti powder of 100～200 purposes, 200 purpose refinery cokes, refinery coke content of impurities after measured are 12.6wt%, are 1: 1 batching by the atomic ratio of carbon in Ti and the refinery coke, get Ti powder 24 grams, and refinery coke 6.86 restrains, and 30.86g altogether prepares burden; Add NaCl salt 12.34 grams account for gross weight 40wt%, put into mixing tank after the mixing, the planet gear type drum's speed of rotation is set at 100 rev/mins, with mixing tank with seal with elastometic washer after, be evacuated to 10
-3～10
-2Torr (1.333～0.133Pa), charge into argon gas, pressure is 1.0atm (1.01 * 10
5Pa), ratio of grinding media to material is 20: 1 during batch mixing, behind the batch mixing 3h, be pressed into the base substrate of φ 20mm under the pressure with 3MPa in mould, base substrate put into 900 ℃ NaCl melting salt insulation 15 minutes, the salt that is loaded with the micro-nano ceramic powder of TiC after the reaction cooling is put into water soaked 15 hours, the weight of water is 5 times of this NaCl weight.After salt 100% incorporates in the water, filter out the micro-nano ceramic powder of TiC, the TiC powder is washed the back oven dry repeatedly with deionized water, the micro-nano ceramic powder granularity of TiC is 100nm～150nm after measured.
Claims (4)
1, a kind of synthetic method for preparing the micro-nano ceramic powder of TiC of refinery coke salt bath of utilizing, it is characterized in that: getting granularity is 100 orders～200 purpose Ti and 200 purpose petroleum coke powders, press 1: 1 mixed of C atomic ratio in Ti and the refinery coke, add the NaCl that accounts for Ti and petroleum coke powder gross weight 40～60wt%, ball milling, make base substrate, base substrate is put into 900 ℃ fusion NaCl, be incubated 15 minutes, remove NaCl after the cooling, prepare size at the TiC of 20nm～150nm ceramic powder.
2, a kind of synthetic method for preparing the micro-nano ceramic powder of TiC 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%NaCl in Ti and refinery coke mixed powder after, pack in the ball grinder, the planet gear type drum's speed of rotation is controlled at 100 rev/mins, ratio of grinding media to material is 20: 1, and ball grinder is evacuated to 1.333～0.133Pa and charges into argon gas, and argon pressure is 1.01 * 10
5Pa, batch mixing 3～5 hours is pressed into base substrate under 3MPa pressure.
3, a kind of synthetic method for preparing the micro-nano ceramic powder of TiC of refinery coke salt bath of utilizing according to claim 1, it is characterized in that, the process that removes NaCl is: the NaCl that will be loaded with the TiC powder after will cooling off puts into water and soaked 10～15 hours, the weight of water is 5 times of this NaCl weight, after NaCl100% is soluble in water, filter out the TiC ceramic powder.
4, a kind of method of utilizing the salt bath synthesis method to prepare micro-nano ceramic powder according to claim 1 and 2, it is characterized in that, the control method of TiC ceramic powder size is: when preparing the ceramic powder of 20nm～70nm, add the NaCl that accounts for described powder gross weight 60wt%, ball milling 5 hours; When preparing the ceramic powder of 70nm～100nm, add the NaCl that accounts for described powder gross weight 50wt%, ball milling 4 hours; When preparing the ceramic powder of 100nm～150nm, add the NaCl that accounts for described powder gross weight 40wt%, ball milling 3 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02159005 CN1247485C (en) | 2002-12-27 | 2002-12-27 | Method for preparing TiC micro nano ceramic powder via refinery coke salt bath synthesis |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02159005 CN1247485C (en) | 2002-12-27 | 2002-12-27 | Method for preparing TiC micro nano ceramic powder via refinery coke salt bath synthesis |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1511803A CN1511803A (en) | 2004-07-14 |
| CN1247485C true CN1247485C (en) | 2006-03-29 |
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| CN 02159005 Expired - Fee Related CN1247485C (en) | 2002-12-27 | 2002-12-27 | Method for preparing TiC micro nano ceramic powder via refinery coke salt bath synthesis |
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102153347B (en) * | 2011-01-21 | 2013-03-20 | 武汉理工大学 | Method for quickly synthesizing Ti3SiC2 submicron powder |
| CN102241514B (en) * | 2011-05-24 | 2014-05-14 | 武汉理工大学 | Method for synthetizing Ti3SiC2 high-purity powder |
| DE102017006658A1 (en) * | 2017-07-13 | 2019-01-17 | Forschungszentrum Jülich GmbH | Process for the preparation of non-oxide, ceramic powders |
| CN111039291A (en) * | 2018-10-12 | 2020-04-21 | 中国科学院金属研究所 | Method for preparing NbC and/or TaC powder in situ by molten salt disproportionation reaction |
| CN111039675A (en) * | 2018-10-12 | 2020-04-21 | 中国科学院金属研究所 | In-situ preparation of Cr by molten salt3C2And/or Mo2Method for preparing C powder |
| CN111039290A (en) * | 2018-10-12 | 2020-04-21 | 中国科学院金属研究所 | Method for preparing transition metal carbide powder in situ by molten salt disproportionation reaction |
| CN109881210B (en) * | 2019-03-13 | 2020-09-22 | 东北大学 | Method for preparing transition metal carbide powder by electric field and/or ultrasonic field reinforcement |
| CN113200547A (en) * | 2021-05-24 | 2021-08-03 | 兰州理工大学 | Preparation method of nanoscale TiC powder with controllable macro-particle size |
| CN115043403A (en) * | 2022-06-14 | 2022-09-13 | 成都先进金属材料产业技术研究院股份有限公司 | Preparation method of titanium carbide superfine powder |
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2002
- 2002-12-27 CN CN 02159005 patent/CN1247485C/en not_active Expired - Fee Related
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