CN1268578C - Method for preparing micronanometer ceramic powder using salt bath synthesis method - Google Patents

Method for preparing micronanometer ceramic powder using salt bath synthesis method Download PDF

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CN1268578C
CN1268578C CN 02123995 CN02123995A CN1268578C CN 1268578 C CN1268578 C CN 1268578C CN 02123995 CN02123995 CN 02123995 CN 02123995 A CN02123995 A CN 02123995A CN 1268578 C CN1268578 C CN 1268578C
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powder
salt
ceramic powder
base substrate
composite
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CN1467175A (en
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崔立山
赵金龙
高万夫
郑雁军
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China University of Petroleum Beijing
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China University of Petroleum Beijing
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Abstract

The present invention discloses a method for preparing micronanometer ceramic powder by a salt bath synthesis method. The present invention comprises the main technological processes: Ti+C powder lot or TiO2+C powder lot or 10Al+3TiO2+3B2O3 powder lot or 4Al+3TiO2+3C powder lot of which the particle size is from 100 meshes to 200 meshes is taken according to stoichiometric amount; compound salt which accounts for 20 to 80 wt% of the gross weight of the powder lot is added, and NaCl and KCl of the compound salt respectively account for 50 wt%; the compound salt is filled in a stainless steel tank of a ball mill; the rotating speed of the ball mill is controlled to be at 200 circle per minute, the ball-to-powder weight ratio is 25:1, and the ball milling time is from 4 to 10 hours. The powder lot is pressed into a green body and is put in compound molten salt of 700 DEG C to 1000 DEG C to keep heat preservation for 20 minutes, and NaCl and KCl respectively account for 50 wt%; after the green body is cooled, TiC or 5Al2O3+3TiB2 or 2Al2O3+3TiC ceramic powder of which the size is from 20 nm to 200 nm is prepared by desalting. The present invention has the main characteristics of simple technology, low cost, purified product, little investment and mature technology; besides the present invention can be popularized for use.

Description

A kind of method of utilizing the salt bath synthesis method to prepare micro-nano ceramic powder
The invention belongs to field of ceramic material preparation, relate to TiC and 5Al 2O 3+ 3TiB 2And 2Al 2O 3The micro-nano ceramic powder material preparation of+3TiC.
Size range presents many attributes that are different from oversize material at the micro-nano pottery of 1～100nm, is described as cross-centennial novel material.Micro-nano pottery can be applied to multiple industries such as chemical industry, pottery, electromagnetism, optics, superconduction, biomedicine, dyestuff, agricultural, the hot fields of the current Materials science research of micro-nano pottery preparation having become.
The main method of the micro-nano ceramic powder of prior art for preparing TiC is: adopt Ti powder and graphite C synthetic TiC pottery under 3200K, perhaps adopt 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; Preparation TiB 2The main method of micro-nano ceramic powder is: utilize high-temperature synthesis to prepare TiB 2Be equipped with ultrafine powder with the mechanical ball milling legal system subsequently.
Prior art for preparing Al 2O 3Two kinds of main method of micro-nano ceramic powder are: (1) mechanical ball milling method, (2) sol-gel processing.The mechanical ball milling legal system is equipped with Al 2O 3Though micro-nano ceramic powder equipment cost is low, technology is simple, the general ball milling time, the material of preparation was seriously polluted in mechanical milling process more than 20～40 hours, and product is impure, and ceramic powder is refine to below the 100nm.
Adopt prior art directly to prepare Al 2O 3+ TiB 2And Al 2O 3That is that all right is ripe for the technology of+TiC composite micro-nano rice ceramic powder material, and not seeing has the report of commercially producing.
In sum, prior art for preparing TiC and TiB 2The shortcoming of micro-nano ceramic powder material is: temperature height, complex process, the mechanical ball milling legal system is equipped with Al 2O 3The shortcoming of micro-nano ceramic powder is: the ball milling time is long, product is impure, ceramic powder is refine to below the 100nm.
In order to overcome the above-mentioned deficiency of prior art, and prepare processing method is simple, cost is low TiC and 5Al 2O 3+ 3TiB 2And 2Al 2O 3The micro-nano ceramic powder of+3TiC, special proposition technical solution of the present invention.
Basic design of the present invention is, according to Ti+C, TiO 2+ C, 10Al+3TiO 2+ 3B 2O 3And 4Al+3TiO 2Chemical reaction at high temperature can take place and emit a large amount of heat in+3C, and generates corresponding TiC and 5Al 2O 3+ 3TiB 2And 2Al 2O 3The characteristics of+3TiC stupalith, in the ball milling ma process, along with the prolongation of time, the powder particle diminishes, specific surface area increases, the active raising; The adding of composite salt makes the powder particle fully disperse in the ball milling ma process, is easy to form micro-nano size ceramic powder when carrying out chemical reaction in high temperature composite 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 the salt bath synthesis method to prepare micro-nano ceramic powder that the present invention is designed is characterized in that: getting granularity by stoichiometry is 100 orders～200 purpose Ti+C powder or TiO 2+ C powder or 10Al+3TiO 2+ 3B 2O 3Powder or 4Al+3TiO 2+ 3C powder, add and to account for the NaCl of powder gross weight 20～80wt% and composite salt that KCl respectively accounts for 50wt% is made base substrate, base substrate is put into the composite molten salt that 700 ℃～1000 ℃ NaCl and KCl respectively account for 50wt%, be incubated 20 minutes, chemical reaction takes place in powder in fused salt, through desalinating process, prepare TiC or the 5Al of size after the cooling at 20nm～200nm 2O 3+ 3TiB 2Or 2Al 2O 3+ 3TiC ceramic powder.
A kind of method of utilizing the salt bath synthesis method to prepare micro-nano ceramic powder that the present invention is designed, it is further characterized in that, the body preparation method is: after the composite salt of powder adding 20～80%, pack in the ball mill stainless steel cylinder of steel, ratio of grinding media to material is 25: 1, and ball grinder is evacuated to 0.133～1.333Pa (10 -2～10 -3Torr) and charge into argon gas, argon pressure is 0.9～1.2 * 10 5(0.9～1.2atm) scope, drum's speed of rotation are controlled at 200 rev/mins to Pa, and ball milling 4～10 hours is pressed into base substrate under 3MPa pressure; The desalinating process process is: the water that the composite 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 composite salt 100% incorporates in the water, filtered out ceramic powder; The control method of ceramic powder size is: when preparing the ceramic powder of 20nm, add the composite salt that accounts for reactant gross weight 80wt%, ball milling 10 hours is when preparing the ceramic powder of 50nm, add the composite salt that accounts for reactant gross weight 60wt%, ball milling 8 hours when preparing the ceramic powder of 100nm, adds the composite salt that accounts for reactant gross weight 40wt%, ball milling 6 hours, when preparing the ceramic powder of 200nm, add the composite salt that accounts for reactant gross weight 20wt%, ball milling 4 hours; The system of selection of 700 ℃～1000 ℃ composite fused salt temperature is: 10Al+3TiO 2+ 3B 2O 3The base substrate of powder preparation is put into 700 ℃ melting salt; The base substrate of Ti+C powder preparation is put into 800 ℃ melting salt; 4Al+3TiO 2The base substrate of+3C powder preparation is put into 900 ℃ melting salt; TiO 2The base substrate of+C powder preparation is put into 1000 ℃ melting salt.
Compared with prior art, major advantage of the present invention is: (1) technology is simple, and (2) cost is low.
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 micro-nano ceramic powder of the TiC of 200nm
Get 100 orders～200 purpose Ti powder and each 24 gram of C powder and 6 grams at 1: 1 by the atom proportioning, 30g altogether prepares burden; Add 6 gram NaCl and KCl and respectively account for the composite salt of 50wt%, put into ball mill stainless steel cylinder of steel after the mixing, with cylinder of steel with seal with elastometic washer after, be evacuated to 1.333Pa (10 -2Torr), charge into argon gas, pressure is 0.9 * 10 5Pa (0.9atm), ratio of grinding media to material is 25: 1, the control drum's speed of rotation is that 200 rev/mins of ball millings are after 4 hours, be pressed into the base substrate of φ 30mm under the axle pressure with 3MPa in mould, base substrate is put into 800 ℃ the fusion composite salt insulation 20 minutes that NaCl and KCl respectively account for 50wt%, the water of the composite salt that is loaded with the micro-nano ceramic powder of TiC after the reaction cooling being put into 5 times of salt weight soaked 15 hours, after composite 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, and the micro-nano ceramic powder granularity of TiC is 200nm after measured.
Embodiment 2:
Prepare main size-grade distribution at the micro-nano ceramic powder of the TiC of 100nm
Getting granularity by stoichiometry is 100 orders～200 purpose TiO 2+ C powder, TiO 2Each 40 gram of powder and C powder and 6 grams, 46g altogether prepares burden; Add 18.4 gram NaCl and KCl and respectively account for the composite salt of 50wt%, put into ball mill stainless steel cylinder of steel after the mixing, with cylinder of steel with seal with elastometic washer after, be evacuated to 0.133Pa (10 -3Torr), charge into argon gas, pressure is 1.1 * 10 5Pa (1.1atm), ratio of grinding media to material is 25: 1, the control drum's speed of rotation is that 200 rev/mins of ball millings are after 6 hours, be pressed into the base substrate of φ 30mm under the axle pressure with 3MPa in mould, base substrate is put into 900 ℃ the fusion composite salt insulation 20 minutes that NaCl and KCl respectively account for 50wt%, the water of the composite salt that is loaded with the micro-nano ceramic powder of TiC after the reaction cooling being put into 5 times of salt weight soaked 13 hours, after composite 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, and the micro-nano ceramic powder granularity of TiC is 100nm after measured.
Embodiment 3:
Prepare the 5Al of main size-grade distribution at 50nm 2O 3+ 3TiB 2Micro-nano ceramic powder
Getting granularity by stoichiometry is 100 orders～200 purpose 10Al+3TiO 2+ 3B 2O 3Powder, Al powder, TiO 2Powder and B 2O 3Powder is respectively 18 grams, 16 grams and 14 grams, and 48g altogether prepares burden; Add 28.8 gram NaCl and KCl and respectively account for the composite salt of 50wt%, put into ball mill stainless steel cylinder of steel after the mixing, with cylinder of steel with seal with elastometic washer after, be evacuated to 1.333Pa (10 -2Torr), charge into argon gas, pressure is 1.2 * 10 5Pa (1.2atm), ratio of grinding media to material is 25: 1, the control drum's speed of rotation is that 200 rev/mins of ball millings are after 8 hours, be pressed into the base substrate of φ 30mm under the axle pressure with 3MPa in mould, base substrate is put into 700 ℃ the fusion composite salt insulation 20 minutes that NaCl and KCl respectively account for 50wt%, will react and be loaded with 5Al after cooling off 2O 3+ 3TiB 2The water that the composite salt of micro-nano ceramic powder is put into 5 times of salt weight soaked 10 hours, after composite salt 100% incorporates in the water, filtered out 5Al 2O 3+ 3TiB 2Micro-nano ceramic powder is with 5Al 2O 3+ 3TiB 2Powder washes back oven dry, 5Al after measured repeatedly with deionized water 2O 3+ 3TiB 2Micro-nano ceramic powder granularity is 50nm.
Embodiment 4:
Prepare the 2Al of main size-grade distribution at 20nm 2O 3The micro-nano ceramic powder of+3TiC
Getting granularity by stoichiometry is 100 orders～200 purpose 4Al+3TiO 2+ 3C powder, Al powder, TiO 2Powder and C powder are respectively 10.8 grams, 24 grams and 3.6 grams, and 38.4g altogether prepares burden; Add 30.72 gram NaCl and KCl and respectively account for the composite salt of 50wt%, put into ball mill stainless steel cylinder of steel after the mixing, with cylinder of steel with seal with elastometic washer after, be evacuated to 1.333Pa (10 -2Torr), charge into argon gas, pressure is 1.O * 10 5Pa (1.0atm), ratio of grinding media to material is 25: 1, the control drum's speed of rotation is that 200 rev/mins of ball millings are after 10 hours, be pressed into the base substrate of φ 30mm under the axle pressure with 3MPa in mould, base substrate is put into 1000 ℃ the fusion composite salt insulation 20 minutes that NaCl and KCl respectively account for 50wt%, will react and be loaded with 2Al after cooling off 2O 3The water that the composite salt of the micro-nano ceramic powder of+3TiC is put into 5 times of salt weight soaked 12 hours, after composite salt 100% incorporates in the water, filtered out 2Al 2O 3The micro-nano ceramic powder of+3TiC is with 2Al 2O 3+ 3TiC powder washes back oven dry, 2Al after measured repeatedly with deionized water 2O 3The micro-nano ceramic powder granularity of+3TiC is 20nm.

Claims (5)

1, a kind of method of utilizing the salt bath synthesis method to prepare micro-nano ceramic powder comprises body preparation and desalinating process process, it is characterized in that: getting granularity by stoichiometry is 100 orders～200 purpose Ti+C powder or TiO 2+ C powder or 10Al+3TiO 2+ 3B 2O 3Powder or 4Al+3TiO 2+ 3C powder, add and to account for the NaCl of powder gross weight 20～80wt% and composite salt that KCl respectively accounts for 50wt% is made base substrate, base substrate is put into the composite molten salt that 700 ℃～1000 ℃ NaCl and KCl respectively account for 50wt%, be incubated 20 minutes, chemical reaction takes place in powder in fused salt, through desalinating process, prepare TiC or the 5Al of size after the cooling at 20nm～200nm 2O 3+ 3TiB 2Or 2Al 2O 3+ 3TiC ceramic powder.
2, a kind of method of utilizing the salt bath synthesis method to prepare micro-nano ceramic powder according to claim 1, it is characterized in that, the preparation method of base substrate is: after powder adds the composite salt of 20～80wt%, pack in the ball mill stainless steel cylinder of steel, ratio of grinding media to material is 25: 1, and ball grinder is evacuated to 0.133～1.333Pa (10 -2～10 -3Torr) and charge into argon gas, argon pressure is 0.9～1.2 * 10 5(0.9～1.2atm) scope, drum's speed of rotation are controlled at 200 rev/mins to Pa, and ball milling 4～10 hours is pressed into base substrate under 3MPa pressure.
3, a kind of method of utilizing the salt bath synthesis method to prepare micro-nano ceramic powder according to claim 1, it is characterized in that, the desalinating process process is: the water that the composite 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 composite salt 100% incorporates in the water, filter out 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 ceramic powder size is: when preparing the ceramic powder of 20nm, add the composite salt that accounts for reactant gross weight 80wt%, ball milling 10 hours; When preparing the ceramic powder of 50nm, add the composite salt that accounts for reactant gross weight 60wt%, ball milling 8 hours; When preparing the ceramic powder of 100nm, add the composite salt that accounts for reactant gross weight 40wt%, ball milling 6 hours; When preparing the ceramic powder of 200nm, add the composite salt that accounts for reactant gross weight 20wt%, ball milling 4 hours.
5, a kind of method of utilizing the salt bath synthesis method to prepare micro-nano ceramic powder according to claim 1 and 2 is characterized in that, the system of selection of 700 ℃～1000 ℃ composite fused salt temperature is: 10Al+3TiO 2+ 3B 2O 3The base substrate of powder preparation is put into 700 ℃ melting salt; The base substrate of Ti+C powder preparation is put into 800 ℃ melting salt; 4Al+3TiO 2The base substrate of+3C powder preparation is put into 900 ℃ melting salt; TiO 2The base substrate of+C powder preparation is put into 1000 ℃ melting salt.
CN 02123995 2002-07-12 2002-07-12 Method for preparing micronanometer ceramic powder using salt bath synthesis method Expired - Fee Related CN1268578C (en)

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CN102910910B (en) * 2012-11-16 2014-03-26 四川理工学院 Method for preparing micro-nano titanium carbonitride powder with controllable carbon-nitrogen ratio by adopting solid state nitrogen source
CN103979538B (en) * 2014-05-30 2015-09-30 四川理工学院 A kind of method preparing micro-nano TiC/TiSi2 composite granule
CN114394834A (en) * 2022-02-22 2022-04-26 中硼科技(威海)有限公司 Preparation method of boron carbide-based nano composite powder
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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