CN1271001C - Method for preparing micronanometer metal-ceramic composite powder using salt bath synthesis method - Google Patents

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

Info

Publication number
CN1271001C
CN1271001C CN 02123994 CN02123994A CN1271001C CN 1271001 C CN1271001 C CN 1271001C CN 02123994 CN02123994 CN 02123994 CN 02123994 A CN02123994 A CN 02123994A CN 1271001 C CN1271001 C CN 1271001C
Authority
CN
China
Prior art keywords
powder
salt
composite
ceramic composite
base substrate
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Fee Related
Application number
CN 02123994
Other languages
Chinese (zh)
Other versions
CN1467173A (en
Inventor
崔立山
赵金龙
高万夫
郑雁军
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
China University of Petroleum Beijing
Original Assignee
China University of Petroleum Beijing
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by China University of Petroleum Beijing filed Critical China University of Petroleum Beijing
Priority to CN 02123994 priority Critical patent/CN1271001C/en
Publication of CN1467173A publication Critical patent/CN1467173A/en
Application granted granted Critical
Publication of CN1271001C publication Critical patent/CN1271001C/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

Links

Landscapes

  • Compositions Of Oxide Ceramics (AREA)

Abstract

The present invention discloses a method for preparing micro-nano metal ceramic composite powder by a salt bath synthesis method. The present invention comprises the main technological processes: 3Fe3O4+8Al or Cr2O3+2Al or 3TiO2+4Al 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; vacuum pumping operation is carried out to a ball milling tank to 10<-2> torr to 10<-3> torr, and argon gas is inflated; argon gas pressure is within the range of 0.9 to 1.2 atm; the rotating speed of the ball mill is controlled 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 under the pressure of 3MPa and is put into compound molten salt of 700 DEG C to 900 DEG C to keep for 20 minutes, wherein NaCl and KCl of the compound molten salt respectively account for 50 wt%; the powder lot of the green body has a chemical reaction in the molten salt; after the green body is cooled, 4Al2O3+9Fe of Al2O3+2Cr or 2Al2O3+3Ti metal ceramic composite powder which has the size of 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 metal ceramic composite powder
The invention belongs to field of ceramic material preparation, relate to 4Al 2O 3+ 9Fe, Al 2O 3+ 2Cr and 2Al 2O 3The preparation of+3Ti metal ceramic composite powder material.
Its technical background is that 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.
One of main method of prior art for preparing Fe, Cr and Ti powder is the metal melt vacuum condensation method, its concrete technology be under high vacuum with raw materials evaporate, control size of particles by control fluid velocity and velocity of evaporation.Characteristics are to obtain highly purified product, but its throughput is lower, and only are suitable for the particle of preparation size less than 20nm, and technical equipment requires high.
Prior art prepares Al 2O 3Two kinds of main method of micro-nano ceramic powder are: (1) mechanical ball-milling method, (2) sol-gel processing.The standby Al of machinery ball milling legal system 2O 3Although micro-nano ceramic powder equipment cost is low, technology is simple, general Ball-milling Time is more than 20～40 hours, and the material of preparation is seriously polluted in mechanical milling process, and product is impure, generally can't make Al 2O 3Micro-nano ceramic powder refine to below the 100nm.
In sum, the shortcoming that prior art prepares Fe, Cr and Ti powder is: production capacity is low, complex process, and technical equipment requires high; The standby Al of prior art machinery ball milling legal system 2O 3The shortcoming of micro-nano ceramic powder is: material contamination is serious, generally can not reach micro-nano granularity.In order to overcome the above-mentioned deficiency of prior art, and prepare the 4Al that process is simple, cost is low 2O 3+ 9Fe, Al 2O 3+ 2Cr and 2Al 2O 3+ 3Ti metal ceramic composite powder, special proposition technical solution of the present invention.
Basic conception of the present invention is, according to 3Fe 3O 4+ 8Al, Cr 2O 3+ 2Al and 3TiO 2Chemical reaction at high temperature can take place and emit a large amount of heat in+4Al, and generates corresponding 4Al 2O 3+ 9Fe, Al 2O 3+ 2Cr and 2Al 2O 3The characteristics of+3Ti metal ceramic composite powder material, in the mechanical mill alloying process, along with the prolongation of time, the powder particle diminishes, specific area increases, the active raising; The adding of complex salt is easy to form the micro-or nano size ceramic powder so that the powder particle fully disperses when carrying out chemical reaction in high temperature complex salt subsequently in the mechanical mill alloying process; The high temperature complex 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 synthetic method to prepare micro-nano metal ceramic composite powder that the present invention is designed is characterized in that: getting granularity by stoichiometry is 100 orders～200 purpose 3Fe 3O 4+ 8Al powder or Cr 2O 3+ 2Al powder or 3TiO 2+ 4Al powder, add and to account for the NaCl of powder gross weight 20～80wt% and complex salt that KCl respectively accounts for 50wt% is made base substrate, base substrate is put into the composite molten salt that 700 ℃～900 ℃ NaCl and KCl respectively account for 50wt%, be incubated 20 minutes, chemical reaction takes place in powder in the base substrate in fused salt, through desalinating process, prepare size at the 4Al of 20nm～200nm after the cooling 2O 3+ 9Fe or Al 2O 3+ 2Cr or 2Al 2O 3+ 3Ti metal ceramic composite powder.
A kind of method of utilizing the salt bath synthesis method to prepare micro-nano metal ceramic composite 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 -3～10 -2Torr) 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 under 3MPa pressure; The desalinating process process is: will react the composite salt that is loaded with ceramic powder after the cooling and put into the water of 5 times of salt weight and soaked 10～15 hours, and after composite salt 100% incorporates in the water, filter out ceramic powder; The control method of metal ceramic composite 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 ℃～900 ℃ composite fused salt temperature is: 3Fe 3O 4The base substrate of+8Al powder preparation is put into 700 ℃ melting salt; Cr 2O 3The base substrate of+2Al powder preparation is put into 800 ℃ melting salt; 3TiO 2The base substrate of+4Al powder preparation is put into 900 ℃ 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 distribution at the 4Al of 200nm 2O 3The micro-nano metal ceramic composite powder of+9Fe
Getting granularity by stoichiometry is 100 orders～200 purpose 3Fe 3O 4+ 8Al powder, Fe 3O 4Each 34.8 gram of powder and Al powder and 10.8 grams, 45.6g altogether prepares burden; Add 9.12 gram NaCl and KCl and respectively account for the complex 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), be filled with 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 axial compressive force with 3MPa in mould, base substrate is put into 700 ℃ the melting complex salt insulation 20 minutes that NaCl and KCl respectively account for 50wt%, will react and be loaded with 4Al after cooling off 2O 3The water that the complex salt of the micro-nano metal ceramic composite powder of+9Fe is put into 5 times of salt weight soaked 15 hours, after complex salt 100% incorporates in the water, filtered out 4Al 2O 3+ 9Fe washes post-drying, after measured 4Al repeatedly with deionized water 2O 3The micro-nano metal ceramic composite powder granularity of+9Fe is 200nm.
Embodiment 2:
Prepare main size distribution at the Al of 100nm 2O 3The micro-nano metal ceramic composite powder of+2Cr
Getting granularity by stoichiometry is 100 orders～200 purpose Cr 2O 3+ 2Al powder, Cr 2O 3Each 15.2 gram of powder and Al powder and 5.4 grams, 20.6g altogether prepares burden; Add 8.24 gram NaCl and KCl and respectively account for the complex 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), be filled with 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 axial compressive force with 3MPa in mould, base substrate is put into 800 ℃ the melting complex salt insulation 20 minutes that NaCl and KCl respectively account for 50wt%, will react and be loaded with Al after cooling off 2O 3The water that the complex salt of the micro-nano metal ceramic composite powder of+2Cr is put into 5 times of salt weight soaked 13 hours, after complex salt 100% incorporates in the water, filtered out Al 2O 3+ 2Cr washes post-drying, after measured Al repeatedly with deionized water 2O 3The micro-nano metal ceramic composite powder granularity of+2Cr is 100nm.
Embodiment 3:
Prepare main size distribution at the 2Al of 50nm 2O 3The micro-nano metal ceramic composite powder of+3Ti
Getting granularity by stoichiometry is 100 orders～200 purpose 3TiO 2+ 4Al powder, TiO 2Powder and Al powder are respectively 24.0 grams and 14.4 grams, and 38.4g altogether prepares burden; Add 23.04 gram NaCl and KCl and respectively account for the complex 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), be filled with 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 axial compressive force with 3MPa in mould, base substrate is put into 900 ℃ the melting complex 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 complex salt of the micro-nano metal ceramic composite powder of+3Ti is put into 5 times of salt weight soaked 10 hours, after complex salt 100% incorporates in the water, filtered out 2Al 2O 3+ 3Ti washes post-drying, after measured 2Al repeatedly with deionized water 2O 3The micro-nano metal ceramic composite powder granularity of+3Ti is 50nm.
Embodiment 4:
Prepare main size distribution at the 4Al of 20nm 2O 3The micro-nano metal ceramic composite powder of+9Fe
Getting granularity by stoichiometry is 100 orders～200 purpose 3Fe 3O 4+ 8Al powder, Fe 3O 4Each 34.8 gram of powder and Al powder and 10.8 grams, 45.6g altogether prepares burden; Add 36.48 gram NaCl and KCl and respectively account for the complex 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), be filled with argon gas, pressure is 1.0 * 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 axial compressive force with 3MPa in mould, base substrate is put into 700 ℃ the melting complex salt insulation 20 minutes that NaCl and KCl respectively account for 50wt%, will react and be loaded with 4Al after cooling off 2O 3The water that the complex salt of the micro-nano metal ceramic composite powder of+9Fe is put into 5 times of salt weight soaked 12 hours, after complex salt 100% incorporates in the water, filtered out 4Al 2O 3+ 9Fe washes post-drying, after measured 4Al repeatedly with deionized water 2O 3The micro-nano metal ceramic composite powder granularity of+9Fe is 20nm.

Claims (5)

1, a kind of method of utilizing the salt bath synthetic method to prepare micro-nano metal ceramic composite powder comprises body preparation and desalinating process process, it is characterized in that: getting granularity by stoichiometry is 100 orders～200 purpose 3Fe 3O 4+ 8Al powder or Cr 2O 3+ 2Al powder or 3TiO 2+ 4Al powder, add and to account for the NaCl of powder gross weight 20～80wt% and complex salt that KCl respectively accounts for 50wt% is made base substrate, base substrate is put into the composite molten salt that 700 ℃～900 ℃ NaCl and KCl respectively account for 50wt%, be incubated 20 minutes, chemical reaction takes place in powder in the base substrate in fused salt, through desalinating process, prepare size at the 4Al of 20nm～200nm after the cooling 2O 3+ 9Fe or Al 2O 3+ 2Cr or 2Al 2O 3+ 3Ti metal ceramic composite powder.
2, a kind of method of utilizing the salt bath synthesis method to prepare micro-nano metal ceramic composite 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 -3～10 -2Torr) 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 under 3MPa pressure.
3, a kind of method of utilizing the salt bath synthesis method to prepare micro-nano metal ceramic composite powder according to claim 1, it is characterized in that, the desalinating process process is: will react the composite salt that is loaded with ceramic powder after the cooling and put into the water of 5 times of salt weight and 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 metal ceramic composite powder according to claim 1 and 2, it is characterized in that, the control method of metal ceramic composite 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 synthetic method to prepare micro-nano metal-ceramic composite powder according to claim 1 and 2 is characterized in that, the system of selection of 700 ℃～900 ℃ composite fused salt temperature is: 3Fe 3O 4The base substrate of+8Al preparation is put into 700 ℃ fuse salt; Cr 2O 3The base substrate of+2Al preparation is put into 800 ℃ fuse salt; 3TiO 2The base substrate of+4Al preparation is put into 900 ℃ fuse salt.
CN 02123994 2002-07-12 2002-07-12 Method for preparing micronanometer metal-ceramic composite powder using salt bath synthesis method Expired - Fee Related CN1271001C (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN 02123994 CN1271001C (en) 2002-07-12 2002-07-12 Method for preparing micronanometer metal-ceramic composite powder using salt bath synthesis method

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN 02123994 CN1271001C (en) 2002-07-12 2002-07-12 Method for preparing micronanometer metal-ceramic composite powder using salt bath synthesis method

Publications (2)

Publication Number Publication Date
CN1467173A CN1467173A (en) 2004-01-14
CN1271001C true CN1271001C (en) 2006-08-23

Family

ID=34142590

Family Applications (1)

Application Number Title Priority Date Filing Date
CN 02123994 Expired - Fee Related CN1271001C (en) 2002-07-12 2002-07-12 Method for preparing micronanometer metal-ceramic composite powder using salt bath synthesis method

Country Status (1)

Country Link
CN (1) CN1271001C (en)

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1314625C (en) * 2005-12-27 2007-05-09 武汉理工大学 Method for synthesizing multi-element, inorganic compound ceramic uniformed powder
CN100347128C (en) * 2006-06-16 2007-11-07 北京工业大学 Molten salt method for synthesizing micropowder body of potass bismuth titanate of piezoelectric ceramics without lead
CN106735256B (en) * 2016-12-05 2019-01-29 四川理工学院 A kind of Ni nanoparticle-Zn powder and preparation method thereof

Also Published As

Publication number Publication date
CN1467173A (en) 2004-01-14

Similar Documents

Publication Publication Date Title
Zhao et al. Microstructure and properties of laser cladded B4C/TiC/Ni-based composite coating
KR100747805B1 (en) Powder mixture or composite powder, a method for production thereof and the use thereof in composite materials
CN105018927B (en) Method for preparing Ti (C, N) -containing coating by taking melamine as carbon-nitrogen precursor
CN107935596A (en) One kind prepares MAX phase ceramics Ti using molten-salt growth method low-temperature sintering3AlC2The method of powder
CN1858001A (en) Method for preparing different shape zinc oxide by vacuum limit oxygen method
CN101812684A (en) Method for preparing metal surface laser strengthened coat
CN1271001C (en) Method for preparing micronanometer metal-ceramic composite powder using salt bath synthesis method
CN113816379A (en) Preparation method of nano hafnium boride powder
CN108164267A (en) A kind of preparation method of multicomponent nanocrystalline metal boride
CN104418383A (en) Improvement method for removing impurities in titanium tetrachloride by virtue of aluminum powder
CN1268578C (en) Method for preparing micronanometer ceramic powder using salt bath synthesis method
CN105821272B (en) A kind of wear-resistant molybdenum alloy material cut and preparation method thereof
CN1167831C (en) Laser melten inter metallic compounds/ceramic composite coatings and preparation thereof
CN1258009C (en) ZnO nano crystal whisker material and its preparing method
CN114875291B (en) High-entropy alloy powder and preparation method thereof, and high-entropy alloy laser cladding layer and preparation method thereof
CN102583515A (en) Method for preparing CaTiO3 composite material from slow-cooling titanium-bearing blast furnace slag
CN1467176A (en) Method for preparing micronanometer NiTi, NiAl powder using salt bath synthesis method
CN112342450B (en) Production process of high-refractive-index coating mixed material
CN103360074A (en) Preparation method for WC-Al2O3 nanometer composite material
JP3165875B2 (en) Method for producing flaky titanium dioxide
Wei et al. Thick (AlTiCrNbTa) O2 high-entropy ceramic coating: Efficient fabrication and characterization
Mashaal Preparation of Insoluble Zirconate from Egyptian Zircon via Alkali Fusion Process to Enhancement Al Alloy Performance
CN114058895B (en) Double nozzle spray forming Y 2 O 3 Process for particle reinforced Monel 400 alloy plate
CN1462732A (en) Method for preparing composite powder of ceramics with bionics structure
CN1035198C (en) Titanium carbonitride-dimolybdenum carbide-nickel-nickel-zirconium chemical compound-yttrium oxide system material and its preparation method

Legal Events

Date Code Title Description
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant
C57 Notification of unclear or unknown address
DD01 Delivery of document by public notice

Addressee: Zhao Jinlong

Document name: Notification of Termination of Patent Right

C19 Lapse of patent right due to non-payment of the annual fee
CF01 Termination of patent right due to non-payment of annual fee