CN1394707A - Method for preparing intermetallic compound powder and its equipment - Google Patents

Method for preparing intermetallic compound powder and its equipment Download PDF

Info

Publication number
CN1394707A
CN1394707A CN 02114332 CN02114332A CN1394707A CN 1394707 A CN1394707 A CN 1394707A CN 02114332 CN02114332 CN 02114332 CN 02114332 A CN02114332 A CN 02114332A CN 1394707 A CN1394707 A CN 1394707A
Authority
CN
China
Prior art keywords
ball
intermetallic compound
compound powder
abrading
grinding cylinder
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.)
Granted
Application number
CN 02114332
Other languages
Chinese (zh)
Other versions
CN1189276C (en
Inventor
陈振华
陈鼎
陈刚
严红革
龙小兵
常龙
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.)
Hunan University
Original Assignee
Hunan University
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 Hunan University filed Critical Hunan University
Priority to CNB021143323A priority Critical patent/CN1189276C/en
Publication of CN1394707A publication Critical patent/CN1394707A/en
Application granted granted Critical
Publication of CN1189276C publication Critical patent/CN1189276C/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

Links

Images

Landscapes

  • Powder Metallurgy (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
  • Crushing And Grinding (AREA)

Abstract

The preparation method of intermetallic compound powder includes the following steps: adopting high-temp. liquid ball grinding equipment and ball-grinding molten metal at high-temp. to prepare intermetallic compound powder of two components of grinding ball and molten metal. The equipment for preparing intermetallic compound powder includes ball grinding cylinder, reducer and speed regulating motor. The exterior of the described ball grinding cylinder is equipped with a heating device on which a temp. control instrument and temp.-measuring element are mounted. The described heating device is an electric resistance furnace in which the ball-grinding cylinder is placed, and the described temp.-measuring element is a thermoelectric couple.

Description

The method and the device thereof that prepare intermetallic compound powder
Technical field the present invention relates to a kind of preparation method and device thereof of intermetallic compound powder.
The background technology intermetallic compound is a kind of one kind of low density, dystectic ordered structure compound between between metal and pottery.Because structural characteristics make it have the unexistent special performance of other traditional material.As structural material applications, have characteristics such as specific modulus height, specific strength height, anti-oxidant, high temperature resistant and corrosion-resistant excellence; Use as functional material, in electricity, magnetics, have some excellent performances especially, and stability is fine.The application prospects that intermetallic compound has, become the focus of American and Britain, day and China's material circle scholar's research in recent decades, how to have prepared the basis that compound promptly becomes intermetallic compound research and uses between various high-performance metals effectively.
Because most intermetallic compounds have the room temperature fragility of intrinsic, so obtain that compound-material generally all is to adopt to prepare compound powder between high-performance metal earlier between the high-performance metal of some specific uses, and then, perhaps directly use as requested with powder compacting.This powder adopts traditional fusion casting or powder metallurgic method to be difficult to preparation.
The technology of preparation intermetallic compound powder mainly contains rapid solidification at present, spreads certainly and mechanical alloying.Preceding two kinds of process energy consumption height, complex process, and the intermetallic compound powder system that can prepare is very limited; Mechanical alloying is comparatively effective a kind of method, have that technology is simple, output is than advantages such as height, the principle of this method is that two or more solid state powder is carried out long-time ball milling or grinding at normal temperatures, make fragmentation repeatedly between solid state powder, cold welding, broken again, finally reach the diffusion of atomic scale and realize alloying, its abrading-ball material generally has chromium steel, stainless steel, carbide alloy, pottery etc., abrading-ball does not participate in reaction in the mechanical milling process, main technologic parameters has ball grinding cylinder rotating speed, ratio of grinding media to material, ball milling time etc., and mechanical milling process is at room temperature to carry out.The major defect of this method is consuming time longer, the energy consumption height, abrading-ball becomes pollution sources easily, and product scope has certain limitation (also finding no intermetallic compound when as present ball milling Ti-Al being generates mutually), particularly can not prepare compound between high-temperature metal.
Summary of the invention the objective of the invention is to overcome the deficiencies in the prior art, a kind of novel method for preparing intermetallic compound powder and device thereof are provided, its equipment and simple to operate, with low cost, technology and product are formed controlled, the intermetallic compound powder that can prepare the difference composition of various alloy systems, especially can prepare compound between the high-temperature metal that other method is difficult to prepare, enrich the product category of intermetallic compound, prepared powder can reach nanoscale structures.
The present invention solves the problems of the technologies described above by the following technical solutions:
The method for preparing intermetallic compound powder of the present invention is characterized in that: adopt the high-temperature liquid state ball mill device, at high temperature, motlten metal is carried out ball milling, produce the intermetallic compound powder of abrading-ball and motlten metal two constituent elements.
Described ball milling temperature is regulated between 200 ℃~1400 ℃, the ball milling time is 6~120 hours, ratio of grinding media to material is 6~30: 1, the ball grinding cylinder rotating speed is 50~110 rev/mins, abrading-ball is one of raw material, under different temperatures, producing with abrading-ball and motlten metal is the intermetallic compound powder of a series of different compositions of constituent element.Its processing step is: (1) puts into the solid metallic raw material in ball grinding cylinder, will be evacuated in the tube, or fills after vacuumizing with inert gas; (2) by heating and heat-insulating device METAL HEATING PROCESS in the ball grinding cylinder also is incubated, temperature is controlled at below the fusing point of grinding ball material, and solid metallic is melted fully, through the ball milling of certain hour, motlten metal and abrading-ball complete reaction generate required intermetallic compound powder; (3) by sieve method excessive abrading-ball is separated with product, obtain fine, pure intermetallic compound powder.
Described abrading-ball material is Ni or Ti or Mo or W or Fe or stainless steel or other metal, and abrading-ball is of a size of one or more.
Can add the part pressed powder identical during ball milling, to quicken the formation of intermetallic compound powder with the abrading-ball material; Also can in ball grinding cylinder, insert the inner lining material identical and participate in reaction directly, participate in reaction to prevent ball grinding cylinder with the abrading-ball material.
The device of preparation intermetallic compound powder of the present invention comprises ball grinding cylinder, reductor and buncher, and described ball grinding cylinder is outside equipped with heater, and temperature controller and temperature element are housed on it.Described heater is a resistance furnace, asks mill tube to place in it, and described temperature element is a thermocouple.
The turning cylinder of described ball grinding cylinder is provided with intercommunicating pore, communicates in one end and the ball grinding cylinder tube, and vacuum valve is equipped with in the another port.
Ball milling of the present invention is to carry out in a kind of solid metal and a kind of liquid metals, generate compound powder between solid metallic, abrading-ball (or ball grinding cylinder inner lining material) is participated in reaction directly, be one of intermetallic compound constituent element of being produced, its beneficial effect is: existing limitation when (1) has overcome the prepared by mechanical alloy intermetallic compound can prepare compound between the high-temperature metal that other method is difficult to prepare; (2) ball milling medium of the same race, under different temperature, it is identical and form compound powder between different series metal to produce constituent element, and this also helps the formation mechanism of intermetallic compound and the still indefinite intermetallic compound of formation temperature are carried out pilot study; It is simple, simple to operate, with low cost also will to produce important effect (3) present device to the research of basic theory aspects such as intermetallic compound, phasor, preparation method and device for effective intermetallic compound powder, it will enrich the production kind of intermetallic compound, further widen its application prospect, produce good society and economic benefit.
Description of drawings
Fig. 1 is the structural representation of the embodiment of the invention.
Drawing reference numeral is represented respectively:
1, thermocouple, 2, temperature controller, 3, resistance furnace, 4, ball grinding cylinder, 5, intercommunicating pore, 6, vacuum valve, 7, reductor, 8, buncher.
Specific embodiment method and the device thereof for preparing intermetallic compound powder of the present invention, its method are to adopt the high-temperature liquid state ball mill device, at high temperature, motlten metal are carried out ball milling, produce the intermetallic compound powder of abrading-ball and motlten metal two constituent elements.Determine the ball milling temperature according to the intermetallic compound that will prepare, temperature can be regulated between 200 ℃-1400 ℃, the ball milling time is 6~120 hours, ratio of grinding media to material is 6~30: 1, and the ball grinding cylinder rotating speed is 50~110 rev/mins, and abrading-ball is one of raw material, in the mechanical milling process, abrading-ball (or ball grinding cylinder inner lining material) is participated in reaction directly, and under different temperatures, producing with abrading-ball and motlten metal is the intermetallic compound powder of a series of different compositions of constituent element; Its processing step is: put into the solid metallic raw material in (1) ball grinding cylinder, with vacuum pumping in the tube, or fill after vacuumizing with inert gas, this process can be repeatedly several times, to eliminate the oxidative phenomena that may occur in the high-temperature reaction process fully; (2) by heating and heat-insulating device the raw material in the ball grinding cylinder is heated and insulation, temperature is controlled at below the fusing point of grinding ball material, and solid metallic is melted fully, through the ball milling of certain hour, motlten metal and abrading-ball complete reaction generate required intermetallic compound powder; (3) in the mechanical milling process, abrading-ball and the liquid metal generation intermetallic compound powder that under the mechanical force field action, reacts, the relative liquid metal of abrading-ball is excessive, after the liquid metal complete reaction generates intermetallic compound powder, by sieve method excessive abrading-ball is separated with product, obtain fine, pure intermetallic compound powder.
Described abrading-ball material is Ni or Ti or Mo or W or Fe or stainless steel or other metal, and abrading-ball is of a size of one or more.Can add the part pressed powder identical during ball milling, to quicken the formation of intermetallic compound powder with the abrading-ball material; Also can in ball grinding cylinder, insert the inner lining material identical and participate in reaction directly, participate in reaction to prevent ball grinding cylinder with the abrading-ball material.
The device of preparation intermetallic compound powder of the present invention, as shown in Figure 1, it comprises ball grinding cylinder 4, reductor 7 and adjusts motor 8 that ball grinding cylinder 4 places in the resistance furnace 3, and temperature controller 2 and thermocouple 1 are housed on the resistance furnace 3; Resistance furnace 3 is heated raw material in the ball grinding cylinder 4 by temperature controller 2 strict control temperature and is incubated; ball grinding cylinder 4 is driven around axial rotation by buncher 8 through reductor 7; rotating speed is regulated by buncher 8; the turning cylinder of ball grinding cylinder 4 is provided with intercommunicating pore 5; communicate in 4 of one end and the ball grinding cylinders; vacuum valve 6 is equipped with in the another port, in order to vacuumizing or feed protective gas in the ball grinding cylinder 4, eliminates the oxidative phenomena that may occur in the high-temperature reaction process.
Embodiment 1 utilizes apparatus of the present invention, abrading-ball is that iron ball, motlten metal are tin, under different temperatures, carry out ball milling, obtain following FeSn intermetallic compound: (ratio of grinding media to material: 30: 1, ball grinding cylinder rotating speed: 70~80 rev/mins) temperature (℃) time (hour) product illustrates 320 48 FeSn 2Mechanical alloying needs FeSn mechanical alloying in 150 hours 600 120 can not generate 760 120 Fe 3Sn 2Mechanical alloying can not generate 800 120 Fe 1.3The Sn mechanical alloying can not generate
Embodiment 2 utilizes apparatus of the present invention, to aluminium liquid ball milling, prepares Al with the titanium ball 3Ti, AlTi 3In powder.Its technological parameter is as follows:
Temperature: 650 ℃~1000 ℃
The ball milling time: 6~30 hours
Ratio of grinding media to material: 10~25: 1
Ball grinding cylinder rotating speed: 60~90 rev/mins
(the conventional mechanical alloying can only generate amorphous structure, and can not get this kind crystalline, powder).
Embodiment 3 utilizes apparatus of the present invention, to aluminium liquid ball milling, prepares Ni with the nickel ball 3Al, Ni 2Al 3, the NiAl powder.(shortening greatly than the conventional mechanical alloying rise time)

Claims (9)

1, a kind of method for preparing intermetallic compound powder is characterized in that: adopt the high-temperature liquid state ball mill device, at high temperature, motlten metal is carried out ball milling, produce the intermetallic compound powder of abrading-ball and motlten metal two constituent elements.
2, the method for preparing intermetallic compound powder according to claim 1, it is characterized in that: described ball milling temperature is regulated between 200 ℃~1400 ℃, the ball milling time is 6~120 hours, ratio of grinding media to material is 6~30: 1, the ball grinding cylinder rotating speed is 50~110 rev/mins, abrading-ball is one of raw material, and under different temperatures, producing with abrading-ball and motlten metal is the intermetallic compound powder of a series of different compositions of constituent element.
3, the method for preparing intermetallic compound powder according to claim 1 and 2 is characterized in that adopting following step:
(1) put into the solid metallic raw material in ball grinding cylinder, will be evacuated in the tube, or fill after vacuumizing with inert gas, this process can be repeatedly several times;
(2) by heating and heat-insulating device the raw material in the ball grinding cylinder is heated and insulation, temperature is controlled at below the grinding ball material fusing point, and solid metallic is melted fully, through the ball milling of certain hour, motlten metal and abrading-ball complete reaction generate required intermetallic compound powder;
(3) by sieve method excessive abrading-ball is separated with product, obtain fine, pure intermetallic compound powder.
4, the method for preparing intermetallic compound powder according to claim 3 is characterized in that described abrading-ball material is Ni or Ti or Mo or W or Fe or stainless steel or other metal, and abrading-ball is of a size of one or more.
5, the method for preparing intermetallic compound powder according to claim 4 is characterized in that: can add the part pressed powder identical with the abrading-ball material during ball milling.
6, the method for preparing intermetallic compound powder according to claim 4 is characterized in that inserting in the ball grinding cylinder inner lining material identical with the abrading-ball material and participates in reaction directly.
7, a kind of device of implementing the described method of claim 1 comprises ball grinding cylinder (4), reductor (7) and buncher (8), it is characterized in that described ball grinding cylinder (4) is outside equipped with heater, is equipped with temperature controller (2) and temperature element on it.
8, the device of preparation intermetallic compound powder according to claim 7 is characterized in that described heater is resistance furnace (3), and ball grinding cylinder (4) places in it, and described temperature element is thermocouple (1).
9, according to the device of claim 7 or 8 described preparation intermetallic compound powders, it is characterized in that the turning cylinder of described ball grinding cylinder (4) is provided with intercommunicating pore (5), communicate in one end and ball grinding cylinder (4) tube, vacuum valve (6) is equipped with in the another port.
CNB021143323A 2002-08-09 2002-08-09 Method for preparing intermetallic compound powder and its equipment Expired - Fee Related CN1189276C (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CNB021143323A CN1189276C (en) 2002-08-09 2002-08-09 Method for preparing intermetallic compound powder and its equipment

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CNB021143323A CN1189276C (en) 2002-08-09 2002-08-09 Method for preparing intermetallic compound powder and its equipment

Publications (2)

Publication Number Publication Date
CN1394707A true CN1394707A (en) 2003-02-05
CN1189276C CN1189276C (en) 2005-02-16

Family

ID=4743052

Family Applications (1)

Application Number Title Priority Date Filing Date
CNB021143323A Expired - Fee Related CN1189276C (en) 2002-08-09 2002-08-09 Method for preparing intermetallic compound powder and its equipment

Country Status (1)

Country Link
CN (1) CN1189276C (en)

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100460074C (en) * 2006-09-19 2009-02-11 东北大学 High temperature energy ball grinder
CN101805839A (en) * 2010-04-23 2010-08-18 东北大学 Preparation method of secondary skeleton infiltration alloy material
CN107138731A (en) * 2017-06-07 2017-09-08 广州艾普纳米科技有限公司 A kind of preparation method of nano metal powder
CN109179466A (en) * 2018-10-09 2019-01-11 湖南工业大学 A kind of metallic aluminium prepares the method and production system of ultra-fine schmigel
CN109396449A (en) * 2018-09-30 2019-03-01 东北大学 One kind preparing Ni by raw material of Ni-Al mixed-powder3The method of Al intermetallic compound powder
CN110524402A (en) * 2019-09-09 2019-12-03 常州大学 Bitubular high energy ball milling machine and its application method for the processing of hot-galvanized steel ironware
CN112847129A (en) * 2021-01-28 2021-05-28 中汽创智科技有限公司 Tumbling mill device
CN109019668B (en) * 2018-10-09 2021-09-28 湖南工业大学 Method for preparing superfine active zinc oxide powder by hot ball milling oxidation

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100460074C (en) * 2006-09-19 2009-02-11 东北大学 High temperature energy ball grinder
CN101805839A (en) * 2010-04-23 2010-08-18 东北大学 Preparation method of secondary skeleton infiltration alloy material
CN101805839B (en) * 2010-04-23 2012-02-01 东北大学 Preparation method of secondary skeleton infiltration alloy material
CN107138731A (en) * 2017-06-07 2017-09-08 广州艾普纳米科技有限公司 A kind of preparation method of nano metal powder
CN109396449A (en) * 2018-09-30 2019-03-01 东北大学 One kind preparing Ni by raw material of Ni-Al mixed-powder3The method of Al intermetallic compound powder
CN109179466A (en) * 2018-10-09 2019-01-11 湖南工业大学 A kind of metallic aluminium prepares the method and production system of ultra-fine schmigel
CN109019668B (en) * 2018-10-09 2021-09-28 湖南工业大学 Method for preparing superfine active zinc oxide powder by hot ball milling oxidation
CN109179466B (en) * 2018-10-09 2021-09-28 湖南工业大学 Method for preparing superfine corundum powder from metal aluminum
CN110524402A (en) * 2019-09-09 2019-12-03 常州大学 Bitubular high energy ball milling machine and its application method for the processing of hot-galvanized steel ironware
CN112847129A (en) * 2021-01-28 2021-05-28 中汽创智科技有限公司 Tumbling mill device

Also Published As

Publication number Publication date
CN1189276C (en) 2005-02-16

Similar Documents

Publication Publication Date Title
Jiang et al. Review of porous intermetallic compounds by reactive synthesis of elemental powders
CN107130125A (en) A kind of preparation method of high-entropy alloy
CN103317128B (en) A kind of Mg-Ni-La base composite hydrogen storage alloy powder and preparation method thereof
CN106167870A (en) A kind of NbMoTaW high-entropy alloy and preparation method thereof
CN108787750B (en) One-step large-deformation rolling method for β solidified TiAl alloy plate
CN105463222A (en) Preparing method for in-situ synthesis TiC-Ti5Si3 particle reinforcement Ti-based composite material
CN1354274A (en) Nickel base amorphous alloy
CN101586197A (en) Method for preparing titanium alloy ingots through electron-beam cold bed furnaces by adopting conventional raw materials
CN101259536A (en) Method for preparing high niobium containing titanium aluminium alloy powder
CN105478771B (en) A kind of manufacture method of inexpensive molybdenum tube target
CN1189276C (en) Method for preparing intermetallic compound powder and its equipment
CN112831694B (en) Rare earth aluminum alloy powder suitable for additive manufacturing and preparation method thereof
CN105568036A (en) Preparing method of high-silicon aluminum composite material
CN103160701A (en) Preparation method for high-temperature-resistant Mo-Si-B alloy
CN114799155B (en) Preparation method of ceramic particle reinforced refractory high-entropy alloy
CN105316501A (en) Rare earth-magnesium-based hydrogen storage alloy and preparation method thereof
CN108588471A (en) The one-step method for synthesizing of the copper base electrode material of ceramic particle containing nano-zirconium carbide
CN110724885A (en) Preparation method of large-size light magnesium-aluminum-based amorphous alloy
Nie Patents of methods to prepare intermetallic matrix composites: A Review
CN100415910C (en) Method of producing hydrogen-storage alloy by discharge plasma sintering technique
CN108179296A (en) A kind of high heat-resistant aluminium alloy material and preparation method thereof
CN109338150B (en) Porous copper alloy and preparation method thereof
CN107470641A (en) A kind of iron-based amorphous powder and preparation method thereof
CN109434121A (en) A method of Nb-Al amorphous thin layer is prepared using mechanical alloying method
CN2561508Y (en) Liquid ball grinder for preparing intermetallic compound powder

Legal Events

Date Code Title Description
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
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