CN109986087A - A kind of micron-size spherical densification tungsten iridium powder and preparation method thereof - Google Patents
A kind of micron-size spherical densification tungsten iridium powder and preparation method thereof Download PDFInfo
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- CN109986087A CN109986087A CN201910316661.8A CN201910316661A CN109986087A CN 109986087 A CN109986087 A CN 109986087A CN 201910316661 A CN201910316661 A CN 201910316661A CN 109986087 A CN109986087 A CN 109986087A
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Abstract
The invention discloses a kind of micron-size spherical densification tungsten iridium powders and preparation method thereof, the tungsten iridium powder that iridium content is 10~60wt.% can be prepared, the micron order WIr powder of preparation has good consistency and spherical morphology, and particle size is 1~5 μm, and average grain diameter is 3 μm.The present invention is with ammonium tungstate [(NH4)10W12O41] and ammonium chloroiridate [(NH4)2IrCl6] it is raw material, micron-size spherical densification WIr powder is prepared for using atomization drying combination microwave calcination technology.Micron-size spherical densification WIr powder prepared by the present invention has the advantages of of uniform size, sphericity is high, consistency and good dispersion, has good mobility and sintering character.This tungsten iridium powder can be used for preparing cathodic discharge material, compared to pure tungsten electrodes, with stronger electron emissivity, the characteristics of high electron current density and low electrode operating temperature.
Description
Technical field
The invention belongs to powder metallurgical technologies, and in particular to a kind of preparation side of micron-size spherical densification tungsten iridium powder
Method.
Background technique
The fusing point of tungsten is up to 3683 DEG C, and electron emissivity is strong, and elasticity modulus is high, and steam forces down, thus very early by with
Make thermionic emission materials.But the launching electronics efficiency of pure metal tungsten electrode is very low, and the shaft-like such as recrystallization formation at high temperature
Grain structure and make its easy fracture.To overcome disadvantages mentioned above, the development of modern industry new technology, new process, various countries' material are adapted to
Worker is committed to researching and developing various new electrode materials.Iridium is added in tungsten, forms tungsten irridium alloy tissue, Ji Nenggai
The problem of kind pure tungsten tissue recrystallization, and its electron emissivity can be enhanced.Therefore before tungsten iridium electrode material has application well
Scape.Since there is very high-melting-point, traditional smelting process to be unable to satisfy its processing request for tungsten and (2466 DEG C) of iridium, powder smelting at present
Golden method is most suitable processing method, and powder metallurgic method can reduce alloying component segregation and tissue odds to the full extent
It is even.Existing frequently-used tungsten alloy powder preparation method is mechanical alloying method, i.e. two kinds of (or a variety of) metal powders are put into high energy
In ball mill, alloy powder is made in mixed grinding, but this alloy powder is a kind of pseudo- alloy structure, and alloying needs further
Sintering is realized, and its pattern is irregular, easy to reunite, therefore powder fluidity and insufficient formability, is unfavorable for the molding and cause of product
Densification.Method proposed by the present invention can prepare a kind of micron-size spherical densification tungsten iridium powder, have dispersion well
Property, the spherical morphology of rule, the characteristic of high-compactness and good size distribution, and the powder is a kind of true alloying
Tissue.
A kind of dipped barium-tungsten cathode based on tungsten irridium alloy of 1 invention of patent document, preparation method is: by tungsten powder and iridium
Powder is respectively put into 1000-1500 DEG C of hydrogen furnace annealing；10-30% iridium powder is taken by weight, and surplus is tungsten powder, by two kinds of materials
It is ground.Mixture is pressed into flat-top cathode with the interior pressing mold for having molybdenum cylinder；Cathode is put into hydrogen furnace, is heated to 1500-
At 2000 DEG C, 1-10 hours are kept the temperature；It is placed it in aluminic acid salt powder again, under hydrogen atmosphere environment, 1500-2000 DEG C of dipping 1-
10 minutes, the floating salt after dipping was removed with tungsten wire cotton mass；Heater is finally installed, the dipping barium tungsten yin based on tungsten irridium alloy is made
Pole.
A kind of preparation process of filament material of 2 invention of patent document, the technique are as follows: choose diameter 0.2mm to 0.25mm
3~5, tungsten-rhenium alloy monofilament be twisted, and stranded filament ontology is subjected to immersion solidity, then gluing and in glue
Yttrium oxide powder is added in liquid, carries out frosted processing after dry, sintering, then be bonded tungsten irridium alloy, finished product is obtained after dry solidification.
The filament bending resistance of invention preparation is superior, has very strong inoxidizability, and effectively improves filament surface transmitting electricity
Sub- ability reduces the power consumption of filament.
A kind of preparation method of high-density iridium alloy preform of 3 invention of patent document, preparation method are as follows: closed according to final iridium
The component requirements of golden base, using high energy ball mill by tungsten powder, tungsten thorium alloy powder and the high energy activation of iridium powder and be uniformly mixed be placed on
It is dried in vacuum drying oven, obtains high energy activation mixed powder, then the mode by high energy activation mixed powder through molding or isostatic cool pressing
Compression moulding is made powder compact, then powder compact is placed in high temperature sintering furnace and is sintered, and furnace cooling obtains high-density iridium conjunction
Golden base.The invention solves trace thorium being uniformly distributed in alloy powder using the activation of component high-energy ball milling in batches and mixing
Problem reduces sintering activating energy, has prepared the requirement for meeting iridium alloy application ware and subsequent thermal processing to blank density,
Its relative density reaches 95% or more.
Patent document 1:CN1538482
Patent document 2:CN105448625A
Patent document 3:CN102168200A
Summary of the invention
The purpose of the present invention is to provide a kind of micron-size spherical densification WIr raw powder's production technologies, are guaranteeing WIr powder
Morphology and size under the premise of, as far as possible improve powder compactness.
WIr morphology microstructure is spherical shape, and having a size of micron order, particle diameter distribution is 1~5 μm, and average grain diameter is 3 μm.
The present invention can prepare the tungsten iridium powder that iridium content is 10~60wt.%, can change WIr powder according to product requirement
In iridium content.
The present invention is with ammonium tungstate [(NH4)10W12O41] and ammonium chloroiridate [(NH4)2IrCl6] it is raw material, using " atomization drying
In conjunction with microwave calcination technology " it is prepared for micron-size spherical densification WIr powder, specific steps method includes the following steps:
(1) atomization drying: with (NH4)10W12O41(NH4)2IrCl6For raw material, one is configured according to required W/Ir equivalent proportion
The mixed solution for determining concentration, using spray drying process, control flow quantity is 4.0~6.0ml/min, atomization air pressure is 0.4~
0.7MPa, inlet temperature are 140~200 DEG C, and hot air flow amount is 4.0~10.0L/min, and spherical shape (NH is made4)10W12O41-
(NH4)2IrCl6Particle；
(2) microwave calcination: by the spheric granules of atomization drying atmosphere be N2/H2In (9:1vol) microwave calcination furnace, temperature
Control keeps the temperature 1~2h at 700~900 DEG C, and micron-size spherical densification WIr powder is made.
The present invention can prepare the tungsten iridium powder that iridium content is 10~60wt.%, and the micron order WIr powder of preparation has very well
Consistency and spherical morphology, particle size be 1~5 μm, average grain diameter be 3 μm.With ammonium tungstate [(NH4)10W12O41] and chlorine iridium
Sour ammonium [(NH4)2IrCl6] it is raw material, micron-size spherical densification WIr is prepared for using " atomization drying combination microwave calcination technology "
Powder, specific steps method include the following steps: (1) atomization drying: with (NH4)10W12O41(NH4)2IrCl6For raw material, press
Certain density mixed solution is configured according to required W/Ir equivalent proportion, using spray drying process, control flow quantity is 4.0~6.0ml/
Min, atomization air pressure are 0.4~0.7MPa, and inlet temperature is 140~200 DEG C, and hot air flow amount is 4.0~10.0L/min,
Spherical shape (NH is made4)10W12O41-(NH4)2IrCl6Particle；(2) microwave calcination: by the spheric granules of atomization drying atmosphere be N2/
H2In (9:1vol) microwave calcination furnace, temperature is controlled at 700~900 DEG C, keeps the temperature 1~2h, and micron-size spherical densification WIr powder is made
Body.The present invention is by atomization drying and microwave calcination technique, the micron-size spherical densification WIr powder of preparation, have it is of uniform size,
The advantages of sphericity is high, consistency and good dispersion, this makes tungsten iridium powder have good mobility and sintering character.It is this
Tungsten iridium powder can be used for preparing cathodic discharge material, compared to pure tungsten electrodes, with stronger electron emissivity, high electricity
The characteristics of electron current density and low electrode operating temperature.
Detailed description of the invention
Fig. 1 is process flow chart of the invention；
Fig. 2 is the XRD analysis map of W20Ir powder of the present invention；
Fig. 3 a and Fig. 3 b are that the SEM of W20Ir powder of the present invention schemes.
Specific embodiment
Embodiment 1
By taking ingredient W20Ir as an example, it is atomized prilling are as follows: control flow quantity is 5.0mL/min, 170 DEG C of inlet temperature, hot
Air draught amount 6.0L/min.The calcine technology are as follows: control calcination atmosphere N2/H2(Vol 9:1), from room temperature to 800 DEG C
Heat preservation 1 hour, furnace cooling obtain the W20Ir powder that particle size is 1~5 μm.
Embodiment 2
Difference from Example 1 is, the atomization prilling are as follows: control flow quantity is 5.0mL/min, import temperature
170 DEG C of degree, hot air flow amount 8.0L/min.The calcine technology are as follows: control calcination atmosphere N2/H2(Vol 9:1), from room temperature
It is warming up to 800 DEG C and keeps the temperature 1 hour, furnace cooling obtains the W20Ir powder that particle size is 0.5~4 μm.
Embodiment 3
Difference from Example 1 is, the atomization prilling are as follows: control flow quantity is 3.0mL/min, import temperature
170 DEG C of degree, hot air flow amount 6.0L/min.The calcine technology are as follows: control calcination atmosphere N2/H2(Vol 9:1), from room temperature
It is warming up to 800 DEG C and keeps the temperature 1 hour, furnace cooling obtains the W20Ir powder that particle size is 0.5~3 μm.
Embodiment 4
Difference from Example 1 is, the atomization prilling are as follows: control flow quantity is 5.0mL/min, import temperature
170 DEG C of degree, hot air flow amount 6.0L/min.The calcine technology are as follows: control calcination atmosphere N2/H2(Vol 9:1), from room temperature
It is warming up to 650 DEG C and keeps the temperature 1 hour, furnace cooling obtains the W20Ir powder that particle size is 1~8 μm.
Comparative example 1
1,2,3 difference of embodiment, in atomization granulation process, hot air flow amount increases or flow quantity is reduced, meeting
So that atomization granulation result particle size reduces.
Comparative example 2
Embodiment 1,4 the difference is that, during microwave calcination, the raising of calcination temperature can make final powder consistency
It improves, size reduces, and specific surface area decreases.
Claims (5)
1. a kind of micron-size spherical densification tungsten iridium powder, it is characterised in that: powder particle is spherical shape, and surface is smooth.
2. a kind of micron-size spherical densification tungsten iridium powder according to claim 1, it is characterised in that: the tungsten iridium powder
Iridium content is the tungsten iridium powder of 10~60wt.%, and can change the iridium content in WIr powder according to product requirement.
3. a kind of micron-size spherical densification tungsten iridium powder according to claim 1, it is characterised in that: the tungsten iridium powder is
Micron order, particle diameter distribution are 1~5 μm, and average grain diameter is 3 μm, and specific surface area is less than 0.2m2/g。
4. a kind of micron-size spherical densification tungsten iridium raw powder's production technology, it is characterised in that: forged using atomization drying combination microwave
Burning technology prepares micron-size spherical densification WIr powder, and specific steps method includes the following steps:
(1) atomization drying: with (NH4)10W12O41(NH4)2IrCl6For raw material, a certain concentration is configured according to required W/Ir equivalent proportion
Mixed solution, using spray drying process, control flow quantity is 4.0~6.0ml/min, and atomization air pressure is 0.4~0.7MPa, into
Mouth temperature is 140~200 DEG C, and hot air flow amount is 4.0~10.0L/min, and spherical shape (NH is made4)10W12O41-(NH4)2IrCl6Particle；
(2) microwave calcination: by the spheric granules of atomization drying atmosphere be N2/H2In (9:1vol) microwave calcination furnace, temperature control
At 700~900 DEG C, 1~2h is kept the temperature, micron-size spherical densification WIr powder is made.
5. a kind of micron-size spherical densification tungsten iridium raw powder's production technology, it is characterised in that:
Spherical shape (NH is prepared using atomization drying technology4)10W12O41-(NH4)2IrCl6Granular precursor, with (NH4)10W12O41With
(NH4)2IrCl6For raw material, certain density (NH is configured according to required W/Ir equivalent proportion4)10W12O41-(NH4)2IrCl6Solution,
Using spray drying process, control flow quantity is 4.0~6.0ml/min, and atomization air pressure is 0.4~0.7MPa, inlet temperature 140
~200 DEG C, hot air flow amount is 4.0~10.0L/min, and spherical shape (NH is made4)10W12O41-(NH4)2IrCl6Particle, partial size 2
~10 μm；
Microwave calcination technology prepares micron-size spherical densification tungsten iridium powder: the granular precursor of above-mentioned spherical shape is placed in microwave calcination
In furnace, protective atmosphere N2/H2(9:1vol), temperature are controlled at 700~900 DEG C, keep the temperature 1~2h, it is fine and close that micron-size spherical is made
WIr powder, partial size are 1~5 μm, and average grain diameter is 3 μm, and powder has good mobility and sintering character.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111128639A (en) * | 2019-12-23 | 2020-05-08 | 北京工业大学 | Method for preparing impregnated MM type cathode by microwave sintering |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5007874A (en) * | 1990-10-15 | 1991-04-16 | The United States Of America As Represented By The Secretary Of The Army | Method of making a cathode from tungsten and iridium powders using a reaction product from reacting a group III A metal with barium peroxide as an impregnant |
| CN101831568A (en) * | 2010-05-21 | 2010-09-15 | 西北有色金属研究院 | Method for preparing superhigh temperature resistant iridium alloy by using powder metallurgy method |
| WO2011054113A1 (en) * | 2009-11-05 | 2011-05-12 | Ap&C Advanced Powders & Coatings Inc. | Methods and apparatuses for preparing spheroidal powders |
| CN105886826A (en) * | 2016-04-21 | 2016-08-24 | 西北有色金属研究院 | Platinum-iridium-zirconium-tungsten-thorium alloy welding flux and preparing method thereof |
| CN106166613A (en) * | 2016-08-18 | 2016-11-30 | 贵研铂业股份有限公司 | A kind of micron-size spherical W Mo alloy powder and preparation method thereof |
| CN108251734A (en) * | 2016-12-28 | 2018-07-06 | 北京有色金属研究总院 | A kind of hot cathode tungsten basal body and preparation method thereof |
| CN108296491A (en) * | 2018-01-24 | 2018-07-20 | 贵研铂业股份有限公司 | A kind of spherical iridium raw powder's production technology of micron order |
-
2019
- 2019-04-19 CN CN201910316661.8A patent/CN109986087A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5007874A (en) * | 1990-10-15 | 1991-04-16 | The United States Of America As Represented By The Secretary Of The Army | Method of making a cathode from tungsten and iridium powders using a reaction product from reacting a group III A metal with barium peroxide as an impregnant |
| WO2011054113A1 (en) * | 2009-11-05 | 2011-05-12 | Ap&C Advanced Powders & Coatings Inc. | Methods and apparatuses for preparing spheroidal powders |
| CN101831568A (en) * | 2010-05-21 | 2010-09-15 | 西北有色金属研究院 | Method for preparing superhigh temperature resistant iridium alloy by using powder metallurgy method |
| CN105886826A (en) * | 2016-04-21 | 2016-08-24 | 西北有色金属研究院 | Platinum-iridium-zirconium-tungsten-thorium alloy welding flux and preparing method thereof |
| CN106166613A (en) * | 2016-08-18 | 2016-11-30 | 贵研铂业股份有限公司 | A kind of micron-size spherical W Mo alloy powder and preparation method thereof |
| CN108251734A (en) * | 2016-12-28 | 2018-07-06 | 北京有色金属研究总院 | A kind of hot cathode tungsten basal body and preparation method thereof |
| CN108296491A (en) * | 2018-01-24 | 2018-07-20 | 贵研铂业股份有限公司 | A kind of spherical iridium raw powder's production technology of micron order |
Non-Patent Citations (3)
| Title |
|---|
| 代书华: "《有色金属冶金概论》", 31 August 2015, 冶金工业出版社 * |
| 印协世: "《钨铼合金和钨铼热电偶》", 31 December 1992, 冶金工业出版社 * |
| 徐克玷: "《钼的材料科学与工程》", 31 July 2014, 冶金工业出版社 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111128639A (en) * | 2019-12-23 | 2020-05-08 | 北京工业大学 | Method for preparing impregnated MM type cathode by microwave sintering |
| CN111128639B (en) * | 2019-12-23 | 2022-08-16 | 北京工业大学 | Method for preparing impregnated MM type cathode by microwave sintering |
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Application publication date: 20190709 |