AU2020103465A4 - Method for preparing high-purity spherical ruthenium powder by microwave one-step method - Google Patents
Method for preparing high-purity spherical ruthenium powder by microwave one-step method Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 48
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 229910052707 ruthenium Inorganic materials 0.000 title claims abstract description 42
- 239000000843 powder Substances 0.000 title claims abstract description 40
- 239000000463 material Substances 0.000 claims abstract description 26
- 238000010438 heat treatment Methods 0.000 claims abstract description 14
- NZIGZHDIUCTKQH-UHFFFAOYSA-M Cl[Ru+2].N Chemical compound Cl[Ru+2].N NZIGZHDIUCTKQH-UHFFFAOYSA-M 0.000 claims abstract description 11
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 239000011261 inert gas Substances 0.000 claims abstract description 6
- 238000001354 calcination Methods 0.000 abstract description 22
- 238000004663 powder metallurgy Methods 0.000 abstract description 2
- 239000002245 particle Substances 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 description 8
- 238000006722 reduction reaction Methods 0.000 description 7
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 5
- 238000005054 agglomeration Methods 0.000 description 5
- 230000002776 aggregation Effects 0.000 description 5
- 230000007547 defect Effects 0.000 description 5
- 239000001257 hydrogen Substances 0.000 description 5
- 229910052739 hydrogen Inorganic materials 0.000 description 5
- 239000013077 target material Substances 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- CBPDZOCGZCDPGA-UHFFFAOYSA-K azane ruthenium(3+) trichloride Chemical compound [Ru+3].[Cl-].N.[Cl-].[Cl-] CBPDZOCGZCDPGA-UHFFFAOYSA-K 0.000 description 2
- 239000003990 capacitor Substances 0.000 description 2
- 150000001768 cations Chemical class 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 238000005485 electric heating Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- WOCIAKWEIIZHES-UHFFFAOYSA-N ruthenium(iv) oxide Chemical compound O=[Ru]=O WOCIAKWEIIZHES-UHFFFAOYSA-N 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 238000000889 atomisation Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 230000021715 photosynthesis, light harvesting Effects 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 1
- -1 platinum group metals Chemical class 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 229910001927 ruthenium tetroxide Inorganic materials 0.000 description 1
- 238000005185 salting out Methods 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
- B22F1/142—Thermal or thermo-mechanical treatment
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/06—Metallic powder characterised by the shape of the particles
- B22F1/065—Spherical particles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2201/00—Treatment under specific atmosphere
- B22F2201/10—Inert gases
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2202/00—Treatment under specific physical conditions
- B22F2202/11—Use of irradiation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2301/00—Metallic composition of the powder or its coating
- B22F2301/25—Noble metals, i.e. Ag Au, Ir, Os, Pd, Pt, Rh, Ru
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- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention relates to a method for preparing high-purity spherical ruthenium powder
by a microwave one-step method and belongs to the technical field of powder metallurgy. The
method comprises the following steps of: feeding an ammonium chlororuthenium material into
a microwave device at a feeding speed of 0.05-0.2kg/min; heating the material from room
temperature to 450-550 DEG C at a speed of 50-100 DEG C/min under the protection of inert
gas in the microwave device with a frequency of 2.45GHz and a microwave power density of
60-95kW/cm 3; keeping the temperature for 10-30min; and naturally cooling the calcined
material to room temperature to obtain the high-purity spherical ruthenium powder product.
Due to the volume heating characteristic of the microwave, the ammonium chlororuthenium is
uniformly heated, the temperature gradient cannot be generated in the calcining process, the
heating is rapid, the particle size of the product components is uniform and spherical, and the
purity of the product is high.
Description
Method for preparing high-purity spherical ruthenium powder by microwave one-step method
TECHNICAL FIELD The invention relates to a method for preparing high-purity spherical ruthenium powder by a microwave one-step method and belongs to the technical field of powder metallurgy.
BACKGROUND Ruthenium is an element with special properties in platinum group metals, and has the characteristics of high melting point, high hardness, difficult mechanical processing and the like, one of the most important applications of the ruthenium powder at present is to produce ruthenium target materials, and the ruthenium target materials are used as computer hard disk memory materials. In addition, ruthenium targets are also widely used in the integrated circuit industry as capacitor electrode films. The noble metal target industry is the industry that Heraeus company, Zhaorong, Zhuyou and Sino-Platinum Metals Co., Ltd are developing vigorously at home and abroad. The target material used for the integrated circuit occupies a large share in the global target material market, and the ruthenium target material has great attention due to large consumption and high added value.
With the progress of technology, the application field of metal nail powder is expanded continuously, the market demand is increased gradually, the product is developed towards high purity and superfine, and the production process is developed towards large scale, reliability and simplicity. The requirements of integrated circuits for ruthenium powder are particularly stringent because there is no excellent ruthenium target without an excellent ruthenium powder and a high quality capacitor electrode film cannot be produced at the same time. At present, the output of high-purity ruthenium powder (such as spectral purity grade) in China is far from meeting the demand, and most of the high-purity ruthenium powder depends on imported high-price foreign products. With the further development of noble metal target industry, the demand for high purity ruthenium powder will increase. Therefore, the research on the method of mass production of high purity ruthenium powder must be paid enough attention to by the relevant scientific and technological workers in China. In addition, the research on the application of the ruthenium powder and the research on the recovery technology of the ruthenium powder are also significant.
At present, a chemical method is mainly adopted for preparing the high-purity Ru powder. The basic principle is as follows: after the Ru-containing material is pretreated, Ru is converted into cations through a certain oxidant, then the separation of Ru and impurity cations is realized through distillation by utilizing the characteristic that RuO4 has higher vapor pressure, and the separation of Ru and impurity anions is realized by adopting an ammonium salt precipitation, calcination and reduction method, so that the high-purity Ru powder is finally prepared. The method comprises the following basic processes: material pretreatment, oxidation dissolution, oxidation distillation, absorption concentration, precipitation crystallization, calcination decomposition and reduction milling. The main production process for preparing the high-purity Ru powder has the defects of long and complex production flow, high treatment temperature, long time, poor sphericity and the like. The main reason that the sphericity of the ruthenium powder is poor is that the ammonium ruthenium chloride is easy to agglomerate when the ammonium ruthenium chloride is decomposed at the temperature of about 240 DEG C, so that the defect is solved by rapidly raising the temperature, crossing an agglomeration area and calcining at high temperature.
For example, patent document 201510893339.3 discloses a method for preparing high-purity spherical ruthenium powder, which takes sponge ruthenium (less than 99.9%) as a raw material and adopts the process of 'distillation-chemical precipitation-atomization granulation-microwave calcination' to prepare the high-purity spherical ruthenium powder. The powder calcining process comprises the following steps of: calcining spherical (NH 4) 2RuC16 powder by using microwaves to prepare spherical Ru powder, wherein in the microwave calcining process, the protective atmosphere is N 2/H 2 ( Vol 9:1), the temperature is raised to 400-600 DEG C from room temperature, the temperature is kept for 2 hours, the temperature is raised to 800-1000 DEG C, the temperature is kept for 2 hours, the furnace is cooled, and the whole calcining process is carried out under the protection of the atmosphere. The invention has the obvious defects that the process flow is complex, the calcining time is long, the product is easy to overbu, and the activity is poor. In addition, patent document 201310112626.7 discloses a method for preparing ruthenium powder for targets, which comprises the following eight stages of: dissolving, precipitating, centrifugally filtering, drying, crushing, calcining, reducing and pulverizing, wherein the calcining stage comprises the following steps of: firstly calcining at 435-460 DEG C for 2.5-3.5 hours after crushing, raising the temperature to 630-660 DEG C for further calcining for 2.5-3.5 hours, and raising the temperature to 730-770 DEG C for calcining for 1.5-2.5 hours; and reducing: introducing hydrogen to reduce for 0.5-1.5 hours at 730-760 DEG C, which is similar to document 201510893339.3, and has the defects of long and complicated production process, high treatment temperature, serious spherical degree of product agglomeration and the like. The invention also discloses a method for separating and purifying ruthenium from ruthenium-containing waste materials in patent document 201510050119.4, which comprises the following steps of: introducing hydrogen at 650-750 DEG C for reducing to obtain 99.95% of ruthenium powder for 1- 4 hours, and purging with nitrogen for 5-30min before introducing the hydrogen.
Therefore, it is urgent to develop a new production method of high purity spherical ruthenium powder with high speed and low energy consumption.
As a green and efficient heating method, microwave can selectively heat materials through energy dissipation inside the materials, and has the advantages of uniform heating, high thermal efficiency, cleanness, no pollution and the like which cannot be compared with conventional heating modes. The application of microwave in the preparation of high-purity spherical ruthenium powder has very wide application prospect.
Aiming at the problems and disadvantages of the prior art, the invention provides a method for preparing high-purity spherical ruthenium powder by a microwave one-step method. According to the method, a high-purity spherical ruthenium powder product is prepared through a microwave calcination self-reduction reaction of ammonium chlororuthenium. The invention is realized by the following technical scheme.
The invention relates to a method for preparing high-purity spherical ruthenium powder by a microwave one-step method, which comprises the following specific steps:
The method comprises the following steps of: feeding an ammonium chlororuthenium material into a microwave device at a feeding speed of 0.05-0.2kg/min; heating the material from room temperature to 450-550 DEG C at a speed of 50-100 DEG C/min under the protection of inert gas in the microwave device with a frequency of 2.45GHz and a microwave power density of -95kW/cm 3; keeping the temperature for 10-30min, and naturally cooling the calcined material to room temperature to obtain the high-purity spherical ruthenium powder product.
The rate of temperature rise from room temperature is 50-100 DEG C/min.
The power density of the microwave device is 6095kW/cm3 .
The purity of the high-purity ruthenium powder product prepared by the method is as high as more than 99.995 wt%, and the product is spherical.
The basic principle of microwave calcination self-reduction is as follows:
(NH 4 ) 2 Ru(C) 3 = RuO 2 + 2NH 3 + H2 0
2NH 3= N 2 + 3H2
RuO2 + 2H 2 = Ru + 2H2 0
The process is characterized in that the microwave can directly penetrate through the material by utilizing the volume heating characteristic of the microwave, so that the internal and external bodies of the material are heated; and meanwhile, the high-power-density microwave is adopted, so that the ammonium chlororuthenium is rapidly heated, the temperature is rapidly raised, and the ammonium chlororuthenium rapidly passes through an agglomeration area at the temperature of about 240 DEG C, so that the high-temperature decomposition is realized. Compared with the conventional electric heating calcination method, the microwave heating overcomes the problem of product agglomeration which cannot be solved by the conventional electric heating method, meanwhile, the microwave calcination self-reduction method is adopted to avoid the complicated process flow of the conventional external hydrogen introduction, and the microwave calcination self-reduction method has the following advantages:
1. Due to the volume heating characteristic of the microwave, the ammonium chlororuthenium
is rapidly heated and decomposed, the product has no agglomeration and is spherical, and the purity
of the product is high;
2. The reducing atmosphere is ensured in a microwave calcination self-reduction mode, and
the defects of long treatment time and complex flow of the conventional calcination external
hydrogen are avoided;
3. The method has short production period, which can reduce energy consumption to a great
extent, realize the production mode of continuous feeding and discharging, and has wide industrial
application prospect.
DESCRIPTION OF THE INVENTION The present invention will be further described with reference to specific embodiment.
Embodiment 1
The method comprises the following steps of: feeding an ammonium chlororuthenium material into a microwave device at a feeding speed of 0.1kg/min; heating the material from room temperature to 500 DEG C at a speed of 70 DEG C/min under the protection of inert gas in the microwave device with a frequency of 2.45GHz and a microwave power density of 65kW/cm3 ,
keeping the temperature for 20min; and naturally cooling the calcined material to room temperature to obtain the high-purity spherical ruthenium powder product.
Through analysis and test, the purity of the product is up to more than 99.995%, and the product is spherical.
Embodiment 2
The method comprises the following steps of: feeding an ammonium chlororuthenium material into a microwave device at a feeding speed of 0.2 kg/min; heating the material from room temperature to 550 DEG C at a speed of 50 DEG C/min under the protection of inert gas in the microwave device with a frequency of 2.45GHz and a microwave power density of 80kW/cm3
, keeping the temperature for 10 minutes; and naturally cooling the calcined material to room temperature to obtain the high-purity spherical ruthenium powder product.
Through analysis and test, the purity of the product is up to more than 99.995%, and the product is spherical.
Embodiment 3
The method comprises the following steps of: feeding an ammonium chlororuthenium material into a microwave device at a feeding speed of 0.05kg/min; heating the material from room temperature to 450 DEG C at a speed of 100 DEG C/min under the protection of inert gas in the microwave device with a frequency of 2.45GHz and a microwave power density of 95kW/cm3
, keeping the temperature for 30min; and naturally cooling the calcined material to room temperature to obtain the high-purity spherical ruthenium powder product.
Through analysis and test, the purity of the product is up to more than 99.995%, and the product is spherical.
While specific embodiment of the present invention have been described in detail above, the present invention is not limited to the above embodiment, and various changes can be made within the knowledge possessed by those skilled in the art without departing from the spirit of the present invention.
Claims (3)
- Claims 1. A method for preparing high-purity spherical ruthenium powder by a microwave one-step method, which is characterized by comprising the following steps:The method comprises the following steps of: feeding an ammonium chlororuthenium material into a microwave device at a feeding speed of 0.05-0.2kg/min; heating the material from room temperature to 450-550 DEG C at a speed of 50-100 DEG C/min under the protection of inert gas in the microwave device with a frequency of 2.45GHz and a microwave power density of -95kW/cm 3; keeping the temperature for 10-30min, and naturally cooling the calcined material to room temperature to obtain the high-purity spherical ruthenium powder product.
- 2. The method for preparing high-purity spherical ruthenium powder by a microwave one-step method according to claim 1 is characterized in that the rate of temperature rise of the material from room temperature is 50-1OODEG C/min.
- 3. The method for preparing high-purity spherical ruthenium powder by the microwave one-step method according to claim 1 is characterized in that the power density of the microwave device is 60-95kW/cm3 .
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| AU2020103465A AU2020103465A4 (en) | 2020-11-16 | 2020-11-16 | Method for preparing high-purity spherical ruthenium powder by microwave one-step method |
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| AU2020103465A AU2020103465A4 (en) | 2020-11-16 | 2020-11-16 | Method for preparing high-purity spherical ruthenium powder by microwave one-step method |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113664210A (en) * | 2021-09-03 | 2021-11-19 | 昆明理工大学 | Preparation method of high-purity spherical ruthenium powder |
| CN113941703A (en) * | 2021-10-18 | 2022-01-18 | 合肥工业大学 | Method for preparing spherical bronze powder for 3D printing through microwave heating |
| CN114524451A (en) * | 2021-12-17 | 2022-05-24 | 中国北方稀土（集团）高科技股份有限公司 | Method for preparing large-particle-size rare earth oxide by one-step microwave at low temperature |
| CN115007851A (en) * | 2022-06-20 | 2022-09-06 | 华材(山东)新材料有限公司 | Device and method for producing superfine spherical ruthenium powder for 3D printing by one-step method |
-
2020
- 2020-11-16 AU AU2020103465A patent/AU2020103465A4/en not_active Ceased
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113664210A (en) * | 2021-09-03 | 2021-11-19 | 昆明理工大学 | Preparation method of high-purity spherical ruthenium powder |
| CN113941703A (en) * | 2021-10-18 | 2022-01-18 | 合肥工业大学 | Method for preparing spherical bronze powder for 3D printing through microwave heating |
| CN114524451A (en) * | 2021-12-17 | 2022-05-24 | 中国北方稀土（集团）高科技股份有限公司 | Method for preparing large-particle-size rare earth oxide by one-step microwave at low temperature |
| CN114524451B (en) * | 2021-12-17 | 2024-02-20 | 中国北方稀土（集团）高科技股份有限公司 | Method for preparing large-granularity rare earth oxide by one-step microwave at low temperature |
| CN115007851A (en) * | 2022-06-20 | 2022-09-06 | 华材(山东)新材料有限公司 | Device and method for producing superfine spherical ruthenium powder for 3D printing by one-step method |
| CN115007851B (en) * | 2022-06-20 | 2024-02-06 | 华材(山东)新材料有限公司 | Device and method for producing superfine spherical ruthenium powder for 3D printing by one-step method |
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