CN112439900A - Preparation method of rhodium metal nanoparticles - Google Patents
Preparation method of rhodium metal nanoparticles Download PDFInfo
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- CN112439900A CN112439900A CN201910817487.5A CN201910817487A CN112439900A CN 112439900 A CN112439900 A CN 112439900A CN 201910817487 A CN201910817487 A CN 201910817487A CN 112439900 A CN112439900 A CN 112439900A
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- rhodium
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- metal nanoparticles
- rhodium metal
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- 229910052703 rhodium Inorganic materials 0.000 title claims abstract description 107
- 239000010948 rhodium Substances 0.000 title claims abstract description 107
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 title claims abstract description 84
- 239000002082 metal nanoparticle Substances 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 208000028659 discharge Diseases 0.000 claims abstract description 43
- 239000000243 solution Substances 0.000 claims abstract description 36
- 238000000034 method Methods 0.000 claims abstract description 30
- -1 rhodium ions Chemical class 0.000 claims abstract description 25
- 239000011259 mixed solution Substances 0.000 claims abstract description 22
- 239000002245 particle Substances 0.000 claims abstract description 19
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 17
- 238000011282 treatment Methods 0.000 claims abstract description 11
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims description 22
- 239000007789 gas Substances 0.000 claims description 20
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 16
- 230000009467 reduction Effects 0.000 claims description 12
- 229910052786 argon Inorganic materials 0.000 claims description 9
- 239000011261 inert gas Substances 0.000 claims description 9
- 229910052751 metal Inorganic materials 0.000 claims description 9
- 239000002184 metal Substances 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 230000009471 action Effects 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 3
- 239000003570 air Substances 0.000 claims description 3
- 239000012298 atmosphere Substances 0.000 claims description 3
- 239000002671 adjuvant Substances 0.000 claims description 2
- 150000003839 salts Chemical class 0.000 claims description 2
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 3
- 238000006722 reduction reaction Methods 0.000 description 19
- 239000003638 chemical reducing agent Substances 0.000 description 8
- 239000002105 nanoparticle Substances 0.000 description 6
- 230000005540 biological transmission Effects 0.000 description 5
- 229910000510 noble metal Inorganic materials 0.000 description 5
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 229910000360 iron(III) sulfate Inorganic materials 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000009616 inductively coupled plasma Methods 0.000 description 2
- 150000002736 metal compounds Chemical class 0.000 description 2
- 239000002923 metal particle Substances 0.000 description 2
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 239000012266 salt solution Substances 0.000 description 2
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 150000001875 compounds Chemical group 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000002815 homogeneous catalyst Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- WJIBZZVTNMAURL-UHFFFAOYSA-N phosphane;rhodium Chemical class P.[Rh] WJIBZZVTNMAURL-UHFFFAOYSA-N 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 238000011946 reduction process Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
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- 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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
-
- 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
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- Chemical & Material Sciences (AREA)
- Nanotechnology (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Composite Materials (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention relates to a preparation method of rhodium metal nanoparticles, which comprises the step of subjecting a mixed solution containing a rhodium solution and an auxiliary agent to plasma glow discharge treatment to reduce rhodium ions in the mixed solution into the rhodium metal nanoparticles. The method adopts a plasma glow discharge method to reduce rhodium ions in the rhodium-containing solution, avoids the introduction of a reducing reagent, and is environment-friendly. Moreover, the preparation method provided by the invention is simple and can be carried out at normal temperature and normal pressure. In addition, the rhodium metal nanoparticles prepared by the preparation method provided by the invention have the advantages of small particle size, high purity, uniform particles and wide application prospect.
Description
Technical Field
The invention belongs to the technical field of material science, and particularly relates to a preparation method of rhodium metal nanoparticles.
Background
Nanoparticles generally refer to particles having a particle size of between 1 and 100 nm. Noble metal nanoparticles have been the focus of research in the field of catalysis because they have many advantages, such as small particle size, large specific surface area, high catalytic efficiency, etc. In addition, the noble metal nanoparticles have unique optical, electrical and catalytic properties. The characteristics make the nano-composite material have very important application value in the fields of surface plasma optics, biochemical sensing, catalysis and the like.
The current methods for preparing metal nanoparticles are mainly chemical reduction methods, which require the addition of strong reducing agents to the solution to reduce the metal compounds to metal particles. The reduction method for reducing metal compounds into metal particles has the disadvantages that a new chemical reduction reagent is introduced into a system, great influence is generated on the environment in the subsequent treatment process, the requirement on the operation condition of the chemical reduction method is high, the number of steps is large, and the result is difficult to control. Patent CN101032754A discloses a method for preparing nano-metals by reduction. The method adopts glow discharge plasma to reduce noble metal in argon atmosphere, and has the advantages of simple device, convenient operation, but certain defects, such as higher voltage at two ends of an electrode, lower gas pressure control, long reduction time consumption, larger obtained nano particles and the like.
Rhodium is used as a noble metal and can be prepared into noble metal homogeneous catalysts such as rhodium-phosphine complexes and the like. In practical applications, rhodium is usually present in solution in ionic form, and is usually utilized in the form of nanoparticles of rhodium to exploit its advantages as nanoparticles.
In view of the above-mentioned drawbacks of the conventional methods for preparing metal nanoparticles, there is a need to develop a new method for preparing rhodium metal nanoparticles.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a preparation method of rhodium metal nanoparticles aiming at the defects of the prior art. The method adopts a plasma glow discharge method to reduce rhodium ions in a rhodium-containing solution to form the rhodium metal nano particles. The method is carried out at normal temperature and normal pressure, does not need to introduce a new reducing agent, and is environment-friendly. Moreover, the method of the invention has the advantages of convenient operation, energy consumption saving and convenient treatment. In addition, the rhodium metal nanoparticles prepared by the method have small particle size and high purity.
Therefore, the invention provides a preparation method of rhodium metal nanoparticles, which comprises the step of subjecting a mixed solution containing a rhodium solution and an auxiliary agent to plasma glow discharge treatment so as to reduce rhodium ions in the mixed solution into the rhodium metal nanoparticles.
In some embodiments, the method for subjecting the mixed solution containing the rhodium solution and the auxiliary agent to plasma glow discharge treatment comprises the following steps:
putting the mixed solution containing the rhodium solution and the auxiliary agent in a plasma discharge gas atmosphere;
under the action of alternating current, the rhodium ions in the mixed solution are reduced into rhodium metal nano particles by plasma formed by plasma discharge gas discharge.
In some embodiments, the plasma discharge gas comprises one or more of an inert gas, nitrogen, and air.
In some embodiments, the inert gas is argon.
In some embodiments, the alternating current has a voltage of 150 to 500V, preferably 150 to 400V.
In some embodiments, the reduction time is 3-15min, preferably 5-15 min.
In some embodiments, the amount of the promoter added is 1 (10-25) mol/g, preferably 1 (15-20) mol/g, based on the ratio of the molar amount of rhodium ions in the rhodium-containing solution to the mass of the promoter.
In some embodiments, the rhodium-containing solution comprises a salt solution of rhodium metal, preferably a chloride solution of rhodium metal.
In some embodiments, the adjuvant comprises perchloric acid.
In some embodiments, the rhodium metal nanoparticles have a particle size of 7 to 20 nm.
Compared with the prior art, the invention has the following beneficial effects:
the preparation method of the rhodium metal nanoparticles adopts a plasma glow discharge method to reduce rhodium ions in a rhodium-containing solution to form the rhodium metal nanoparticles. In the reduction process, the plasma discharge gas generates a large amount of high-energy electrons under the action of alternating current, rhodium ions in the rhodium-containing solution are directly reduced to form rhodium metal nano particles, and the reduction reaction speed is high. Moreover, the preparation method of the rhodium metal nano-particles provided by the invention is simple, can be carried out at normal temperature and normal pressure, does not need to introduce a new reducing agent, and is environment-friendly. In addition, the rhodium metal nanoparticles prepared by the preparation method of the rhodium metal nanoparticles have the advantages of small particle size, high purity, uniform particles, good catalytic performance and wide application prospect.
Detailed Description
In order that the present invention may be more readily understood, the following detailed description of the invention is given by way of example only, and is not intended to limit the scope of the invention.
In view of the fact that the existing method for preparing metal nanoparticles needs to introduce a new chemical reduction reagent, which not only has a great influence on the environment, but also has more post-treatment steps, and the result is not easy to control, and the existing method for preparing nanoparticles by adopting plasma glow discharge also has the defects of higher voltage, lower gas pressure, long reduction reaction time and larger particle size of the obtained nanoparticles, the inventor of the invention finds through repeated experimental research that rhodium-containing solution can be prepared and obtained under the conditions of lower discharge voltage, normal temperature and pressure and shorter reduction reaction time by adding an auxiliary agent; meanwhile, the prepared rhodium metal nano particles have small particle size and high purity. The present invention has been made based on the above findings.
Therefore, the invention provides a preparation method of rhodium metal nanoparticles, which comprises the step of subjecting a mixed solution containing a rhodium solution and an auxiliary agent to plasma glow discharge treatment so as to reduce rhodium ions in the mixed solution into the rhodium metal nanoparticles.
Specifically, the preparation method of the rhodium metal nanoparticles provided by the invention comprises the following steps:
s1, placing the mixed solution containing the rhodium solution and the auxiliary agent in the plasma discharge gas atmosphere;
and S2, under the action of alternating current, enabling the plasma formed by the discharge of the plasma discharge gas to reduce rhodium ions in the mixed solution into rhodium metal nano particles.
The rhodium-containing solution of the present invention comprises a salt solution of rhodium metal, preferably a chloride solution of rhodium metal. And reducing rhodium ions in the rhodium metal salt in the rhodium-containing solution into rhodium metal nano particles through plasma glow discharge treatment.
In step S1, the auxiliary agent includes perchloric acid. The perchloric acid used in the present invention is pure perchloric acid. The auxiliary agent in the invention plays a role in destroying organic matters in the rhodium-containing solution, so that rhodium metal is completely released, and rhodium ions can be more rapidly and effectively reduced by the rhodium-containing solution under the glow discharge condition.
In step S1, the addition amount of the auxiliary agent is 1 (10-25) mol/g, preferably 1 (15-25) mol/g, and more preferably 1 (15-20) mol/g, based on the ratio of the molar amount of the rhodium ions in the rhodium-containing solution to the mass of the auxiliary agent. The invention can realize better rhodium reduction effect under the condition of less additive amount of the auxiliary agent.
In step S2, the plasma discharge gas is a gas plasma capable of generating positively and negatively charged ions at high pressure. The plasma discharge gas comprises one or more of an inert gas, nitrogen and air, preferably an inert gas, more preferably argon. The inventors of the present invention have found that the selectivity and efficiency of the inert gas are higher compared to nitrogen and air because: (1) inert gases and other elements are difficult to form in a stable compound form; (2) inert gas, such as argon, has a high first ionization point, and the formed argon anions exist as electron-rich substances, so that high energy can be provided to act on rhodium ions to be reduced into rhodium metal nanoparticles, and finally the argon anions become argon.
In step S2, the voltage of the alternating current is 150 to 500V, preferably 150 to 400V, more preferably 150 to 300V. The reduction time is 3-15min, preferably 5-15min, and more preferably 7-15 min. In the present invention, the discharge voltage (ac voltage) needs to be strictly controlled. Too low a discharge voltage results in a weak reduction reaction; the discharge voltage is too high, so that the requirements on equipment, a grounding environment and the like are high, and the requirements are difficult to meet in practical application.
The rhodium metal nanoparticles prepared by the method have a particle size of 7-20 nm.
The starting materials used in the present invention are commercially available unless otherwise specified.
The operations and treatments involved in the present invention are conventional in the art unless otherwise specified.
The apparatus used in the present invention is an apparatus conventional in the art unless otherwise specified.
The purity of the rhodium metal nanoparticles was analyzed by an ICP (inductively coupled plasma emission spectrometer) after the rhodium metal nanoparticles were dissolved by energization with concentrated hydrochloric acid (37 wt%).
Examples
Example 1
Will contain H3RhCl6、FeCl3And NiCl2Mixed solution (H) of rhodium-containing solution and pure perchloric acid3RhCl6Molar amount of rhodium ion and HClO4The mass ratio of the components is 1:25mol/g) is arranged between two electrode plates of a discharge tube in a vacuum chamber, the vacuum chamber is sealed, then argon is filled as discharge gas, the normal pressure is realized, 150V alternating voltage is applied to the electrodes, and H is reduced by adopting plasma glow discharge3RhCl6Reducing for 8min to obtain rhodium metal nanoparticles with purity of 99.95% by transmission electron microscopeThe particle size was measured to be 7-14 nm.
Example 2
Will contain H3RhCl6、Fe2(SO4)3And NiSO4Mixed solution (H) of rhodium-containing solution and pure perchloric acid3RhCl6Molar amount of rhodium ion and HClO4The mass ratio of the components is 1:15mol/g) is arranged between two electrode plates of a discharge tube in a vacuum chamber, the vacuum chamber is sealed, the vacuum chamber is vacuumized, then air is filled as discharge gas, the normal pressure is realized, 300V alternating voltage is applied to the electrodes, and H is reduced by adopting plasma glow discharge3RhCl6And the reduction time is 15min, so that the rhodium metal nano-particles with the purity of 99.95 percent and the particle size of 9-17nm are prepared by adopting a transmission electron microscope.
Example 3
Will contain H3RhCl6、Fe2(SO4)3And NiCl2Mixed solution (H) of rhodium-containing solution and pure perchloric acid3RhCl6Molar amount of rhodium ion and HClO4The mass ratio of the components is 1:20mol/g) is arranged between two electrode plates of a discharge tube in a vacuum chamber, the vacuum chamber is sealed, air is filled in the vacuum chamber to be used as discharge gas, the voltage is applied to the electrodes at normal pressure, 350V alternating voltage is applied to the electrodes, and H is reduced by adopting plasma glow discharge3RhCl6And the reduction time is 5min, so that the rhodium metal nano-particles with the purity of 99.95 percent and the particle size of 10-20nm measured by a transmission electron microscope are prepared.
Example 4
Will contain H3RhCl6And NiCl2Mixed solution (H) of rhodium-containing solution and pure perchloric acid3RhCl6Molar amount of rhodium ion and HClO4The mass ratio of the components is 1:25mol/g) is arranged between two electrode plates of a discharge tube in a vacuum chamber, the vacuum chamber is sealed, then argon is filled as discharge gas, the normal pressure is realized, the alternating voltage of 400V is applied to the electrodes, and the H is reduced by adopting plasma glow discharge3RhCl6And the reduction time is 7min, so that the rhodium metal nano-particles with the purity of 99.95 percent and the particle size of 7-20nm are prepared by adopting a transmission electron microscope.
Example 5
Will contain H3RhCl6、Fe2(SO4)3And NiSO4Mixed solution (H) of rhodium-containing solution and pure perchloric acid3RhCl6Molar amount of rhodium ion and HClO4The mass ratio of the components is 1:10mol/g) is arranged between two electrode plates of a discharge tube in a vacuum chamber, the vacuum chamber is sealed, air is filled in the vacuum chamber to be used as discharge gas, the voltage is applied to the electrodes at normal pressure, 500V alternating voltage is applied to the electrodes, and H is reduced by adopting plasma glow discharge3RhCl6And the reduction time is 3min, so that the rhodium metal nano-particles with the purity of 99.95 percent and the particle size of 7-20nm are prepared by adopting a transmission electron microscope.
Comparative example 1
Will contain H3RhCl6、FeCl3And NiCl2Mixed solution (H) of rhodium-containing solution and pure perchloric acid3RhCl6Molar amount of rhodium ion and HClO4The mass ratio of the components is 1:25mol/g) is arranged between two electrode plates of a discharge tube in a vacuum chamber, the vacuum chamber is sealed, the vacuum chamber is vacuumized, then air is filled as discharge gas, the voltage is applied to the electrodes at normal pressure, 100V alternating voltage is applied to the electrodes, and H is reduced by adopting plasma glow discharge3RhCl6The reduction time is 3min, and the rhodium-containing solution has no obvious change.
The embodiment shows that the preparation method of the rhodium metal nanoparticles is simple, can be carried out at normal temperature and normal pressure, does not need to introduce a new reducing agent, and is environment-friendly. In addition, the rhodium metal nanoparticles prepared by the preparation method of the rhodium metal nanoparticles have small particle size, high purity and wide application prospect.
It should be noted that the above-mentioned embodiments are only for explaining the present invention, and do not constitute any limitation to the present invention. The present invention has been described with reference to exemplary embodiments, but the words which have been used herein are words of description and illustration, rather than words of limitation. The invention can be modified, as prescribed, within the scope of the claims and without departing from the scope and spirit of the invention. Although the invention has been described herein with reference to particular means, materials and embodiments, the invention is not intended to be limited to the particulars disclosed herein, but rather extends to all other methods and applications having the same functionality.
Claims (10)
1. A preparation method of rhodium metal nanoparticles comprises the step of subjecting a mixed solution containing a rhodium solution and an auxiliary agent to plasma glow discharge treatment, so that rhodium ions in the mixed solution are reduced into the rhodium metal nanoparticles.
2. The preparation method according to claim 1, wherein the method for subjecting the mixed solution containing the rhodium solution and the auxiliary agent to plasma glow discharge treatment comprises the following steps:
putting the mixed solution containing the rhodium solution and the auxiliary agent in a plasma discharge gas atmosphere;
under the action of alternating current, the rhodium ions in the mixed solution are reduced into rhodium metal nano particles by plasma formed by plasma discharge gas discharge.
3. The method of claim 2, wherein the plasma discharge gas comprises one or more of an inert gas, nitrogen, and air.
4. The method of claim 3, wherein the inert gas is argon.
5. A method according to any of claims 2-4, characterized in that the voltage of the alternating current is 150-500V, preferably 150-400V.
6. The method according to any one of claims 1 to 5, wherein the reduction is carried out for a period of 3 to 15min, preferably 5 to 15 min.
7. The method according to any one of claims 1 to 6, wherein the addition amount of the auxiliary agent is 1 (10 to 25) mol/g, preferably 1 (15 to 20) mol/g, based on the ratio of the molar amount of rhodium ions in the rhodium-containing solution to the mass of the auxiliary agent.
8. A method according to any one of claims 1 to 7, wherein the rhodium-containing solution comprises a solution of a salt of rhodium metal, preferably a solution of a chloride of rhodium metal.
9. The method according to any one of claims 1 to 8, wherein the adjuvant comprises perchloric acid.
10. The method of any one of claims 1-9, wherein the rhodium metal nanoparticles have a particle size of 7-20 nm.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113618076A (en) * | 2021-07-21 | 2021-11-09 | 无锡威孚环保催化剂有限公司 | Sponge rhodium powder and preparation method thereof |
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| CN113618076A (en) * | 2021-07-21 | 2021-11-09 | 无锡威孚环保催化剂有限公司 | Sponge rhodium powder and preparation method thereof |
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