CN113427012A - Method for preparing nano metal powder - Google Patents
Method for preparing nano metal powder Download PDFInfo
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- CN113427012A CN113427012A CN202110828928.9A CN202110828928A CN113427012A CN 113427012 A CN113427012 A CN 113427012A CN 202110828928 A CN202110828928 A CN 202110828928A CN 113427012 A CN113427012 A CN 113427012A
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- sulfide
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- nano metal
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- 239000000843 powder Substances 0.000 title claims abstract description 57
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 33
- 239000002184 metal Substances 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title claims abstract description 16
- 238000000498 ball milling Methods 0.000 claims abstract description 42
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000012265 solid product Substances 0.000 claims abstract description 24
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910000103 lithium hydride Inorganic materials 0.000 claims abstract description 15
- 239000000463 material Substances 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 8
- 229910052976 metal sulfide Inorganic materials 0.000 claims abstract description 8
- 238000002791 soaking Methods 0.000 claims abstract description 3
- 238000005406 washing Methods 0.000 claims abstract description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 229910052786 argon Inorganic materials 0.000 claims description 6
- 238000004108 freeze drying Methods 0.000 claims description 6
- 238000001291 vacuum drying Methods 0.000 claims description 6
- 239000001307 helium Substances 0.000 claims description 5
- 229910052734 helium Inorganic materials 0.000 claims description 5
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- MBMLMWLHJBBADN-UHFFFAOYSA-N Ferrous sulfide Chemical compound [Fe]=S MBMLMWLHJBBADN-UHFFFAOYSA-N 0.000 claims description 3
- 239000005083 Zinc sulfide Substances 0.000 claims description 3
- XUKVMZJGMBEQDE-UHFFFAOYSA-N [Co](=S)=S Chemical compound [Co](=S)=S XUKVMZJGMBEQDE-UHFFFAOYSA-N 0.000 claims description 3
- NGTSQWJVGHUNSS-UHFFFAOYSA-N bis(sulfanylidene)vanadium Chemical compound S=[V]=S NGTSQWJVGHUNSS-UHFFFAOYSA-N 0.000 claims description 3
- OMZSGWSJDCOLKM-UHFFFAOYSA-N copper(II) sulfide Chemical compound [S-2].[Cu+2] OMZSGWSJDCOLKM-UHFFFAOYSA-N 0.000 claims description 3
- 239000011261 inert gas Substances 0.000 claims description 3
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 claims description 3
- 229910052982 molybdenum disulfide Inorganic materials 0.000 claims description 3
- WWNBZGLDODTKEM-UHFFFAOYSA-N sulfanylidenenickel Chemical compound [Ni]=S WWNBZGLDODTKEM-UHFFFAOYSA-N 0.000 claims description 3
- CFJRPNFOLVDFMJ-UHFFFAOYSA-N titanium disulfide Chemical compound S=[Ti]=S CFJRPNFOLVDFMJ-UHFFFAOYSA-N 0.000 claims description 3
- ITRNXVSDJBHYNJ-UHFFFAOYSA-N tungsten disulfide Chemical compound S=[W]=S ITRNXVSDJBHYNJ-UHFFFAOYSA-N 0.000 claims description 3
- 229910052984 zinc sulfide Inorganic materials 0.000 claims description 3
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 claims description 3
- DBULDCSVZCUQIR-UHFFFAOYSA-N chromium(3+);trisulfide Chemical compound [S-2].[S-2].[S-2].[Cr+3].[Cr+3] DBULDCSVZCUQIR-UHFFFAOYSA-N 0.000 claims description 2
- 238000007789 sealing Methods 0.000 claims description 2
- CADICXFYUNYKGD-UHFFFAOYSA-N sulfanylidenemanganese Chemical compound [Mn]=S CADICXFYUNYKGD-UHFFFAOYSA-N 0.000 claims description 2
- 239000007769 metal material Substances 0.000 abstract description 5
- 238000009776 industrial production Methods 0.000 abstract description 4
- 238000006555 catalytic reaction Methods 0.000 abstract description 3
- 238000012824 chemical production Methods 0.000 abstract description 3
- 239000003814 drug Substances 0.000 abstract description 3
- 238000004146 energy storage Methods 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 239000002086 nanomaterial Substances 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract 1
- 238000002156 mixing Methods 0.000 description 9
- 238000003756 stirring Methods 0.000 description 9
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 4
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 4
- 238000001000 micrograph Methods 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 229910052721 tungsten Inorganic materials 0.000 description 3
- 239000010937 tungsten Substances 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
- 239000011733 molybdenum Substances 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000004870 electrical engineering Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Images
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
- 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
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
-
- 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)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Crystallography & Structural Chemistry (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Physics & Mathematics (AREA)
- Materials Engineering (AREA)
- Composite Materials (AREA)
- Manufacturing & Machinery (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
A method for preparing nano metal powder relates to the technical field of metal nano material synthesis, lithium hydride and metal sulfide are used as raw materials, the lithium hydride and the metal sulfide are added into a ball milling tank according to the mol ratio of 1: 0.1-10 under the protection of inert atmosphere, the weight ratio of materials to balls is 1: 20-50, and ball milling is carried out for 10-60 hours at the rotating speed of 50-1000 rpm. And (4) taking out the solid product after the ball milling is finished, soaking the solid product in ethanol, washing, centrifuging and drying to obtain the nano metal powder. The method is simple and easy to control, has high efficiency and low cost, and is easy to realize industrial production. The prepared nano metal material can be used in the fields of chemical production, energy storage catalysis, electronics and electricians, biological medicine and the like.
Description
Technical Field
The invention relates to the technical field of metal nano material synthesis, in particular to a method for preparing nano metal powder.
Background
The nano metal material has wide application in the fields of chemical production, energy storage catalysis, electronic and electrical engineering, biological medicine and the like. The existing mature method for synthesizing the nano metal material mainly comprises the following steps: inert gas evaporation, high temperature pressurization, chemical hydrothermal synthesis, etc.
The preparation methods of the nano metal materials have the defects of complex process, high energy consumption, low yield, high cost and the like, and are not beneficial to large-scale production. Therefore, the preparation method of the novel nano metal powder, which is efficient, energy-saving, environment-friendly, low in cost and easy for industrial production, has important significance.
Disclosure of Invention
The invention aims to provide a novel method for preparing nano metal powder, which is efficient, economical, environment-friendly, low in cost and easy for industrial production.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: a method for preparing nano metal powder by utilizing lithium hydride and metal sulfide to react under the condition of ball milling to generate the nano metal powder specifically comprises the following steps:
(1) under the protection of inert atmosphere, adding lithium hydride and metal sulfide into a ball-milling tank according to the molar ratio of 1: 0.1-10, and sealing the ball-milling tank, wherein the weight ratio of materials to balls in the ball-milling tank is 1: 20-50;
(2) ball milling for 10-60 h at the rotating speed of 50-1000 rpm;
(3) and (4) taking out the solid product after the ball milling is finished, soaking the solid product in ethanol, washing, centrifuging and drying to obtain the nano metal powder.
As a preferred technical scheme of the invention, the preparation method comprises the following steps:
the inert gas in the step (1) is one or more of nitrogen, argon and helium.
The metal sulfide in the step (1) is one of molybdenum disulfide, tungsten disulfide, copper sulfide, ferrous sulfide, cobalt disulfide, manganese sulfide, zinc sulfide, titanium disulfide, vanadium disulfide, nickel sulfide and chromium sulfide.
The drying in the step (3) comprises normal pressure drying, freeze drying or vacuum drying.
Compared with the prior art, the invention has the beneficial effects that:
(1) the method is simple and easy to control, energy-saving and environment-friendly, low in cost and easy for industrial production.
(2) The nano metal material prepared by the method can be used in the fields of chemical production, energy storage catalysis, electronics and electricians, biological medicine and the like.
Drawings
Fig. 1 is an X-ray diffraction pattern of the nano-metal powder prepared in example 1.
Fig. 2 is a transmission electron microscope image of the nano metal powder prepared in example 1.
Fig. 3 is an X-ray diffraction pattern of the nano-metal powder prepared in example 2.
Fig. 4 is a transmission electron microscope photograph of the nano metal powder prepared in example 2.
Detailed Description
Example 1
Under the protection of argon gas, lithium hydride powder and molybdenum disulfide powder are mixed according to a molar ratio of 2: 1, mixing and ball milling for 30 hours, wherein the weight ratio of materials to balls is 1: 50, and the ball milling rotating speed is 580 rpm. And after the ball milling is finished, taking out the powder, adding the powder into ethanol, continuously stirring, centrifugally separating out a solid product, and performing vacuum drying to obtain the solid product, namely the uniformly dispersed nano-metal molybdenum.
Fig. 1 is an X-ray diffraction pattern of the nano-metal powder prepared in example 1, and fig. 2 is a transmission electron microscope image of the nano-metal powder prepared in example 1. From FIG. 1, it can be seen that the diffraction peak position of the sample completely corresponds to the PDF # -42-1120 card of molybdenum, indicating that the nano-metal molybdenum powder is successfully prepared by the invention. As can be seen from FIG. 2, the prepared molybdenum metal particles are ellipsoidal, the size distribution is 5-20 nm, the morphology is uniform, and the dispersibility is high.
Example 2
Under the protection of argon gas, lithium hydride powder and tungsten disulfide powder are mixed according to a molar ratio of 4: 1, mixing and ball milling for 36h, wherein the weight ratio of materials to balls is 1: 45, and the ball milling rotating speed is 500 rpm. And after the ball milling is finished, taking out the powder, adding the powder into ethanol, continuously stirring, centrifugally separating out a solid product, and performing vacuum drying to obtain the solid product, namely the uniformly dispersed nano metal tungsten.
Fig. 3 is an X-ray diffraction pattern of the nano-metal powder prepared in example 2, and fig. 4 is a transmission electron microscope image of the nano-metal powder prepared in example 2. From FIG. 3, it can be seen that the diffraction peak position of the sample completely corresponds to the PDF # -04-0806 card of tungsten, indicating that the nano-metal tungsten powder is successfully prepared by the invention. As can be seen from FIG. 4, the prepared metal tungsten particles are spherical, the size distribution is 5-10 nm, the morphology is uniform, and the dispersibility is high.
Example 3
Under the protection of helium, lithium hydride powder and copper sulfide powder are mixed according to a molar ratio of 2: 1, mixing and ball milling for 24 hours, wherein the weight ratio of materials to balls is 1: 40, and the ball milling rotating speed is 100 rpm. And after the ball milling is finished, taking out the powder, adding the powder into ethanol, continuously stirring, centrifugally separating out a solid product, and freeze-drying to obtain the solid product, namely the uniformly dispersed nano metal copper.
Example 4
Under the protection of nitrogen, lithium hydride powder and ferrous sulfide powder are mixed according to a molar ratio of 2: 1, mixing and ball milling for 48 hours, wherein the weight ratio of materials to balls is 1: 20, and the ball milling rotating speed is 200 rpm. And after the ball milling is finished, taking out the powder, adding the powder into ethanol, continuously stirring, centrifugally separating out a solid product, and drying under normal pressure to obtain the solid product, namely the uniformly dispersed nano metallic iron.
Example 5
Under the protection of argon, lithium hydride powder and cobalt disulfide powder are mixed according to a molar ratio of 4: 1, mixing and ball milling for 48 hours, wherein the weight ratio of materials to balls is 1: 25, and the ball milling rotating speed is 350 rpm. And after the ball milling is finished, taking out the powder, adding the powder into ethanol, continuously stirring, centrifugally separating out a solid product, and freeze-drying to obtain the solid product, namely the uniformly dispersed nano metal cobalt.
Example 6
Under the protection of helium, lithium hydride powder and zinc sulfide powder are mixed according to a molar ratio of 2: 1, mixing and ball milling for 30 hours, wherein the weight ratio of materials to balls is 1: 30, and the ball milling rotating speed is 750 rpm. And after the ball milling is finished, taking out the powder, adding the powder into ethanol, continuously stirring, centrifugally separating out a solid product, and performing vacuum drying to obtain the solid product, namely the uniformly dispersed nano metal zinc.
Example 7
Under the protection of nitrogen, lithium hydride powder and titanium disulfide powder are mixed according to a molar ratio of 4: 1, mixing and ball milling for 48 hours, wherein the weight ratio of materials to balls is 1: 35, and the ball milling rotating speed is 500 rpm. And after the ball milling is finished, taking out the powder, adding the powder into ethanol, continuously stirring, centrifugally separating out a solid product, and freeze-drying to obtain the solid product, namely the uniformly dispersed nano metal titanium.
Example 8
Under the condition of helium protection, lithium hydride powder and nickel sulfide powder are mixed according to a molar ratio of 2: 1, mixing and ball milling for 60 hours, wherein the weight ratio of materials to balls is 1: 40, and the ball milling rotating speed is 400 rpm. And after the ball milling is finished, taking out the powder, adding the powder into ethanol, continuously stirring, centrifugally separating out a solid product, and performing vacuum drying to obtain the solid product, namely the uniformly dispersed nano metallic nickel.
Example 9
Under the protection of argon, lithium hydride powder and vanadium disulfide powder are mixed according to a molar ratio of 4: 1, mixing and ball milling for 30 hours, wherein the weight ratio of materials to balls is 1: 30, and the ball milling rotating speed is 100 rpm. And after the ball milling is finished, taking out the powder, adding the powder into ethanol, continuously stirring, centrifugally separating out a solid product, and freeze-drying to obtain the solid product, namely the uniformly dispersed nano metal vanadium.
The foregoing is merely exemplary and illustrative of the principles of the present invention and various modifications, additions and substitutions of the specific embodiments described herein may be made by those skilled in the art without departing from the principles of the present invention or exceeding the scope of the claims set forth herein.
Claims (4)
1. The method for preparing the nano metal powder is characterized in that lithium hydride and metal sulfide react under the ball milling condition to generate the nano metal powder, and the method specifically comprises the following steps:
(1) under the protection of inert atmosphere, adding lithium hydride and metal sulfide into a ball-milling tank according to the molar ratio of 1: 0.1-10, and sealing the ball-milling tank, wherein the weight ratio of materials to balls in the ball-milling tank is 1: 20-50;
(2) ball milling for 10-60 h at the rotating speed of 50-1000 rpm;
(3) and (4) taking out the solid product after the ball milling is finished, soaking the solid product in ethanol, washing, centrifuging and drying to obtain the nano metal powder.
2. The method of claim 1, wherein: the inert gas in the step (1) is one or more of nitrogen, argon and helium.
3. The method of claim 1, wherein: the metal sulfide in the step (1) is one of molybdenum disulfide, tungsten disulfide, copper sulfide, ferrous sulfide, cobalt disulfide, manganese sulfide, zinc sulfide, titanium disulfide, vanadium disulfide, nickel sulfide and chromium sulfide.
4. The method of claim 1, wherein: the drying in the step (3) comprises normal pressure drying, freeze drying or vacuum drying.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110828928.9A CN113427012A (en) | 2021-07-21 | 2021-07-21 | Method for preparing nano metal powder |
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| CN202110828928.9A CN113427012A (en) | 2021-07-21 | 2021-07-21 | Method for preparing nano metal powder |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114682786A (en) * | 2022-04-06 | 2022-07-01 | 合肥学院 | Preparation method of micro-nano metal powder |
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- 2021-07-21 CN CN202110828928.9A patent/CN113427012A/en active Pending
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