CN115194173A - Novel preparation method of nano-zirconia dispersion strengthened platinum - Google Patents
Novel preparation method of nano-zirconia dispersion strengthened platinum Download PDFInfo
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- CN115194173A CN115194173A CN202210625151.0A CN202210625151A CN115194173A CN 115194173 A CN115194173 A CN 115194173A CN 202210625151 A CN202210625151 A CN 202210625151A CN 115194173 A CN115194173 A CN 115194173A
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- zirconia
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- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 title claims abstract description 80
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 title claims abstract description 64
- 229910052697 platinum Inorganic materials 0.000 title claims abstract description 36
- 239000006185 dispersion Substances 0.000 title claims abstract description 14
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000000463 material Substances 0.000 claims abstract description 22
- 239000000843 powder Substances 0.000 claims abstract description 20
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 16
- 239000002253 acid Substances 0.000 claims abstract description 11
- 238000005242 forging Methods 0.000 claims abstract description 8
- 238000003825 pressing Methods 0.000 claims abstract description 8
- 238000001354 calcination Methods 0.000 claims abstract description 7
- 238000005245 sintering Methods 0.000 claims abstract description 7
- 238000001556 precipitation Methods 0.000 claims abstract description 6
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 16
- 238000010438 heat treatment Methods 0.000 claims description 12
- 235000019270 ammonium chloride Nutrition 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 239000002244 precipitate Substances 0.000 claims description 5
- 239000012065 filter cake Substances 0.000 claims description 4
- 239000000706 filtrate Substances 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 230000007935 neutral effect Effects 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 claims 1
- 238000005728 strengthening Methods 0.000 abstract description 3
- 239000013078 crystal Substances 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract description 2
- 238000002156 mixing Methods 0.000 abstract description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000003365 glass fiber Substances 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000006722 reduction reaction Methods 0.000 description 2
- ZSLUVFAKFWKJRC-IGMARMGPSA-N 232Th Chemical compound [232Th] ZSLUVFAKFWKJRC-IGMARMGPSA-N 0.000 description 1
- 229910001260 Pt alloy Inorganic materials 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 229910052776 Thorium Inorganic materials 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052790 beryllium Inorganic materials 0.000 description 1
- ATBAMAFKBVZNFJ-UHFFFAOYSA-N beryllium atom Chemical compound [Be] ATBAMAFKBVZNFJ-UHFFFAOYSA-N 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000000156 glass melt Substances 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- PXXKQOPKNFECSZ-UHFFFAOYSA-N platinum rhodium Chemical compound [Rh].[Pt] PXXKQOPKNFECSZ-UHFFFAOYSA-N 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 150000003839 salts Chemical group 0.000 description 1
- 239000003238 silicate melt Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
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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
- 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
- B22F1/12—Metallic powder containing non-metallic 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
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- 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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- 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)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention provides a novel preparation method of nano-zirconia dispersion strengthened platinum, which is used for realizing the strengthening effect of nano-zirconia in a strengthened platinum material and improving the high-temperature performance and the processing performance of the strengthened platinum material. The method introduces nano zirconia seed crystals in the ammonium precipitation process of chloroplatinic acid, and then forms ammonium chloroplatinate powder containing nano zirconia by crushing and mixing. Then decomposing ammonium chloroplatinate by a calcination reduction method to prepare platinum powder, and preparing the nano zirconia dispersion strengthened platinum material by the working procedures of pressing, sintering, forging and the like.
Description
Technical Field
The invention relates to a production method for preparing a dispersion-strengthened platinum material, in particular to a novel preparation method for nano zirconia dispersion-strengthened platinum, and belongs to the technical field of metal materials.
Background
The platinum metal has excellent chemical stability and higher melting point, the melting point is 1769 ℃, meanwhile, the platinum metal also has good corrosion resistance to various molten oxides, glass and silicate melts, and the platinum-based glass fiber bushing processed by platinum is common high-temperature equipment in the glass fiber industry at present. However, since the platinum equipment is used under a high temperature condition for a long time, the grains in the microstructure of pure platinum and platinum alloys can grow seriously, and the high temperature strength and the mechanical property stability of the equipment are further influenced.
At present, a novel structural material dispersion-strengthened platinum-rhodium material taking oxides of zirconium, yttrium, thorium, beryllium and the like as dispersion-strengthened phases is widely developed and used for improving the high-temperature performance and prolonging the service life of platinum equipment. How to improve the strength, toughness and dispersivity of the nano-zirconia dispersion-strengthened platinum can greatly improve the performance of the nano-zirconia dispersion-strengthened platinum.
Disclosure of Invention
The invention provides a novel preparation method of nano-zirconia dispersion-strengthened platinum, and the obtained material has the characteristics of high strength, high toughness, high dispersion and the like. Compared with the traditional internal oxidation method and the powder metallurgy method, the method avoids the processes of smelting, powder making, high-temperature oxidation and the like in the preparation process, and also avoids the defects of uneven dispersion, uncontrollable size and the like of the reinforced material.
A novel preparation method of nano-zirconia dispersion strengthened platinum comprises the following steps:
step 1, adding a proper amount of nano zirconia powder into a chloroplatinic acid solution, and uniformly stirring; preferably, the zirconia powder has a particle size of 10 to 100nm. The concentration of platinum in the chloroplatinic acid solution is 50-400g/L, the mass ratio of the zirconium oxide to the chloroplatinic acid is 0.01-0.5.
Step 2, adding a proper amount of ammonium chloride into the solution obtained in the step 1, and heating and stirring until ammonium chloroplatinate is completely precipitated; preferably, the mass ratio of the ammonium chloride to the chloroplatinic acid is 1-5.
Step 3, filtering, washing a filter cake by using an ammonium chloride solution, drying, placing ammonium chloroplatinate precipitate containing nano zirconia into a crusher, and crushing into powder; preferably, the rotating speed of the crusher for precipitation is 1000-5000r/min, and the crushing time is 5-20min.
Step 4, placing the powder in a calcining furnace, heating until ammonium chloroplatinate is completely decomposed, washing the reduced powder (namely, the powder obtained after heating until ammonium chloroplatinate is completely decomposed) by pure water until the pH value of the filtrate is neutral, and further preparing a platinum powder material containing nano zirconia; preferably, the heating temperature of the calcining furnace is 400-600 ℃, and the heating time is 1-4h.
And 5, performing pressing, sintering and forging processes on the obtained material to prepare the nano zirconia dispersion strengthened platinum finished material. Preferably, the pressing weight of the press is 50-500t, the sintering temperature is 600-1500 ℃, and the forging temperature is 1200-1500 ℃.
The invention has the following beneficial effects: the invention provides a novel preparation method of nano-zirconia dispersion strengthened platinum, which is used for realizing the strengthening effect of nano-zirconia in a strengthened platinum material and improving the high-temperature performance and the processing performance of the strengthened platinum material. The method introduces nano zirconia seed crystals in the ammonium precipitation process of chloroplatinic acid, and then forms ammonium chloroplatinate powder containing nano zirconia by crushing and mixing. And then decomposing ammonium chloroplatinate by a calcination reduction method to prepare platinum powder, and preparing the nano zirconia dispersion strengthened platinum material by the working procedures of pressing, sintering, forging and the like.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention. In the drawings:
FIG. 1 is a diagram of enhanced nanophase distribution.
Detailed Description
The following description of the preferred embodiments of the present invention is provided for the purpose of illustration and description, and is in no way intended to limit the invention.
Examples
A new preparation method of nano-zirconia dispersion strengthened platinum comprises the following steps:
step 1, taking 0.2g of nano zirconia powder with the size of 20nm, adding the nano zirconia powder into 1L of chloroplatinic acid solution with the concentration of 200g/L, and stirring for 1h to be in a uniform state;
step 2, adding 300g of ammonium chloride solid into the solution obtained in the step 1, heating to 80 ℃, and stirring until ammonium chloroplatinate is completely precipitated, wherein the reaction time is 1h;
and 3, filtering the yellow precipitate by using a funnel, and washing a filter cake by using an ammonium chloride solution until the filtrate is colorless. Drying the filter cake in a vacuum oven, placing the ammonium chloroplatinate precipitate containing nano zirconia in a crusher, crushing for 10min at the rotation speed of 4000r/min, and crushing the precipitate into powder;
step 4, placing the powder in a calcining furnace, controlling the heating temperature to be 600 ℃, heating for 3 hours until ammonium chloroplatinate is completely decomposed, washing the reduced powder with pure water until the pH value of the filtrate is neutral, and further preparing a platinum powder material containing nano zirconia;
and 5, pressing the platinum powder, wherein the pressing weight of a press is 400t, and then placing the pressed material into a high-temperature furnace for high-temperature sintering at 1250 ℃. And (3) placing the sintered material on an air hammer to complete a forging process, wherein the forging temperature is 1200 ℃, and finally preparing the nano zirconia dispersion strengthened platinum finished product material.
The tensile strength of the reinforced platinum prepared by the embodiment at high temperature (1100 ℃) is improved by more than 10 percent compared with that of the traditional reinforced platinum, and the lasting time at high temperature (1400 ℃,10.8 MPa) is improved by more than 30 percent compared with that of the traditional reinforced platinum.
The size of the strengthening phase can be controlled within 100nm. Compared with other chemical reduction methods, the powder material has no salt residue. FIG. 1 is a diagram of enhanced nanophase distribution.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the embodiments described above, or equivalents may be substituted for elements thereof. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (6)
1. A novel preparation method of nano-zirconia dispersion strengthened platinum is characterized by comprising the following steps:
step 1, adding a proper amount of nano zirconia powder into a chloroplatinic acid solution, and uniformly stirring;
step 2, adding a proper amount of ammonium chloride into the solution obtained in the step 1, and heating and stirring until ammonium chloroplatinate is completely precipitated;
step 3, filtering, washing a filter cake by using an ammonium chloride solution, drying, placing ammonium chloroplatinate precipitate containing nano zirconia into a crusher, and crushing into powder;
step 4, placing the powder in a calcining furnace, heating until ammonium chloroplatinate is completely decomposed, washing the reduced powder with pure water until the pH value of the filtrate is neutral, and further preparing a platinum powder material containing nano zirconia;
and 5, pressing, sintering and forging the material obtained in the step 4 to prepare the nano zirconia dispersion strengthened platinum finished material.
2. The novel preparation method of nano-zirconia dispersion-strengthened platinum according to claim 1, wherein in the step 1, the particle size of the zirconia powder is 10-100nm, the concentration of platinum in the chloroplatinic acid solution is 50-400g/L, the mass ratio of the zirconia to the chloroplatinic acid is 0.01-0.5.
3. The novel preparation method of nano zirconia dispersion-strengthened platinum as claimed in claim 1, wherein the mass ratio of ammonium chloride to chloroplatinic acid in step 2 is 1-5, the precipitation reaction time is 0.5-2h, and the precipitation reaction temperature is 50-90 ℃.
4. The method for preparing nano-zirconia dispersion-strengthened platinum according to claim 1, wherein in the step 3, the rotating speed of a crusher used for precipitation is 1000-5000r/min, and the crushing time is 5-20min.
5. The novel preparation method of nano-zirconia dispersion-strengthened platinum as claimed in claim 1, wherein the heating temperature of the calcining furnace in the step 4 is 400-600 ℃, and the heating time is 1-4h.
6. The novel preparation method of the nano-zirconia dispersion-strengthened platinum as claimed in claim 1, wherein the pressing weight of the press in the step 5 is 50-500t, the sintering temperature is 600-1500 ℃, and the forging temperature is 1200-1500 ℃.
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| CN202210625151.0A CN115194173B (en) | 2022-06-02 | 2022-06-02 | New preparation method of nano zirconia dispersion strengthening platinum |
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| CN202210625151.0A CN115194173B (en) | 2022-06-02 | 2022-06-02 | New preparation method of nano zirconia dispersion strengthening platinum |
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1383456A (en) * | 2000-06-28 | 2002-12-04 | 田中贵金属工业株式会社 | Method for producing platinum material reinforced with dispersed oxide |
| JP2008106349A (en) * | 2006-09-28 | 2008-05-08 | Kojima Kagaku Yakuhin Kk | Method for producing platinum powder |
| CN102296183A (en) * | 2011-08-19 | 2011-12-28 | 天津市化学试剂研究所 | Method for preparing high-purity platinum |
| CN103146942A (en) * | 2013-03-29 | 2013-06-12 | 吉林大学 | Nano-zironia dispersion strengthening diamond composite material and preparation method thereof |
| CN104328301A (en) * | 2014-07-18 | 2015-02-04 | 河南科技大学 | Preparation method of particular-reinforced molybdenum-based composite material |
| CN104550931A (en) * | 2014-12-25 | 2015-04-29 | 铜陵市经纬流体科技有限公司 | Scattering particle reinforced iron-based powder metallurgical valve and preparation method thereof |
| CN106191508A (en) * | 2016-08-31 | 2016-12-07 | 无锡英特派金属制品有限公司 | A kind of ZrO2 dispersion intensifying platinum or the preparation method of platinum rhodium |
| CN113337786A (en) * | 2021-05-31 | 2021-09-03 | 华中科技大学 | Nano zirconium oxide/amorphous alloy composite material and preparation method thereof |
-
2022
- 2022-06-02 CN CN202210625151.0A patent/CN115194173B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1383456A (en) * | 2000-06-28 | 2002-12-04 | 田中贵金属工业株式会社 | Method for producing platinum material reinforced with dispersed oxide |
| JP2008106349A (en) * | 2006-09-28 | 2008-05-08 | Kojima Kagaku Yakuhin Kk | Method for producing platinum powder |
| CN102296183A (en) * | 2011-08-19 | 2011-12-28 | 天津市化学试剂研究所 | Method for preparing high-purity platinum |
| CN103146942A (en) * | 2013-03-29 | 2013-06-12 | 吉林大学 | Nano-zironia dispersion strengthening diamond composite material and preparation method thereof |
| CN104328301A (en) * | 2014-07-18 | 2015-02-04 | 河南科技大学 | Preparation method of particular-reinforced molybdenum-based composite material |
| CN104550931A (en) * | 2014-12-25 | 2015-04-29 | 铜陵市经纬流体科技有限公司 | Scattering particle reinforced iron-based powder metallurgical valve and preparation method thereof |
| CN106191508A (en) * | 2016-08-31 | 2016-12-07 | 无锡英特派金属制品有限公司 | A kind of ZrO2 dispersion intensifying platinum or the preparation method of platinum rhodium |
| CN113337786A (en) * | 2021-05-31 | 2021-09-03 | 华中科技大学 | Nano zirconium oxide/amorphous alloy composite material and preparation method thereof |
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