CN114406274A - Method for preparing nano reinforced phase dispersed reinforced platinum - Google Patents
Method for preparing nano reinforced phase dispersed reinforced platinum Download PDFInfo
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- CN114406274A CN114406274A CN202111680358.XA CN202111680358A CN114406274A CN 114406274 A CN114406274 A CN 114406274A CN 202111680358 A CN202111680358 A CN 202111680358A CN 114406274 A CN114406274 A CN 114406274A
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/14—Making metallic powder or suspensions thereof using physical processes using electric discharge
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- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/17—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by forging
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- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/18—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by using pressure rollers
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/001—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C5/00—Alloys based on noble metals
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- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/17—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by forging
- B22F2003/175—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by forging by hot forging, below sintering temperature
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The invention discloses a method for preparing nano reinforced phase dispersed reinforced platinum, which comprises the following steps: preparing sol; step two: preparing platinum powder; step three: resonance coating; step four: pressing and hot forging; step five: rolling and forming; the invention provides a manufacturing method of nano reinforced phase dispersed reinforced platinum, which is characterized in that nano-scale reinforced phase particles are prepared by adopting a sol-gel method, the nano reinforced phase dispersed reinforced platinum is obtained after the nano reinforced phase dispersed reinforced platinum is coated with pure platinum powder in a resonance manner, then the defects of the material are reduced by an optimized pressing hot forging and rolling technology, a stable texture structure is obtained, nano particle clusters are uniformly distributed in crystal grains and on crystal boundary, dislocation movement and crystal grain growth can be effectively blocked according to an Orowan mechanism and a Hall-Petch mechanism, the room temperature and high temperature strength of the material are obviously improved, and proper toughness is kept.
Description
Technical Field
The invention belongs to the technical field of manufacturing of nano reinforced phase dispersed reinforced platinum, and particularly relates to a manufacturing method of nano reinforced phase dispersed reinforced platinum.
Background
The reduction of ore storage resources is gradually promoted, the price of noble metal rhodium is greatly increased in recent years, so that the noble metal platinum rhodium equipment for the glass industry is developed towards the direction of low rhodium and no rhodium, and higher requirements on the high-temperature strength and toughness of the existing dispersion-strengthened platinum material are provided.
The strengthening means adopted in the industry at present mainly introduces new strengthening elements including Sc and Re. However, the above-mentioned process technology still has the following disadvantages and shortcomings: (1) the use of a large amount of rare earth elements not only increases the manufacturing cost of materials, but also brings about the problems of glass coloring and wettability change; (2) the strengthening mechanism is still the traditional alloy precipitation strengthening, but the method has limited improvement on the strength of the material and often reduces the plasticity to improve the strength; (3) the burning loss during smelting makes the rare earth content difficult to control.
Disclosure of Invention
The present invention aims at providing a method for preparing nano reinforced phase dispersed reinforced platinum to solve the problems in the background art.
In order to achieve the purpose, the invention provides the following technical scheme: a manufacturing method of nano reinforced phase dispersed reinforced platinum comprises the following steps: sol preparation: zirconium acetate and yttrium acetate are mixed according to the molar ratio of zirconium to yttrium metal ions of (5-10): 1, adding the mixture into deionized water with the same volume, heating and stirring the mixture in a water bath at the temperature of 60-70 ℃, then dropwise adding an ammonia water solution of ethylenediamine tetraacetic acid until the pH value reaches 5.0-5.5, continuously heating and stirring the mixture for 1.0-2.0 h, dropwise adding a proper amount of acetic acid, continuously heating and stirring the mixture for 10min, and standing the mixture for 6.0-10.0 h to obtain a viscous colloid;
step two: preparing platinum powder: smelting a pure platinum ingot in a high-frequency induction furnace, casting the pure platinum ingot into a cylindrical strip with the diameter of phi 3.0-phi 6.0mm, cutting the cylindrical strip into small particles with the thickness of 3.0mm, and preparing pure platinum powder by adopting an electric spark plasma discharge method;
step three: resonance coating: filling the sol in the step one and the platinum powder in the step two into a specially-made glass tank according to the weight ratio of (1-30) to 1000, and then carrying out resonance treatment on the specially-made glass tank by using a resonance coating machine, wherein the resonance frequency is set to be 50-100 Hz, and the resonance time is set to be 1-10 min;
step four: pressing and hot forging: placing the mixed powder obtained in the third step in an oven for 1-2 hours at the temperature of 300-400 ℃, drying, then placing the dried mixed powder in a mold, pressing the dried mixed powder into a compact alloy ingot at room temperature and the pressure of 100-300 MPa, annealing the obtained alloy ingot for 20-50 minutes at the temperature of 1200-1400 ℃, and then forging the alloy ingot for 15-20 times by using a 250kg air hammer to obtain a nano reinforced phase dispersed reinforced platinum alloy ingot;
step five: rolling and forming: and (4) annealing the alloy ingot obtained in the fourth step for 20-60 minutes at 1100-1300 ℃ when the alloy ingot is rolled to be 1.5-2 times of the required thickness, and then rolling the alloy ingot on a rolling mill to obtain a finished product with the required thickness.
Preferably, the ammonia water solution of ethylenediaminetetraacetic acid in the step one contains a proper amount of organic dispersant, and the organic dispersant is 10-50% by volume of polyethylene glycol-2000.
Preferably, the particle size of the powder in the second step is 5-20 μm finally.
Preferably, the total thickness forging deformation of the alloy ingot in the fifth step is 20-50%.
Preferably, the air hammer in the fourth step is forged for 15-20 times, which can be divided into two steps of initial forging and final forging, wherein the initial forging temperature is 1300-1400 ℃, the initial forging temperature is 10-15 times, the final forging temperature is 1200-1300 ℃, and the final forging temperature is 5-10 times.
Compared with the prior art, the invention has the beneficial effects that: the invention provides a manufacturing method of nano reinforced phase dispersed reinforced platinum, which is characterized in that nano-scale reinforced phase particles are prepared by adopting a sol-gel method, the nano reinforced phase dispersed reinforced platinum is obtained after the nano reinforced phase dispersed reinforced platinum is coated with pure platinum powder in a resonance manner, then the defects of the material are reduced by an optimized pressing hot forging and rolling technology, a stable texture structure is obtained, nano particle clusters are uniformly distributed in crystal grains and on crystal boundary, dislocation movement and crystal grain growth can be effectively blocked according to a 0rowan mechanism and a Hall-Petch mechanism, the room temperature and high temperature strength of the material are obviously improved, and proper toughness is retained.
Drawings
FIG. 1 is a schematic diagram of the results of a nano-particle size test of a sol according to the present invention;
FIG. 2 is a structural diagram of the structure of the nano-reinforcing phase dispersed reinforced platinum grain according to the present invention;
FIG. 3 is an enlarged view of the microstructure of the nano-reinforcing phase dispersed reinforced platinum grain according to the present invention;
FIG. 4 is a structural diagram of a grain boundary of nano reinforcing phase diffusion strengthened platinum according to the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
(1) Sol preparation: adding 100ml of zirconium acetate (15%) and yttrium acetate (15%) into deionized water with the same volume according to the molar ratio of zirconium to yttrium metal ions of 9: 1, placing the deionized water in a 65 ℃ water bath for heating and stirring, then dropwise adding an ammonia water solution of ethylenediamine tetraacetic acid (containing a proper amount of organic dispersant) until the pH value reaches 5.1, continuously heating and stirring for 1.5h, dropwise adding 4ml of acetic acid, continuously heating and stirring for 10min, and standing for 7h to obtain a viscous colloid;
(2) preparing platinum powder: smelting 4kg of pure platinum ingot in a high-frequency induction furnace, casting the pure platinum ingot into a cylindrical strip with the diameter of 4.0mm, cutting the pure platinum ingot into small particles with the thickness of 3.0mm, and preparing pure platinum powder by adopting an electric spark plasma discharge method;
(3) resonance coating: putting the sol in the step (1) and the platinum powder in the step (2) into a specially-made glass tank according to the weight ratio of 15: 1000, and then carrying out resonance treatment on the glass tank by using a resonance coating machine, wherein the resonance frequency is set to be 60Hz, and the resonance time is set to be 5 min;
(4) pressing and hot forging: placing the mixed powder obtained in the step (3) in an oven for 1.5h at the temperature of 400 ℃, drying, placing the dried mixed powder in a die, pressing the dried mixed powder into a compact alloy ingot at room temperature and the pressure of 280MPa, annealing the obtained alloy ingot at 1300 ℃ for 30 minutes, then forging the compact alloy ingot for 15 times by using a 250kg air hammer, wherein the initial forging temperature is 1400 ℃, the initial forging temperature is 10 times, the final forging temperature is 1200 ℃, and the final forging time is 5 times to obtain a nano reinforced phase diffusion reinforced platinum alloy ingot;
(5) rolling and forming: and (4) annealing the alloy ingot obtained in the step (4) at 1300 ℃ for 30 minutes when the alloy ingot is rolled to be 2 times of the required thickness, and then rolling the alloy ingot on a rolling mill to obtain a finished product with the required thickness.
Example 2
The preparation method is basically the same as that in example 1, except that: the sol reactants are in different proportions, and 100ml of zirconium acetate (15%) and yttrium acetate (15%) are added into deionized water with the same volume according to the molar ratio of 5: 1 of zirconium to yttrium metal ions.
Example 3
The preparation method is basically the same as that in example 1, except that: the proportion of the sol and the platinum powder is different, and the sol and the platinum powder are filled according to the weight ratio of 25: 1000.
The specific mechanical properties of the dispersion strengthened platinum of the nano reinforcing phase with different volume fractions in each example are shown in the following table:
table 1 shows the performance test results of nano-reinforced diffusion strengthened platinum
Tests prove that compared with the traditional dispersion strengthened platinum, the nano reinforced phase dispersion strengthened platinum of the invention has the following outstanding advantages: the material has uniform tissue and good consistency, the nano-particle clusters are uniformly distributed in crystal grains and on crystal boundary, dislocation motion and crystal grain growth can be effectively hindered according to an Orowan mechanism and a Hall-Petch mechanism, the room temperature and high temperature strength of the material are obviously improved, and proper toughness is kept.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (5)
1. A method for preparing nano reinforced phase dispersed reinforced platinum is characterized in that: the method comprises the following steps: sol preparation: adding zirconium acetate and yttrium acetate into deionized water with the same volume according to the molar ratio of zirconium to yttrium metal ions of (5-10) to 1, heating in a water bath at 60-70 ℃ and stirring, then dropwise adding an ammonia water solution of ethylenediamine tetraacetic acid until the pH value reaches 5.0-5.5, continuously heating and stirring for 1.0-2.0 h, dropwise adding a proper amount of acetic acid, continuously heating and stirring for 10min, and standing for 6.0-10.0 h to obtain a viscous colloid;
step two: preparing platinum powder: smelting a pure platinum ingot in a high-frequency induction furnace, casting the pure platinum ingot into a cylindrical strip with the diameter of phi 3.0-phi 6.0mm, cutting the cylindrical strip into small particles with the thickness of 3.0mm, and preparing pure platinum powder by adopting an electric spark plasma discharge method;
step three: resonance coating: filling the sol in the step one and the platinum powder in the step two into a specially-made glass tank according to the weight ratio of (1-30) to 1000, and then carrying out resonance treatment on the specially-made glass tank by using a resonance coating machine, wherein the resonance frequency is set to be 50-100 Hz, and the resonance time is set to be 1-10 min;
step four: pressing and hot forging: placing the mixed powder obtained in the third step in an oven for 1-2 hours at the temperature of 300-400 ℃, drying, then placing the dried mixed powder in a mold, pressing the dried mixed powder into a compact alloy ingot at room temperature and the pressure of 100-300 MPa, annealing the obtained alloy ingot for 20-50 minutes at the temperature of 1200-1400 ℃, and then forging the alloy ingot for 15-20 times by using a 250kg air hammer to obtain a nano reinforced phase dispersed reinforced platinum alloy ingot;
step five: rolling and forming: and (4) annealing the alloy ingot obtained in the fourth step for 20-60 minutes at 1100-1300 ℃ when the alloy ingot is rolled to be 1.5-2 times of the required thickness, and then rolling the alloy ingot on a rolling mill to obtain a finished product with the required thickness.
2. The method for preparing nano reinforced phase dispersion strengthened platinum according to claim 1, wherein the method comprises the following steps: the ammonia water solution of the ethylenediamine tetraacetic acid in the step one contains a proper amount of organic dispersing agent, and the organic dispersing agent is 10-50% by volume of polyethylene glycol-2000.
3. The method for preparing nano reinforced phase dispersion strengthened platinum according to claim 1, wherein the method comprises the following steps: and in the second step, the particle size of the powder is 5-20 μm finally.
4. The method for preparing nano reinforced phase dispersion strengthened platinum according to claim 1, wherein the method comprises the following steps: and fifthly, the total thickness forging deformation of the alloy ingot is 20-50%.
5. The method for preparing nano reinforced phase dispersion strengthened platinum according to claim 1, wherein the method comprises the following steps: and the air hammer in the fourth step is forged for 15-20 times, which can be divided into two steps of initial forging and final forging, wherein the initial forging temperature is 1300-1400 ℃, the initial forging temperature is 10-15 times, the final forging temperature is 1200-1300 ℃, and the final forging temperature is 5-10 times.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020112563A1 (en) * | 2000-06-28 | 2002-08-22 | Toru Shoji | Platinum material reinforced by oxide dispersion and process for producing the same |
| 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 |
| CN102876911A (en) * | 2012-10-12 | 2013-01-16 | 无锡英特派金属制品有限公司 | Method for manufacturing dispersion-strengthened platinum-rhodium alloy sheet |
| CN105039768A (en) * | 2015-08-26 | 2015-11-11 | 付亚波 | Preparation method for preparing high-strength high-conductivity nano dispersion strengthened copper through sol-gel method |
| 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 |
| CN109732090A (en) * | 2019-01-22 | 2019-05-10 | 雷洪贵 | A kind of preparation method of the high-strength porous self-lubricating material of anti-scorching type |
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2021
- 2021-12-30 CN CN202111680358.XA patent/CN114406274B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020112563A1 (en) * | 2000-06-28 | 2002-08-22 | Toru Shoji | Platinum material reinforced by oxide dispersion and process for producing the same |
| 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 |
| CN1386137A (en) * | 2000-06-28 | 2002-12-18 | 田中贵金属工业株式会社 | Platinum material reinforced by oxide dispersion and process for producing the same |
| CN102876911A (en) * | 2012-10-12 | 2013-01-16 | 无锡英特派金属制品有限公司 | Method for manufacturing dispersion-strengthened platinum-rhodium alloy sheet |
| CN105039768A (en) * | 2015-08-26 | 2015-11-11 | 付亚波 | Preparation method for preparing high-strength high-conductivity nano dispersion strengthened copper through sol-gel method |
| 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 |
| CN109732090A (en) * | 2019-01-22 | 2019-05-10 | 雷洪贵 | A kind of preparation method of the high-strength porous self-lubricating material of anti-scorching type |
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