CN108149055B - A kind of dispersion strengthening type material and its preparation method and application for platinum rhodium base vessel - Google Patents
A kind of dispersion strengthening type material and its preparation method and application for platinum rhodium base vessel Download PDFInfo
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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
- C22C5/04—Alloys based on a platinum group metal
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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
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- B22F1/145—Chemical treatment, e.g. passivation or decarburisation
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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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- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
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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
- C22C32/0015—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 with only single oxides as main non-metallic constituents
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
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Abstract
The present invention provides a kind of dispersion strengthening type material for platinum rhodium base vessel, including substrate, and the hardening constituent of Dispersed precipitate in the substrate, the substrate is platinum-rhodium alloy, the hardening constituent element is zirconium, scandium, any one or a few in cerium, and the content of rhodium is > 0~≤20wt% in each component；Zirconium content is > 0~≤0.4wt%；Scandium content is 0~0.4wt%；Cerium content is 0~0.4wt%；Platinum is surplus；Zirconium+scandium+cerium < 0.6wt%, hardening constituent element Dispersed precipitate in the form of its oxide in the substrate, constitute dispersion strengthening type material.There is good antiscour, anticorrosive and high-temperature creep resistance provided by the present invention for the dispersion strengthening type material of platinum rhodium base vessel, the vessel long service life prepared using this material, can be effectively reduced the production cost of such as optical glass and glass fibre industrial circle.
Description
Technical field
The present invention relates to precious metal material fields, and in particular to a kind of dispersion strengthening type material for platinum rhodium base vessel and
Preparation method and application.
Background technique
In the production process of the industrial circles such as optical glass, glass fibre, need to be carried out in platinum-rhodium alloy vessel melting,
Molding etc..Since operating condition is severe, it is desirable that vessel material has stronger resistance to deformation, antiscour, anti-corruption under the high temperature conditions
Corrosion energy reduces the loss of platinum-rhodium alloy to guarantee the service life of alloy vessel, realizes the purpose for reducing production cost.
However, the vessel of platinum-rhodium alloy material production commonly used at present, resistance to deformation under the high temperature conditions, anti-impact
Brush, corrosion resistance are unable to satisfy expected requirement, so that using the vessel of these materials preparation in the easy deformation of creep of hot conditions,
So that such materials'use service life is short, cause the production cost of optical glass and glass fibre high.
Summary of the invention
The object of the present invention is to provide a kind of dispersion strengthening type material for platinum rhodium base vessel, which has good
Antiscour, anticorrosive and high-temperature creep resistance, the vessel long service life prepared using this material, can be effectively reduced such as light
Learn the production cost of the industrial circles such as glass and glass fibre.The present invention also provides this disperse for platinum rhodium base vessel is strong
Change the preparation method of profile material.
To achieve the above object, the present invention provides following technical scheme, a kind of dispersion strengthening type for platinum rhodium base vessel
Material, including the hardening constituent of substrate and Dispersed precipitate in the substrate, the substrate are platinum-rhodium alloy, the hardening constituent element
For any one or a few in zirconium, scandium, cerium, the content of metallic element in each component are as follows:
Rhodium > 0~≤20wt%；
Zirconium > 0~≤0.4wt%；
0~0.4wt% of scandium；
0~0.4wt% of cerium；
Platinum surplus；
Wherein, zirconium+scandium+cerium < 0.6wt%,
Hardening constituent element Dispersed precipitate in the form of its oxide in the substrate, constitutes dispersion strengthening type material.
Further, in each component metallic element content are as follows:
3~20wt% of rhodium；
0.2~0.4wt% of zirconium；
0~0.05wt% of scandium；
Platinum surplus.
The oxide of the zirconium, the oxide of scandium, cerium the metal oxygenation efficiency of oxide be all larger than 99.5%.
The oxide of the zirconium, the oxide of scandium, cerium the partial size of oxide be respectively less than 1 μm.
The preparation method of any of the above-described dispersion strengthening type material for platinum rhodium base vessel, has follow steps:
1) raw material is configured
By the weight percent ingredient of each metallic element；
2) vacuum intermediate-frequency melting
In protective atmosphere, the raw material prepared is placed in melting in vacuum intermediate-frequency smelting furnace, smelting temperature 1800-1950
DEG C, vacuum degree 10-2-10-3Pa after raw material is completely melt, keeps the temperature 2-5min after mixing, ingot casting of quickly casting to obtain；
3) hot-working
The ingot casting that step 2 is obtained is placed in heat-treatment furnace, homogenization heat treatment 30-60min, heat at 1200-1400 DEG C
Forging, initial forging temperature are 1200-1400 DEG C, and final forging temperature is 900-1300 DEG C, and heat treatment is then homogenized at 900-1300 DEG C
0.5-2h obtains alloy bar；
4) drawing
The resulting alloy bar of step 3) is drawn to the alloy wire of 0.5~5.0mm, deflection is 5- per pass
15%；
5) alloy powder is prepared
Under protective atmosphere, the alloy wire that step 4) is obtained is melted, and molten state alloy is spraying, condensation obtains ball
The alloy powder of shape；
6) it is sieved
The alloy powder sieving that step 5) is obtained, obtains partial size less than 40 μm in the globular powder of size distribution；
7) Powder Oxidation
By globular powder that step 6) obtains temperature is 700-1200 DEG C, oxygen pressure is 2~6 × 105It is aoxidized under the conditions of Pa
2-10h guarantees that the oxygenation efficiency of hardening constituent metallic element is all larger than 99.5%, obtains uniform mixed-powder；
8) mixed-powder briquetting
First pressing billet is made in the pushing of 10-300MPa pressure in the mixed-powder that step 7) obtains；
9) it is sintered
The first pressing billet that step 8) obtains is sintered 2-10h under the conditions of 900-1400 DEG C, obtains formed body；
10) it is hot-forged
The formed body that step 9) obtains is hot-forged under the conditions of 900-1400 DEG C and obtains slab；
11) cold rolling
The slab that step 10) obtains is obtained into the dispersion-strengtherning profile for being used for platinum rhodium base vessel of predetermined size through cold rolling
Material.
Mixing described in step 2 is mixed using electromagnetic agitation.
Melting described in step 5) is melted alloy wire using arc pistol；It is described that electric arc is directed at using high-pressure nozzle by spraying
The muzzle of spray gun sprays high pressure gas for the alloy atomisation of melting；The alloy for being condensed into mist is sprayed to from water meter
Face is condensed.
Any of the above-described dispersion strengthening type material for platinum rhodium base vessel is being used to prepare optical glass material and glass fibers
Purposes in dimension production vessel.
Gas is protected to use nitrogen or argon gas in the present invention.
Provided by the present invention for the dispersion strengthening type material of platinum rhodium base vessel, by adding micro Zirconium oxide, scandium
Oxide, cerium oxide one or more as hardening constituent, Dispersed precipitate in platinum-rhodium alloy, obtain dispersion strengthening type conjunction
Gold has good antiscour, anticorrosive and high-temperature creep resistance, is less than 0.6wt% by control zirconium+scandium+cerium content,
It avoids excessive zirconium or/and cerium or/and scandium from becoming impurity and forms harmful phase in the substrate, guarantee alloy property.Prepare this use
When the dispersion strengthening type material of platinum rhodium base vessel, silk material is made through vacuum intermediate-frequency smelting process, contour machining procedure in raw material, really
The ingredient and microstructure homogenization of alloy are protected；Silk material obtains the spherical alloy powder of high uniformity, ball by electric arc atomization powder
Shape alloy powder is through high temperature oxidation process, it is ensured that the trace zirconium or/and scandium or/and cerium in spherical alloy powder are by abundant oxygen
Change, obtains dispersion strengthening phase；The powder metallurgical techniques such as compacting, sintering, hot forging, cold rolling are eventually passed through, obtaining has metallurgy
The dispersion strengthening type material of quality.The oxide of resulting material compactness height, zirconium or/and scandium or/and cerium is dispersed in platinum
In rhodium material, the mechanical property of material at high temperature especially high-temperature creep resistance is effectively improved, so that is be prepared is used for
The dispersion strengthening type material of platinum rhodium base vessel has excellent high-temperature and durable and high-temperature creep resistance, while also having good
Antiscour and corrosion resistance.Using machined manufactured use of vessel under the conditions of high temperature hostile of this alloy material
Service life is long, reduces noble metal loss, so that realizing reduces such as production cost of optical glass and glass fibre industrial circle.
The purity of metal used in the present invention is >=99.99%.
Specific embodiment
Below with reference to embodiment, the present invention is further illustrated, but does not therefore limit the present invention to the reality
It applies among a range.
Embodiment 1
Platinum: 2394g(weight percent 79.8%), rhodium: 600g(weight percent 20%), zirconium: 6g(weight percent
0.20%).
Embodiment 2
Platinum: 2692.5g(weight percent 89.75%), rhodium: 300g(weight percent 10%), zirconium: 6g(weight percent
0.20%), scandium: 1.5g(weight percent 0.05%).
The dispersion strengthening type material for platinum rhodium base vessel is prepared by the following method:
(1) raw material is configured
Each proportioning materials described in Example 1-2；
(2) vacuum intermediate-frequency melting
The raw material prepared is put into vacuum drying oven and carries out melting, smelting temperature is 1850 ~ 1950 DEG C, vacuum degree 10-2-
10-3Pa, while it being filled with argon gas protection, after raw material is completely melt, magnetic stirs evenly and keeps the temperature 2-5min, and the liquid metal of acquisition is fast
Speed, which is poured to cast from, obtains ingot casting in water cooled copper mould；
(3) hot-working
Obtained ingot casting even heat treatment 60min at 1300 DEG C, hot forging is at rodlike, the homogenization heat treatment at 1200 DEG C
30min, stress relief annealing obtain alloy bar；
(4) drawing
Alloy bar is drawn into the alloy wire of 1.5mm, deflection is 5% ~ 15% per pass；
(5) alloy powder is prepared
In argon atmosphere, alloy wire is sent into arc pistol, is melted alloy wire with electric arc, by high pressure spray
The muzzle of head alignment arc pistol, sprays high pressure gas, the alloy of melting is sprayed to from water surface, collection obtains spherical conjunction
Bronze end；
(6) it is sieved
The spherical alloy powder sieving that step 5) is collected, obtain size distribution preferably, partial size is less than 40 μm
In the globular powder of size distribution；
(7) Powder Oxidation
By the globular powder of step 6) sieving temperature is 1000 DEG C, oxygen pressure is 5*105High-temperature oxydation under the conditions of Pa, oxidation
Time is 5h；
(8) powder compact
Powder through high temperature oxidation process pours into φ 100 × 150mm shaping mould, is pressed under the pressure of 100MPa
System, obtains first pressing billet；
(9) it is sintered
First pressing billet is sintered at a temperature of 1400 DEG C, sintering time 2h obtains formed body；
(10) it is hot-forged
Formed body is hot-forged at a temperature of 1300 DEG C, obtains required slab；
(11) cold rolling
By slab obtained as above, through cold rolling, (cold rolling pass deflection≤15%, total deformation≤70%, when cold rolling, are as needed
Made annealing treatment) obtain the dispersion strengthening type material for platinum rhodium base vessel of required thickness size；
(12) processing and forming
The obtained dispersion strengthening type material for being used for platinum rhodium base vessel is machined, required dispersion-strengtherning is obtained
Noble metal vessel.
Performance test:
Metalware made of the material of embodiment 1 or 2 does stress-rupture tester, compared to using platinum-rhodium alloy material
The vessel of production, duration improve 2 times or more.
Claims (8)
1. a kind of dispersion strengthening type material for platinum rhodium base vessel, which is characterized in that including substrate and Dispersed precipitate in base
Hardening constituent in material, the substrate are platinum-rhodium alloy, and the hardening constituent element is zirconium, scandium, any one or a few in cerium, respectively
The content of metallic element in component are as follows: rhodium > 0~≤20wt%；Zirconium > 0~≤0.4wt%；0~0.4wt% of scandium；Cerium 0~
0.4wt%；Platinum surplus；Wherein, zirconium+scandium+cerium < 0.6wt%, hardening constituent element Dispersed precipitate in the form of its oxide exist
In substrate, dispersion strengthening type material is constituted；The material is prepared using following methods step:
1) raw material is configured
By the weight percent ingredient of above-mentioned each metallic element；
2) vacuum intermediate-frequency melting
In protective atmosphere, the raw material prepared is placed in melting in vacuum intermediate-frequency smelting furnace, smelting temperature is 1850-1950 DEG C,
Vacuum degree is 10-2-10-3Pa after raw material is completely melt, keeps the temperature 2-5min after mixing, ingot casting of quickly casting to obtain；
3) hot-working
The ingot casting that step 2 is obtained is placed in heat-treatment furnace, homogenization heat treatment 30-60min at 1200-1400 DEG C, hot forging,
Initial forging temperature is 1200-1400 DEG C, and final forging temperature is 900-1300 DEG C, then the homogenization heat treatment 0.5- at 900-1300 DEG C
2h obtains alloy bar；
4) drawing
The resulting alloy bar of step 3) is drawn to the alloy wire of 0.5~5.0mm, deflection is 5-15% per pass；
5) alloy powder is prepared
Under protective atmosphere, the alloy wire that step 4) is obtained is melted, and molten state alloy is spraying, condensation obtains spherical
Alloy powder；
6) it is sieved
The alloy powder sieving that step 5) is obtained, obtains partial size less than 40 μm in the globular powder of size distribution；
7) Powder Oxidation
By globular powder that step 6) obtains temperature is 700-1200 DEG C, oxygen pressure is 2~6 × 1052-10h is aoxidized under the conditions of Pa,
Guarantee that the oxygenation efficiency of hardening constituent metallic element is all larger than 99.5%, obtains uniform mixed-powder；
8) mixed-powder briquetting
First pressing billet is made in the pushing of 10-300MPa pressure in the mixed-powder that step 7) obtains；
9) it is sintered
The first pressing billet that step 8) obtains is sintered 2-10h under the conditions of 900-1400 DEG C, obtains formed body；
10) it is hot-forged
The formed body that step 9) obtains is hot-forged under the conditions of 900-1400 DEG C and obtains slab；
11) cold rolling
The slab that step 10) obtains is obtained into the dispersion strengthening type material for being used for platinum rhodium base vessel of predetermined size through cold rolling.
2. being used for the dispersion strengthening type material of platinum rhodium base vessel according to claim 1, it is characterised in that: metal in each component
The content of element are as follows:
3~20wt% of rhodium；
0.2~0.4wt% of zirconium；
0~0.05wt% of scandium；
Platinum surplus.
3. the dispersion strengthening type material according to claim 1 or claim 2 for platinum rhodium base vessel, it is characterised in that: the zirconium
Oxide, the oxide of scandium, cerium the metal oxygenation efficiency of oxide be all larger than 99.5%.
4. the dispersion strengthening type material according to claim 1 or claim 2 for platinum rhodium base vessel, it is characterised in that: the zirconium
Oxide, the oxide of scandium, cerium the partial size of oxide be respectively less than 1 μm.
5. a kind of preparation method of the dispersion strengthening type material as claimed in claim 1 or 2 for platinum rhodium base vessel, feature exist
In having follow steps:
1) raw material is configured
By the weight percent ingredient of each metallic element as claimed in claim 1 or 2；
2) vacuum intermediate-frequency melting
In protective atmosphere, the raw material prepared is placed in melting in vacuum intermediate-frequency smelting furnace, smelting temperature is 1850-1950 DEG C,
Vacuum degree is 10-2-10-3Pa after raw material is completely melt, keeps the temperature 2-5min after mixing, ingot casting of quickly casting to obtain；
3) hot-working
The ingot casting that step 2 is obtained is placed in heat-treatment furnace, homogenization heat treatment 30-60min at 1200-1400 DEG C, hot forging,
Initial forging temperature is 1200-1400 DEG C, and final forging temperature is 900-1300 DEG C, then the homogenization heat treatment 0.5- at 900-1300 DEG C
2h obtains alloy bar；
4) drawing
The resulting alloy bar of step 3) is drawn to the alloy wire of 0.5~5.0mm, deflection is 5-15% per pass；
5) alloy powder is prepared
Under protective atmosphere, the alloy wire that step 4) is obtained is melted, and molten state alloy is spraying, condensation obtains spherical
Alloy powder；
6) it is sieved
The alloy powder sieving that step 5) is obtained, obtains partial size less than 40 μm in the globular powder of size distribution；
7) Powder Oxidation
By globular powder that step 6) obtains temperature is 700-1200 DEG C, oxygen pressure is 2~6 × 1052-10h is aoxidized under the conditions of Pa,
Guarantee that the oxygenation efficiency of hardening constituent metallic element is all larger than 99.5%, obtains uniform mixed-powder；
8) mixed-powder briquetting
First pressing billet is made in the pushing of 10-300MPa pressure in the mixed-powder that step 7) obtains；
9) it is sintered
The first pressing billet that step 8) obtains is sintered 2-10h under the conditions of 900-1400 DEG C, obtains formed body；
10) it is hot-forged
The formed body that step 9) obtains is hot-forged under the conditions of 900-1400 DEG C and obtains slab；
11) cold rolling
The slab that step 10) obtains is obtained into the dispersion strengthening type material for being used for platinum rhodium base vessel of predetermined size through cold rolling.
6. preparation method according to claim 5, it is characterised in that: mixing described in step 2 is mixed using electromagnetic agitation.
7. preparation method according to claim 5, it is characterised in that: melting described in step 5) uses arc pistol by alloy
Silk material melting；The muzzle for being directed at arc pistol using high-pressure nozzle by spraying is sprayed high pressure gas and is sprayed into the alloy of melting
It is misty；The alloy for being condensed into mist is sprayed to be condensed from water surface.
8. being used to prepare optical glass using any dispersion strengthening type material for platinum rhodium base vessel of claim 1-4
Purposes in material and glass fibre production vessel.
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| EP3971311A1 (en) * | 2020-09-17 | 2022-03-23 | Heraeus Deutschland GmbH & Co. KG | Improved dispersion-hardened precious metal alloy |
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| CN110387483B (en) * | 2019-07-25 | 2021-02-09 | 无锡英特派金属制品有限公司 | Manufacturing method of Pt-Au alloy |
| CN111020273B (en) * | 2019-11-22 | 2021-11-02 | 重庆材料研究院有限公司 | High-temperature deformation resistant high-strength platinum group metal material and preparation method thereof |
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| CN116116928A (en) * | 2023-02-09 | 2023-05-16 | 重庆材料研究院有限公司 | Platinum-based alloy protection sleeve and preparation method thereof |
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| CN117733164A (en) * | 2023-11-16 | 2024-03-22 | 重庆材料研究院有限公司 | Method for preparing high-temperature strength dispersion material by adopting noble metal nano powder |
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| DE102006015167B3 (en) * | 2006-03-30 | 2007-07-19 | W.C. Heraeus Gmbh | Production of a wire or strip used e.g. as an electrode in spark plugs comprises producing an intermetallic compound, grinding, mixing with metal powder, feeding the mixture into a tube and deforming the filled tube |
| CN100500898C (en) * | 2006-09-08 | 2009-06-17 | 国内贸易部物资再生利用研究所 | Reinforced platinum material and method of manufacture and use thereof |
| CN101550500A (en) * | 2009-03-18 | 2009-10-07 | 重庆国际复合材料有限公司 | A zircite dispersion strengthening platinum-rhodium alloy with low rhodium content |
| CN101561323B (en) * | 2009-05-18 | 2011-04-20 | 无锡英特派金属制品有限公司 | Dispersion strengthening platinum/rhodium30-platinum/rhodium6 thermocouple wires and production 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 |
-
2017
- 2017-11-16 CN CN201711134031.6A patent/CN108149055B/en active Active
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP3971311A1 (en) * | 2020-09-17 | 2022-03-23 | Heraeus Deutschland GmbH & Co. KG | Improved dispersion-hardened precious metal alloy |
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| CN108149055A (en) | 2018-06-12 |
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