CN104164584A - Ultrahigh-resistance-temperature-coefficient palladium-iron alloy and preparation method thereof - Google Patents
Ultrahigh-resistance-temperature-coefficient palladium-iron alloy and preparation method thereof Download PDFInfo
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- CN104164584A CN104164584A CN201410382770.7A CN201410382770A CN104164584A CN 104164584 A CN104164584 A CN 104164584A CN 201410382770 A CN201410382770 A CN 201410382770A CN 104164584 A CN104164584 A CN 104164584A
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Abstract
The invention discloses an ultrahigh-resistance-temperature-coefficient palladium-iron alloy and a preparation method thereof. The alloy comprises the following components in percentage by mass: 72-75% of Pd and 25-28% of Fe. The preparation method comprises the following steps: carrying out quick setting (alloy solution injection quick-cooling process) to obtain a Phi0.2mm palladium-iron alloy wire, and carrying out normal-temperature plastic deformation to prepare the Phi0.015-0.03mm ultrathin wire. The palladium-iron alloy finished product is subjected to heat treatment (including high-temperature solid solution continuous annealing and ordered transition heat treatment) to obtain the palladium-iron alloy with ultrahigh resistance temperature coefficient (8720 ppm/DEG C); and the palladium-iron alloy with ultrahigh resistance temperature coefficient is used instead of the pure Pt wire (3927 ppm/DEG C) to prepare the contact-combustion gas sensor coil, thereby enhancing the sensitivity of the sensor and lowering the manufacturing cost of the sensor.
Description
Technical field
The invention belongs to metal material field, relate to the preparation method of the palladium iron alloy with ultra-high resistance temperature factor, the ultrafine wire of preparing can replace pure Pt silk to prepare catalytic combustion type gas sensor coil.
Background technology
In precious metal material, the maximum (α of the temperature coefficient of resistance of platinum
0～100 ℃=3927ppm/ ℃), physical and chemical performance is the most stable, platinum filament first-selection is as the coil method of gas sensor, but RTD rate is little, intensity is low, for improving the sensitivity of sensor, conventionally can only use the platinum filament that wire diameter is very little, tiny and soft platinum filament brings very large difficulty to the making of element, and gas sensor is scrapped because platinum filament ruptures.Conventionally, after precious metal element solid solution alloying, resistivity rising, temperature coefficient of resistance decline, yet Pd3Fe phase alloy is contrary, and it is closely related that this and palladium iron alloy form ordered phase Pd3Fe structure.
The palladium iron alloy of Pd3Fe ordered phase structure has good over-all properties: the temperature coefficient of resistance of superelevation, high resistivity and intensity, can be used as the coil method of catalytic combustion type and hot wire type gas sensor, replace the high-purity platinum filament generally adopting at present, not only reduce sensor cost, and can improve its sensitivity (particularly can be used for detecting the gases such as lower concentration CO).Britain and Japan prepare highly sensitive catalytic combustion type CO sensor with the PdFe alloy ultrafine wire with Pd3Fe ordered phase, but concrete composition and manufacture craft also do not have relevant open report.
Summary of the invention
The object of this invention is to provide a kind of palladium iron alloy ultrafine wire, temperature coefficient of resistance is up to 8720ppm/ ℃, be used for replacing pure Pt silk to prepare catalytic combustion type gas sensor, in the time of the sensitivity that improves sensor, lower the cost of manufacture of sensor, fill up this field domestic blank.
The palladium iron alloy with ultra-high resistance temperature factor that the present invention proposes, its composition quality per-cent is 72～75Pd, 25～28Fe.There is Pd3Fe ordered phase structure (being similar to AuCu3) in the palladium iron alloy of this composition range, has the unique electrical performance of the temperature coefficient of resistance of superelevation.
The palladium iron alloy that the present invention proposes is prepared with the following method: each constituent element of alloy is prepared burden by nominal content, and material purity is greater than 99.99%, adopts the alloy molten solution in flash set technology to inject fast cold process, has prepared the non-crystaline amorphous metal wire rod of Ф 0.2mm.Processing parameter is as follows: temperature of fusion-1350～1480 ℃, nozzle diameter-300 μ m, jet velocity-1.5m/s, cooling fluid-20～28%MgCl
2temperature 213～the 257K of salt solution, cooling fluid, the cooling fluid flow velocity-1.65～2.15m/s in thrust-augmenting nozzle, the diameter-0.15～0.28mm of acquisition non-crystaline amorphous metal wire rod.
Adopt normal temperature drawing viscous deformation, in pass deformation 0.5～1.5%, total deformation 40～60%, process annealing adopt 600～750 ℃ of temperature (soaking time 20～40 minutes), finally prepare the ultra-fine wire that diameter is 0.015～0.03mm.
Palladium iron alloy carries out order transformation after high temperature solid solution continuous annealing again, the temperature coefficient of resistance obtaining directly carries out will improving much of order transformation than palladium iron alloy, so the finished product pack processing of palladium iron alloy contains: (750 ℃～880 ℃ of high temperature solid solution continuous annealing (900～1000 ℃) and order transformation thermal treatments, insulation 12h), alloy obtains the temperature coefficient of resistance (8015～8720ppm/ ℃) of superelevation.
Embodiment
Each constituent element of embodiment 1 alloy is pressed 75.0%Pd, the content batching (mass percent) of 25.0%Fe, material purity is greater than 99.99%, adopt alloy molten solution in flash set technology to inject fast cold process (processing parameter is as follows: the temperature 224K of temperature of fusion-1390 ℃, nozzle diameter-300 μ m, jet velocity-1.5m/s, cooling fluid-23%MgCl2 salt solution, cooling fluid, cooling fluid are at the flow velocity-1.95m/s of thrust-augmenting nozzle), prepared the non-crystaline amorphous metal wire rod of Ф 0.2mm.Adopt normal temperature drawing viscous deformation, in pass deformation 0.8%, total deformation 50%, process annealing adopt 700 ℃ of temperature (soaking time 20～40 minutes), finally prepare the ultra-fine wire that diameter is 0.015mm.Carry out subsequently 950 ℃ of solid solution continuous annealings (20 revs/min of take-up speeds) and 800 ℃ of insulations order transformation thermal treatment of 12 hours, the temperature coefficient of resistance of alloy reaches maximum value, finally measure its temperature coefficient of resistance 8015ppm/ ℃, resistivity 36 μ Ω cm, tensile strength 1150MPa.
Each constituent element of embodiment 2 alloys is pressed 73.0%Pd, the content batching of 27.0%Fe, material purity is greater than 99.99%, adopt alloy molten solution in flash set technology to inject fast cold process (processing parameter is as follows: the temperature 224K of temperature of fusion-1420 ℃, nozzle diameter-300 μ m, jet velocity-1.5m/s, cooling fluid-23%MgCl2 salt solution, cooling fluid, cooling fluid are at the flow velocity-1.95m/s of thrust-augmenting nozzle), prepared the non-crystaline amorphous metal wire rod of Ф 0.2mm.Adopt normal temperature drawing viscous deformation, in pass deformation 0.8%, total deformation 50%, process annealing adopt 700 ℃ of temperature (soaking time 20～40 minutes), finally prepare the ultra-fine wire that diameter is 0.015mm.Carry out subsequently 950 ℃ of solid solution continuous annealings (20 revs/min of take-up speeds) and 830 ℃ of insulations order transformation thermal treatment of 12 hours, the temperature coefficient of resistance of alloy reaches maximum value, finally measure its temperature coefficient of resistance 8450ppm/ ℃, resistivity 32 μ Ω cm, tensile strength 1208MPa.
Each constituent element of embodiment 3 alloys is pressed 72.0%Pd, the content batching of 28.0%Fe, material purity is greater than 99.99%, adopt alloy molten solution in flash set technology to inject fast cold process (processing parameter is as follows: the temperature 224K of temperature of fusion-1450 ℃, nozzle diameter-300 μ m, jet velocity-1.5m/s, cooling fluid-23%MgCl2 salt solution, cooling fluid, cooling fluid are at the flow velocity-1.95m/s of thrust-augmenting nozzle), prepared the non-crystaline amorphous metal wire rod of Ф 0.2mm.Adopt normal temperature drawing viscous deformation, in pass deformation 0.8%, total deformation 50%, process annealing adopt 700 ℃ of temperature (soaking time 20～40 minutes reduces soaking time with silk material diameter and reduces), finally prepare the ultra-fine wire that diameter is 0.015mm.Carry out subsequently 950 ℃ of solid solution continuous annealings (20 revs/min of take-up speeds) and 850 ℃ of insulations order transformation thermal treatment of 12 hours, the temperature coefficient of resistance of alloy reaches maximum value, finally measure its temperature coefficient of resistance 8720ppm/ ℃, resistivity 30 μ Ω cm, tensile strength 1260MPa.
Table 1 is palladium iron alloy and pure Pt silk performance comparison.
Palladium iron alloy and pure Pt silk performance comparison
Table 2 is performance comparison of palladium iron alloy of the present invention and the palladium iron alloy reported.
Claims (5)
1. a palladium iron alloy with ultra-high resistance temperature factor, is characterized in that: alloying constituent mass percent is 72～75Pd and 25～28Fe, and it is AuCu3 structure that the palladium iron alloy of this composition range exists Pd3Fe ordered phase structure.
2. the palladium iron alloy of claim 1 is applied to catalytic combustion type gas sensor coil method.
3. a preparation method with the palladium iron alloy of ultra-high resistance temperature factor, it is characterized in that: adopt the alloy molten solution in flash set technology to inject fast cold process, processing parameter is as follows: temperature of fusion is that 1350～1480 ℃, nozzle diameter are that 300 μ m, jet velocity are that 1.5m/s, cooling fluid are 20～28%MgCl
2the temperature of salt solution, cooling fluid is that 213～257K, the cooling fluid flow velocity in thrust-augmenting nozzle is 1.65～2.15m/s, the diameter that adopts normal temperature drawing viscous deformation to obtain non-crystaline amorphous metal wire rod is 0.15～0.28mm, passes through subsequently high temperature solid solution continuous annealing and order transformation thermal treatment.
4. the preparation method with the palladium iron alloy of ultra-high resistance temperature factor according to claim 3, it is characterized in that: while adopting normal temperature drawing viscous deformation, in pass deformation 0.5～1.5%, total deformation 40～60%, process annealing adopt 600～750 ℃ of temperature, soaking time 20～40 minutes, finally prepares the ultra-fine wire that diameter is 0.015～0.03mm.
5. the preparation method with the palladium iron alloy of ultra-high resistance temperature factor according to claim 3, it is characterized in that: described palladium iron alloy through the temperature of high temperature solid solution continuous annealing is: 900～1000 ℃, order transformation heat-treat condition: 750 ℃～880 ℃, insulation 12h.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1301875A (en) * | 1999-12-29 | 2001-07-04 | 贵研铂业股份有限公司 | Palladium base alloy of electric contact material and palladium base composite contactor |
| CN102809634A (en) * | 2012-08-28 | 2012-12-05 | 济南大学 | Gas-sensitive sensor made of palladium hybridization ferroferric oxide nanometer material |
| CN103173646A (en) * | 2013-01-22 | 2013-06-26 | 昆明理工大学 | Iron-palladium alloy nanometer wire and preparation method thereof |
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- 2014-08-06 CN CN201410382770.7A patent/CN104164584A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1301875A (en) * | 1999-12-29 | 2001-07-04 | 贵研铂业股份有限公司 | Palladium base alloy of electric contact material and palladium base composite contactor |
| CN102809634A (en) * | 2012-08-28 | 2012-12-05 | 济南大学 | Gas-sensitive sensor made of palladium hybridization ferroferric oxide nanometer material |
| CN103173646A (en) * | 2013-01-22 | 2013-06-26 | 昆明理工大学 | Iron-palladium alloy nanometer wire and preparation method thereof |
Non-Patent Citations (1)
| Title |
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| 尹俊美等: "钯铁合金有序化转变与性能研究", 《贵金属》 * |
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Application publication date: 20141126 |