CN103952583B - Reinforced platinum/rhodium 10-platinum fine thermocouple wire for quick temperature measurement and preparation method thereof - Google Patents
Reinforced platinum/rhodium 10-platinum fine thermocouple wire for quick temperature measurement and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a reinforced platinum/rhodium 10-platinum fine thermocouple wire for quick temperature measurement and a preparation method thereof. The material comprises a positive pole PtRh10 material and a negative pole Pt material, wherein the positive pole PtRh10 material comprises the following components in parts by weight: 89.9-90.1 parts of platinum, 9.9-10.1 parts of rhodium, 0-0.003 part of yttrium, 0-0.003 part of zirconium, and 0-0.003 part of cerium; the negative pole Pt material comprises the following components in parts by weight: 99.9-100 parts of platinum, 0-0.003 part of yttrium, 0-0.003 part of zirconium and 0-0.003 part of cerium; and the yttrium, zirconium and cerium are distributed in the material matrix in a dispersed manner in the form of fine oxide. When the materials are prepared into the platinum/rhodium thermocouple wire, the minimum diameter is phi0.035mm, and the application range is phi0.035-0.07mm. The reinforced platinum/rhodium 10-platinum fine thermocouple wire has the properties of quick, accurate and stable temperature measurement, high reliability, high strength and the like.
Description
Technical field
The invention belongs to precious metal material field, particularly to a kind of quick temperature measurement strengthening platinum rhodium fine thermo wires of 10-platinum
And preparation method and preparation method.
Background technology
In metallurgy industry, the requirement of molten steel thermometric is quick, accurate, stable, and only reaching requirements above could realize
Smelting iron and steel and the accurate control of processing key technique.The used material of molten steel thermometric belongs to quick consumption-type thermal couple material
(being called for short fast even material), this material is mainly platinum rhodium aeries of thermocouples microfilament, and the thermal response time of platinum rhodium thermo wires is straight with silk material
Footpath is inversely proportional to, and the thermo wires diameter the thinnest response time is the fastest.At present, domestic measuring temp of molten steel is with fine platinum rhodium thermo wires diameter usually, it is impossible to more rapid, accurately, stably thermometric, affect the technology controlling and process of smelting iron and steel.Meanwhile,
When preparing platinum rhodium thermo wires, silk material is the thinnest, and because intensity and glacing flatness difference are wayward, its yield rate is the lowest.
Summary of the invention
The purpose of the present invention is aiming at the deficiencies in the prior art, it is provided that a kind of quick temperature measurement strengthening platinum rhodium 10-platinum is micro-
Thin thermo wires and preparation method, when described material is prepared as platinum rhodium thermo wires, its minimum diameter is, range is, have quick, accurately, stably thermometric, and the performance such as high reliability, high intensity.
For achieving the above object, the present invention adopts the following technical scheme that
Quick temperature measurement strengthening platinum rhodium 10-platinum fine thermo wires material, including positive pole PtRh10 material and negative pole Pt material,
The weight portion of the described positive pole each component of PtRh10 material is:
The weight portion of the described negative pole each component of Pt material is:
Yttrium in positive and negative electrode, zirconium, cerium are distributed in material matrix with the fine oxide dispersion obtained through high temperature oxidation process
In, zirconium oxide, yittrium oxide, cerium oxide all represent containing the weight portion of zirconium, yttrium or cerium with it.
Described zirconium oxide, yittrium oxide, the metal oxygen rate of cerium oxide are more than 99.5%.
The preparation method of quick temperature measurement strengthening platinum rhodium 10-platinum fine thermo wires material, has following steps:
1) according to the proportion ingredient of each material of above-mentioned both positive and negative polarity；
2) fine vacuum intermediate frequency (IF) smelting:
Step 1) described by each for positive pole proportioning materials under the conditions of argon shield, vacuum is 1 × 10-3～1 × 10-5Pa,
Smelting temperature is 1850～1900 DEG C, melting, and after each material is completely melt, magnetic stirs and is incubated 2～5 minutes, quickly waters
Casting obtains positive pole ingot casting；
Step 1) described by each for negative pole material dispensing under the conditions of argon shield, vacuum is 1 × 10-3～1 × 10-5Pa,
Smelting temperature is 1770～1850 DEG C, melting, and material carries out intermediate frequency magnetic and stirs and be incubated 2～5 minutes, soon after being completely melt
Speed casting obtains negative pole ingot casting；
3) hot-working:
Step 2) described in middle positive pole ingot casting be placed in heat-treatment furnace, at 1250～1400 DEG C make annealing treatment 30～60 points
Clock；Forge hot, initial forging temperature is 1300～1400 DEG C, and forging 5～10 times of beginning, final forging temperature is 1100～1250 DEG C, finish-forging 5～10
Secondary；Homogenization heat treatment 0.5～2 hours at 1100～1250 DEG C subsequently, repeatedly rolling obtainsAlloy billet；?
Homogenization heat treatment 15～30 minutes at 1000～1100 DEG C, stress relief annealing；
By step 2) gained negative pole ingot casting is placed in heat-treatment furnace, makes annealing treatment 30～60 points at 1150～1300 DEG C
Clock, forge hot, initial forging temperature is 1200～1300 DEG C, and forging 5～10 times of beginning, final forging temperature is 1000～1200 DEG C, finish-forging 5～10
Secondary, homogenization heat treatment 0.5～2 hours at 850～1100 DEG C subsequently, repeatedly rolling obtainsAlloy billet,
Homogenization heat treatment 15～30 minutes stress relief annealings is carried out at 700～900 DEG C；
4) just silk drawing:
By step 3) described in the respectively drawing of both positive and negative polarity alloy billet, every time deflection is 8%～15%, is drawn to, obtain positive and negative polar filament material；
5) positive and negative polar filament material high temperature oxidation process:
High-temperature oxydation temperature is 700～1000 DEG C；Oxygen pressure is 102～105Pa；Silk material string diameter Φ 2mm time high-temperature oxydation 5～
10 hours, during string diameter Φ 0.2mm, high-temperature oxydation 8～40 hours；
6) fine drawing:
Through the positive and negative polar filament material drawing of high temperature oxidation process, it is 5%～12% according to pass deformation, is drawn to minimum straight
Footpath reachesMicrofilament, obtains rolling positive and negative polar filament material；
7) microfilament stress relief annealing:
Step 6) described in rolling positive polar filament material annealing, temperature 350～550 DEG C, threading speed is 30～70r/m, rolling
Negative electrode filament material is annealed, and temperature 300～450 DEG C, threading speed is 30～70r/m.
In step 7) stress relief annealing during apply a backward pull device and make a material exceptionally straight, its effect is both to have reduced to move back
Fire temperature, can guarantee that again preferable intensity and preferable glacing flatness simultaneously, it is simple to fast even processing and fabricating.Positive polar filament material is applied
Backward pull is 3～20N, and the backward pull that negative electrode filament material is applied is 3～15N.
Material of the present invention compared with platinum rhodium 10-platinum thermocouple microfilament of the prior art, by add trace zirconium,
Yttrium, cerium one or several, carry out high temperature oxidation process, make zirconium, yttrium, cerium be formed during high temperature oxidation process and be uniformly distributed
Hardening constituent zirconium oxide in platinum-rhodium alloy (positive pole) and platinum alloy (negative pole), or/and yittrium oxide is or/and cerium oxide, is greatly improved
The tensile strength of material and processing characteristics, significantly improve material miniaturization simultaneously and prepare yield rate, reduce platinum, rhodium precious metal
Consumption, cost is greatly lowered, meets the requirements such as molten steel thermometric in the industry such as iron and steel, metallurgy is quick, accurate and effective, stable.
When material of the present invention is prepared as platinum rhodium thermo wires, its diameter up to, range is, there is high reliability, the performance of high intensity.
The unit of weight portion of the present invention is gram, kilogram.
Platinum, rhodium, zirconium, yttrium, the tenor of cerium are 99.99%.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is further illustrated, but the most therefore limits the present invention to described reality
Execute among example scope.
The proportioning of the quick temperature measurement strengthening platinum rhodium 10-platinum fine thermo wires each component of material of embodiment 1 to 3 is shown in Table 1
Table 1 platinum rhodium 10-platinum thermocouple material component table
Take each material described in table 1 embodiment 1-3, prepare quick temperature measurement strengthening platinum rhodium 10-the most by the following method
Platinum fine thermo wires material:
(1), fine vacuum intermediate frequency (IF) smelting: each for the positive pole prepared in step 1 component raw material is put in fine vacuum intermediate frequency, very
Reciprocal of duty cycle is 1 × 10-3～1 × 10-5Pa, smelting temperature is 1850～1900 DEG C, is filled with argon shield simultaneously, the most molten at material
Carry out intermediate frequency magnetic after change stir and be incubated 2～5 minutes, it is thus achieved that liquid metal quickly water to cast from water cooled copper mould and just obtain
Pole ingot casting.Each for the negative pole prepared in step a component raw material is put in fine vacuum intermediate frequency, is 1 × 10 in vacuum-3～1 × 10-5Pa, smelting temperature is 1770～1850 DEG C, is filled with argon shield simultaneously, carries out the stirring of intermediate frequency magnetic all after material is completely melt
Even and be incubated 2～5 minutes, it is thus achieved that liquid metal quickly water to cast from water cooled copper mould obtain negative pole ingot casting；
(2), hot-working: positive pole ingot casting in (1) is placed in heat-treatment furnace, at 1250～1400 DEG C make annealing treatment 30～
60 minutes, then carrying out forge hot on the pneumatic hammer of 250Kg, initial forging temperature is 1300～1400 DEG C, forging 5～10 times of beginning, finish-forging
Temperature is 1100～1250 DEG C, finish-forging 5～10 times, and the platinum rhodium ingot after forge hot is carried out at uniform heat-transformation at 1100～1250 DEG C
Managing 0.5～2 hour, on bar mill, repeatedly homogeneous deformation rolling obtainsAlloy billet, enter at 1000～1100 DEG C
Row homogenization heat treatment 15～30 minutes stress relief annealings.Negative pole ingot casting in (1) is placed in heat-treatment furnace, 1150～1300
Making annealing treatment 30～60 minutes at DEG C, then carry out forge hot on the pneumatic hammer of 250Kg, initial forging temperature is 1200～1300 DEG C,
Beginning to forge 5～10 times, final forging temperature is 1000～1200 DEG C, finish-forging 5～10 times, and the platinum rhodium ingot after forge hot is at 850～1100 DEG C
Under carry out homogenization heat treatment 0.5～2 hours, on bar mill, repeatedly homogeneous deformation rolling obtainsAlloy billet,
Homogenization heat treatment 15～30 minutes stress relief annealings is carried out at 700～900 DEG C；
(3), first silk drawing: the alloy billet of (2) is carried out cold deformation drawing processing on rope type drawbench, according to passage
Deflection is 8%～15%, is drawn to, it is thus achieved that become curled hair material；
(4), high temperature oxidation process: high-temperature oxydation temperature is 700～1000 DEG C；Oxygen pressure is 102～105Pa；Silk material string diameter Φ
High-temperature oxydation 5～10 hours during 2mm, during string diameter Φ 0.2mm, high-temperature oxydation 8～40 hours；
(5), filament draws: draws on water tank drawbench through the silk material of high temperature oxidation process, deforms according to passage
Amount is 5%～12%, is drawn to minimum diameter and reachesMicrofilament, it is thus achieved that monotubular weight reaches more than 100g's
Become curled hair material；
(6), microfilament stress relief annealing: described quick temperature measurement novel platinum rhodium thermocouple microfilament positive polar filament material is being answered
Carrying out filament annealing, temperature 350～550 DEG C on machine, threading speed is 30～70r/m, and negative electrode filament material is carried out on rewinding machine
Filament is annealed, and temperature 300～450 DEG C, threading speed is 30～70r/m.The backward pull that positive polar filament material is applied is 3～20N, negative
The backward pull that polar filament material is applied is 3～15N.
Performance test:
After testing, material room temperature tensile strength values and the more common thermo wires of high temperature endurance performance described in embodiment 1 to 3 improve
More than 30%.Potential test according to GB GB/T1598-2010 for S type PtRh10-Pt thermocouple wire thermoelectrical potential requirement,
Test its electromotive force at different temperatures and meet Standard.
The ultimate principle of the present invention, principal character and advantages of the present invention have more than been shown and described.The technology of the industry
Personnel, it should be appreciated that the present invention is not restricted to the described embodiments, simply illustrating this described in above-described embodiment and description
The principle of invention, without departing from the spirit and scope of the present invention, the present invention also has various changes and modifications, and these become
Change and improvement both falls within scope of the claimed invention.Claimed scope by appending claims and
Equivalent defines.
Claims (4)
1. quick temperature measurement strengthening platinum rhodium 10-platinum fine thermo wires material, it is characterised in that include positive pole PtRh10 material and
Negative pole Pt material,
The weight portion of the described positive pole each component of PtRh10 material is: platinum 89.9～90.1 parts；Rhodium 9.9～10.1 parts；Yttrium 0～
0.003 part；Zirconium 0～0.003 part；Cerium 0～0.003 part；
The weight portion of the described negative pole each component of Pt material is: platinum 99.9～100 parts；Yttrium 0～0.003 part；Zirconium 0～0.003 part；Cerium
0～0.003 part；
Yttrium in positive and negative electrode, zirconium, cerium are distributed in material matrix with the fine oxide dispersion obtained through high temperature oxidation process,
Zirconium oxide, yittrium oxide, cerium oxide all represent containing the weight portion of zirconium, yttrium or cerium with it
This material is prepared by the following method and obtains:
1) according to the proportion ingredient of each material of above-mentioned both positive and negative polarity；
2) fine vacuum intermediate frequency (IF) smelting:
Described in step 1) by each for positive pole proportioning materials under the conditions of argon shield, vacuum is 1 × 10-3~1×10-5Pa, melting temperature
Degree is 1850 ~ 1900 DEG C, melting, and after each material is completely melt, magnetic stirs and is incubated 2 ~ 5 minutes, and quickly casting just obtains
Pole ingot casting；
Described in step 1) by each for negative pole material dispensing under the conditions of argon shield, vacuum is 1 × 10-3~1×10-5Pa, melting temperature
Degree is 1770 ~ 1850 DEG C, melting, and material carries out intermediate frequency magnetic and stirs and be incubated 2 ~ 5 minutes after being completely melt, quickly cast
To negative pole ingot casting；
3) hot-working:
Step 2) described in positive pole ingot casting be placed in heat-treatment furnace, at 1250～1400 DEG C make annealing treatment 30～60 minutes；Heat
Forging, initial forging temperature is 1300～1400 DEG C, and forging 5～10 times of beginning, final forging temperature is 1100～1250 DEG C, finish-forging 5～10 times；Subsequently
Homogenization heat treatment 0.5～2 hours at 1100～1250 DEG C, repeatedly rolling obtains the alloy billet of 4.0mm；1000～
Homogenization heat treatment 15～30 minutes at 1100 DEG C, stress relief annealing；
By step 2) gained negative pole ingot casting is placed in heat-treatment furnace, makes annealing treatment 30～60 minutes at 1150～1300 DEG C, heat
Forging, initial forging temperature is 1200～1300 DEG C, and forging 5～10 times of beginning, final forging temperature is 1000～1200 DEG C, finish-forging 5～10 times, subsequently
Homogenization heat treatment 0.5～2 hours at 850～1100 DEG C, repeatedly rolling obtains the alloy billet of 4.0mm, 700～900
Homogenization heat treatment 15～30 minutes stress relief annealings is carried out at DEG C；
4) just silk drawing:
By the drawing respectively of the both positive and negative polarity alloy billet described in step 3), every time deflection is 8% ~ 15%, is drawn to 0.2mm,
Obtain positive and negative polar filament material；
5) positive and negative polar filament material high temperature oxidation process:
High-temperature oxydation temperature is 700 ~ 1000 DEG C；Oxygen pressure is 102~105Pa；During string diameter 0.2mm, high-temperature oxydation 8 ~ 40 hours；
6) fine drawing:
Through the positive and negative polar filament material drawing of high temperature oxidation process, it is 5% ~ 12% according to pass deformation, is drawn to minimum diameter and reaches
0.035mm microfilament, obtains rolling positive and negative polar filament material；
7) microfilament stress relief annealing:
Rolling positive polar filament material annealing described in step 6), temperature 350 ~ 550 DEG C, threading speed is 30 ~ 70r/min, rolling negative pole
Silk material annealing, temperature 300 ~ 450 DEG C, threading speed is 30 ~ 70r/min.
Material the most according to claim 1, it is characterised in that: zirconium oxide, yittrium oxide, the metal oxygen rate of cerium oxide are more than
99.5%。
3. the preparation method of material described in claim 1 or 2, it is characterised in that have following steps:
1) according to the proportion ingredient of each component of both positive and negative polarity described in claim 1；
2) fine vacuum intermediate frequency (IF) smelting:
Described in step 1) by each for positive pole proportioning materials under the conditions of argon shield, vacuum is 1 × 10-3~1×10-5Pa, melting temperature
Degree is 1850 ~ 1900 DEG C, melting, and after each material is completely melt, magnetic stirs and is incubated 2 ~ 5 minutes, and quickly casting just obtains
Pole ingot casting；
Described in step 1) by each for negative pole material dispensing under the conditions of argon shield, vacuum is 1 × 10-3~1×10-5Pa, melting temperature
Degree is 1770 ~ 1850 DEG C, melting, and material carries out intermediate frequency magnetic and stirs and be incubated 2 ~ 5 minutes after being completely melt, quickly cast
To negative pole ingot casting；
3) hot-working:
Step 2) described in positive pole ingot casting be placed in heat-treatment furnace, at 1250～1400 DEG C make annealing treatment 30～60 minutes；Heat
Forging, initial forging temperature is 1300～1400 DEG C, and forging 5～10 times of beginning, final forging temperature is 1100～1250 DEG C, finish-forging 5～10 times；Subsequently
Homogenization heat treatment 0.5～2 hours at 1100～1250 DEG C, repeatedly rolling obtains the alloy billet of 4.0mm；1000～
Homogenization heat treatment 15～30 minutes at 1100 DEG C, stress relief annealing；
By step 2) gained negative pole ingot casting is placed in heat-treatment furnace, makes annealing treatment 30～60 minutes at 1150～1300 DEG C, heat
Forging, initial forging temperature is 1200～1300 DEG C, and forging 5～10 times of beginning, final forging temperature is 1000～1200 DEG C, finish-forging 5～10 times, subsequently
Homogenization heat treatment 0.5～2 hours at 850～1100 DEG C, repeatedly rolling obtains the alloy billet of 4.0mm, 700～900
Homogenization heat treatment 15～30 minutes stress relief annealings is carried out at DEG C；
4) just silk drawing:
By the drawing respectively of the both positive and negative polarity alloy billet described in step 3), every time deflection is 8% ~ 15%, is drawn to 0.2mm,
Obtain positive and negative polar filament material；
5) positive and negative polar filament material high temperature oxidation process:
High-temperature oxydation temperature is 700 ~ 1000 DEG C；Oxygen pressure is 102~105Pa；During string diameter 0.2mm, high-temperature oxydation 8 ~ 40 hours；
6) fine drawing:
Through the positive and negative polar filament material drawing of high temperature oxidation process, it is 5% ~ 12% according to pass deformation, is drawn to minimum diameter and reaches
0.035mm microfilament, obtains rolling positive and negative polar filament material；
7) microfilament stress relief annealing:
Rolling positive polar filament material annealing described in step 6), temperature 350 ~ 550 DEG C, threading speed is 30 ~ 70r/min, rolling negative pole
Silk material annealing, temperature 300 ~ 450 DEG C, threading speed is 30 ~ 70r/min.
Preparation method the most according to claim 3, it is characterised in that: apply posttension during the stress relief annealing of step 7)
Power is by exceptionally straight for silk material, and the backward pull that its positive polar filament material is applied is 3 ~ 20N, and the backward pull that negative electrode filament material is applied is 3 ~ 15N.
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| CN105483583B (en) * | 2015-12-25 | 2017-07-28 | 无锡英特派金属制品有限公司 | The preparation method of dispersion intensifying platinum thermo wires |
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| CN111519058B (en) * | 2020-04-29 | 2021-10-15 | 重庆国际复合材料股份有限公司 | Preparation method of in-situ synthesized nano-oxide particle dispersion strengthened platinum-based alloy material |
| CN111910099B (en) * | 2020-06-24 | 2022-03-08 | 重庆材料研究院有限公司 | Fine platinum wire for nuclear grade platinum resistance thermometer and preparation method thereof |
| CN111922114B (en) * | 2020-06-24 | 2022-08-02 | 重庆材料研究院有限公司 | High-purity fine platinum wire and preparation method thereof |
| CN111876624B (en) * | 2020-07-15 | 2022-06-28 | 英特派铂业股份有限公司 | Preparation method of high-performance pure platinum thermocouple wire |
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