CN103952585B - Platinum-rhodium thermocouple fine wire material for quick temperature measurement and preparation method thereof - Google Patents
Platinum-rhodium thermocouple fine wire material for quick temperature measurement and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a platinum-rhodium thermocouple fine wire material for quick temperature measurement and a preparation method thereof. The material comprises a positive pole PtRh30 material and a negative pole PtRh6 material. The positive pole PtRh30 material comprises the following components in parts by weight: 69.9-70.4 parts of platinum, 29.6-30.1 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 PtRh6 material comprises the following components in parts by weight: 93.8-94.1 parts of platinum, 5.9-6.2 parts of rhodium, 0-0.003 part of yttrium, 0-0.003 part of zirconium and 0-0.003 part of cerium. The yttrium, zirconium and cerium are dispersed in the material in the form of fine oxides. The oxides are represented by parts by weight of zirconium, yttrium or cerium. When the material is prepared into a platinum-rhodium couple wire, the minimum diameter is phi0.035mm, and the application range is phi0.035-0.07mm. The material has the advantages of high speed, accuracy and stability for temperature measurement, high reliability, high strength and the like.
Description
Technical field
The invention belongs to precious metal material field, fine particularly to a kind of platinum rhodium thermocouple for quick temperature measurement
Wire material and preparation method.
Background technology
In metallurgy industry, the requirement of molten steel thermometric is quick, accurate, stable, only reaches requirements above
The accurate control of smelting iron and steel and processing key technique could be realized.The used material of molten steel thermometric belongs to quick
Consumption-type thermal couple material (is called for short fast even material), and this material is mainly platinum rhodium aeries of thermocouples microfilament, platinum
The thermal response time of rhodium thermo wires is inversely proportional to silk material diameter, 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 usuallyCan not be more rapid, accurate
Really, stably thermometric, affect the technology controlling and process of smelting iron and steel.Meanwhile, when preparing platinum rhodium thermo wires, silk material is more
Carefully, 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 platinum rhodium heat for quick temperature measurement
Galvanic couple microfilament material, when described material is prepared as platinum rhodium thermo wires, its minimum diameter isUse
Scope isHave thermometric quickly, accurately, stable and high reliability, high-strength
The performances such as degree.
For achieving the above object, the present invention adopts the following technical scheme that
For the platinum rhodium thermocouple microfilament material of quick temperature measurement, including positive pole PtRh30 material and negative pole PtRh6
Material,
The weight portion of described its each component of positive pole PtRh30 is:
The weight portion of the described negative pole each component of PtRh6 material is:
Yttrium in positive and negative electrode, zirconium, cerium are distributed in the fine oxide dispersion obtained through high temperature oxidation process
In material matrix, 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%.
For the preparation method of the platinum rhodium thermocouple microfilament material of quick temperature measurement, there are 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 1900～1980 DEG C, melting, and after each material is completely melt, magnetic stirs and protects
Temperature 2～5 minutes, quickly 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 1800～1880 DEG C, melting, and material carries out intermediate frequency magnetic after being completely melt and stirs
And it is incubated 2～5 minutes, quickly casting obtains negative pole ingot casting；
3) hot-working:
Step 2) described in positive pole ingot casting be placed in heat-treatment furnace, at 1350～1500 DEG C make annealing treatment 30～
60 minutes；Forge hot, initial forging temperature is 1350～1500 DEG C, begin forging 5～10 times, final forging temperature be 1300～
1400 DEG C, finish-forging 5～10 times；Homogenization heat treatment 0.5～2 hours at 1250～1350 DEG C, many subsequently
Secondary rolling obtainsAlloy billet；Homogenization heat treatment 15～30 minutes at 1250～1350 DEG C,
Stress relief annealing；
By step 2) gained negative pole ingot casting is placed in heat-treatment furnace, make annealing treatment at 1250～1350 DEG C 30～
60 minutes, forge hot, initial forging temperature is 1250～1350 DEG C, begin forging 5～10 times, final forging temperature be 1100～
1250 DEG C, finish-forging 5～10 times, homogenization heat treatment 0.5～2 hours at 1100～1250 DEG C, many subsequently
Secondary rolling obtainsAlloy billet, at 1000～1100 DEG C, carry out homogenization heat treatment 15～30 points
Clock stress relief annealing；
4) just silk drawing:
By step 3) described in the respectively drawing of both positive and negative polarity alloy billet, every time deflection is 5%～12%,
It is drawn toObtain 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；High temperature during silk material string diameter Φ 2mm
Aoxidize 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%～10% according to pass deformation, is drawn to
Minimum diameter 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 500～700 DEG C, threading speed is 30～70r/m,
Rolling negative electrode filament material is annealed, and temperature 350～500 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
Reduce annealing temperature, can guarantee that again preferable intensity and preferable glacing flatness simultaneously, it is simple to fast even processing and fabricating.
The backward pull that positive polar filament material is applied is 3～20N, and the backward pull that negative electrode filament material is applied is 3～15N.
Material of the present invention is compared with Platinum-30Rhodium-Platinum-6Rhodium thermocouple microfilament of the prior art, by adding
Add trace zirconium, yttrium, cerium one or several, carry out high temperature oxidation process, make zirconium, yttrium, cerium in high temperature oxygen
Change and processing procedure forms the hardening constituent zirconium oxide being evenly distributed in platinum-rhodium alloy or/and yittrium oxide is or/and oxygen
Change cerium, substantially increase tensile strength and the processing characteristics of material, significantly improve material miniaturization simultaneously and prepare
Yield rate, reduces platinum, the consumption of rhodium precious metal, cost is greatly lowered, and meets the row such as iron and steel, metallurgy
The requirement such as in industry molten steel thermometric is quick, accurate and effective, stable.
When material of the present invention is prepared as platinum rhodium thermo wires, its diameter up toRange isThere 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 institute
Among the scope of embodiments stated.
The proportioning for the platinum rhodium thermocouple each component of microfilament material of quick temperature measurement of embodiment 1 to 3 is shown in Table 1
Table 1 Platinum-30Rhodium-Platinum-6Rhodium thermocouple material component table
Take each material described in table 1 embodiment 1-3, prepare the platinum rhodium for quick temperature measurement the most by the following method
Thermocouple microfilament material:
(1), fine vacuum intermediate frequency (IF) smelting:
The each component raw material of positive pole prepared in step 1 is put in fine vacuum intermediate frequency, is 1 × 10 in vacuum-3～1
×10-5Pa, smelting temperature is 1900～1980 DEG C, is filled with argon shield simultaneously, is completely melt at material laggard
Row intermediate frequency magnetic stirs and is incubated 2～5 minutes, it is thus achieved that liquid metal quickly water and cast from water cooled copper mould
To positive pole ingot casting.
The each component raw material of negative pole that step 1 prepares is put in fine vacuum intermediate frequency, is 1 × 10 in vacuum-3～1 ×
10-5Pa, smelting temperature is 1800～1880 DEG C, is filled with argon shield simultaneously, carries out after material is completely melt
Intermediate frequency magnetic stirs and is incubated 2～5 minutes, it is thus achieved that liquid metal quickly water to cast from water cooled copper mould and obtain
Negative pole ingot casting；
(2), hot-working: the middle positive pole ingot casting described in step 1 is placed in heat-treatment furnace, 1350～1500
Make annealing treatment 30～60 minutes at DEG C；Forge hot, initial forging temperature is 1350～1500 DEG C, forging 5～10 times of beginning,
Final forging temperature is 1300～1400 DEG C, finish-forging 5～10 times；Subsequently at 1250～1350 DEG C at uniform heat-transformation
Managing 0.5～2 hour, repeatedly rolling obtainsAlloy billet；Uniform heat-transformation at 1250～1350 DEG C
Process 15～30 minutes, stress relief annealing；Negative pole ingot casting in step 1 is placed in heat-treatment furnace, 1250～
Make annealing treatment 30～60 minutes at 1350 DEG C, on the pneumatic hammer of 250Kg, then carry out forge hot, initial forging temperature
It is 1250～1350 DEG C, forging 5～10 times of beginning, final forging temperature is 1100～1250 DEG C, finish-forging 5～10 times,
Platinum rhodium ingot after forge hot carries out homogenization heat treatment 0.5～2 hours at 1100～1250 DEG C, at bar mill
On repeatedly homogeneous deformation rolling obtainAlloy billet, carry out at uniform heat-transformation at 1000～1100 DEG C
Manage 15～30 minutes stress relief annealings；
(3), first silk drawing: the alloy billet of step 2 is carried out cold deformation drawing on rope type drawbench and adds
Work, is 5%～12% according to pass deformation, is drawn toObtain into curled hair material；
(4), high temperature oxidation process: high-temperature oxydation temperature is 700～1000 DEG C；Oxygen pressure is 102～105Pa；Silk
High-temperature oxydation 5～10 hours during material string diameter Φ 2mm, during string diameter Φ 0.2mm, high-temperature oxydation 8～40 hours；
(5), filament draws: draw on water tank drawbench through the silk material of high temperature oxidation process, according to
Pass deformation is 5%～10%, is drawn to minimum diameter and reachesMicrofilament, it is thus achieved that monotubular weight
Amount reaches the one-tenth curled hair material of more than 100g；
(6), microfilament stress relief annealing: described quick temperature measurement is with novel platinum rhodium thermocouple microfilament positive pole
Silk material carries out filament annealing, temperature 500～700 DEG C on rewinding machine, and threading speed is 30～70r/m, negative pole
Silk material carries out filament annealing, temperature 350～500 DEG C on rewinding machine, and threading speed is 30～70r/m.Positive pole
The silk backward pull that applied of material is 3～20N, and the backward pull that negative electrode filament material is applied is 3～15N, obtain for
The Platinum-30Rhodium-Platinum-6Rhodium thermocouple microfilament material of quick temperature measurement.
Performance test:
After testing, material room temperature tensile strength values and high temperature endurance performance described in embodiment 1 to 3 are more common
Thermo wires improves more than 30%.Potential test according to GB GB/T1598-2010 for Type B
PtRh30-PtRh6 thermocouple wire thermoelectrical potential requirement, tests its electromotive force at different temperatures and meets Standard.
The ultimate principle of the present invention, principal character and advantages of the present invention have more than been shown and described.The skill of the industry
Art personnel are it should be appreciated that the present invention is not restricted to the described embodiments, described in above-described embodiment and description
The principle that the present invention is simply described, without departing from the spirit and scope of the present invention, the present invention also can
Having various changes and modifications, these changes and improvements both fall within scope of the claimed invention.The present invention
Claimed scope is defined by appending claims and equivalent thereof.
Claims (4)
1. the platinum rhodium thermocouple microfilament material for quick temperature measurement, it is characterised in that include positive pole PtRh30 material and negative pole PtRh6 material,
The weight portion of described its each component of positive pole PtRh30 is: 69.9 ~ 70.4 parts of platinum;Rhodium 29.6～30.1 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 PtRh6 material is: 93.8 ~ 94.1 parts of platinum；Rhodium 5.9～6.2 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, and 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, smelting temperature is 1900 ~ 1980 DEG C, melting, and after each material is completely melt, magnetic stirs and is incubated 2 ~ 5 minutes, and quickly casting obtains positive 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, smelting temperature is 1800 ~ 1880 DEG C, melting, and material carries out intermediate frequency magnetic and stirs and be incubated 2 ~ 5 minutes after being completely melt, quickly casting obtains negative pole ingot casting；
3) hot-working:
Step 2) described in positive pole ingot casting be placed in heat-treatment furnace, at 1350～1500 DEG C make annealing treatment 30～60 minutes；Forge hot, initial forging temperature is 1350～1500 DEG C, and forging 5～10 times of beginning, final forging temperature is 1300～1400 DEG C, finish-forging 5～10 times；Homogenization heat treatment 0.5～2 hours at 1250～1350 DEG C subsequently, repeatedly rolling obtains the alloy billet of 4.0mm；Homogenization heat treatment 15～30 minutes at 1250～1350 DEG C, stress relief annealing；
By step 2) gained negative pole ingot casting is placed in heat-treatment furnace, make annealing treatment 30～60 minutes at 1250～1350 DEG C, forge hot, initial forging temperature is 1250～1350 DEG C, forging 5～10 times of beginning, and final forging temperature is 1100～1250 DEG C, finish-forging 5～10 times, homogenization heat treatment 0.5～2 hours at 1100～1250 DEG C subsequently, repeatedly rolling obtains the alloy billet of 4.0mm, carries out homogenization heat treatment 15～30 minutes stress relief annealings at 1000～1100 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 5% ~ 12%, is drawn to 0.2mm, obtains 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% ~ 10% according to pass deformation, is drawn to minimum diameter and reaches 0.035mm microfilament, obtain rolling positive and negative polar filament material；
7) microfilament stress relief annealing:
Rolling positive polar filament material annealing described in step 6), temperature 500 ~ 700 DEG C, threading speed is 30 ~ 70r/ min, and rolling negative electrode filament material is annealed, and temperature 350 ~ 500 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 material 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, smelting temperature is 1900 ~ 1980 DEG C, melting, and after each material is completely melt, magnetic stirs and is incubated 2 ~ 5 minutes, and quickly casting obtains positive 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, smelting temperature is 1800 ~ 1880 DEG C, melting, and material carries out intermediate frequency magnetic and stirs and be incubated 2 ~ 5 minutes after being completely melt, quickly casting obtains negative pole ingot casting；
3) hot-working:
Step 2) described in positive pole ingot casting be placed in heat-treatment furnace, at 1350～1500 DEG C make annealing treatment 30～60 minutes；Forge hot, initial forging temperature is 1350～1500 DEG C, and forging 5～10 times of beginning, final forging temperature is 1300～1400 DEG C, finish-forging 5～10 times；Homogenization heat treatment 0.5～2 hours at 1250～1350 DEG C subsequently, repeatedly rolling obtains the alloy billet of 4.0mm；Homogenization heat treatment 15～30 minutes at 1250～1350 DEG C, stress relief annealing；
By step 2) gained negative pole ingot casting is placed in heat-treatment furnace, make annealing treatment 30～60 minutes at 1250～1350 DEG C, forge hot, initial forging temperature is 1250～1350 DEG C, forging 5～10 times of beginning, and final forging temperature is 1100～1250 DEG C, finish-forging 5～10 times, homogenization heat treatment 0.5～2 hours at 1100～1250 DEG C subsequently, repeatedly rolling obtains the alloy billet of 4.0mm, carries out homogenization heat treatment 15～30 minutes stress relief annealings at 1000～1100 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 5% ~ 12%, is drawn to 0.2mm, obtains 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% ~ 10% according to pass deformation, is drawn to minimum diameter and reaches 0.035mm microfilament, obtain rolling positive and negative polar filament material；
7) microfilament stress relief annealing:
Rolling positive polar filament material annealing described in step 6), temperature 500 ~ 700 DEG C, threading speed is 30 ~ 70r/ min, and rolling negative electrode filament material is annealed, and temperature 350 ~ 500 DEG C, threading speed is 30 ~ 70r/ min.
Preparation method the most according to claim 3, it is characterised in that: during the stress relief annealing of step 7), applying backward pull 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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| GB201615272D0 (en) * | 2016-09-08 | 2016-10-26 | Johnson Matthey Plc | Method |
| CN109518016A (en) * | 2018-10-10 | 2019-03-26 | 安徽鑫国合金有限公司 | A kind of production technology of sensor 20 compensating wire alloy wire of copper-cupro-nickel |
| CN109916529B (en) * | 2019-02-26 | 2021-08-31 | 重庆材料研究院有限公司 | Platinum resistor element for nuclear-grade armored platinum resistor and preparation process |
| 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 |
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