CN103952585A - 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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- CN103952585A CN103952585A CN201410213350.6A CN201410213350A CN103952585A CN 103952585 A CN103952585 A CN 103952585A CN 201410213350 A CN201410213350 A CN 201410213350A CN 103952585 A CN103952585 A CN 103952585A
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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, particularly a kind of platinum rhodium thermocouple microfilament material and preparation method for quick temperature measurement.
Background technology
In metallurgy industry, the requirement of molten steel thermometric is quick, accurate, stable, only reaches the accurate control that above requirement could realize smelting iron and steel and processing key technique.Molten steel material that thermometric is used belongs to quick consumption-type thermal couple material (being called for short fast even material), and this material is mainly platinum rhodium series of heat galvanic couple microfilament, and the thermal response time of platinum rhodium thermo wires is inversely proportional to silk material diameter, and the thinner reaction times of thermo wires diameter is faster.At present, domestic measuring temp of molten steel typically has a diameter from fine platinum rhodium thermo wires
can not be more fast, accurately, thermometric stably, affect the technology controlling and process of smelting iron and steel.Meanwhile, while preparing platinum rhodium thermo wires, silk material thinner, because of intensity and planeness poor wayward, its yield rate is lower.
Summary of the invention
Object of the present invention is exactly for the deficiencies in the prior art, and a kind of platinum rhodium thermocouple microfilament material for quick temperature measurement is provided, and when described material is prepared into platinum rhodium thermo wires, its minimum diameter is
use range is
have thermometric fast, accurately, stable, and the performance such as high reliability, high strength.
For achieving the above object, the present invention adopts following technical scheme:
Platinum rhodium thermocouple microfilament material for quick temperature measurement, comprises anodal PtRh30 material and negative pole PtRh6 material,
The weight part of described anodal its each component of PtRh30 is:
The weight part of described each component of negative pole PtRh6 material is:
Yttrium in positive and negative electrode, zirconium, cerium are distributed in material matrix with the fine oxide dispersion obtaining through high temperature oxidation process, and all with it, the weight part containing zirconium, yttrium or cerium represents for zirconium white, yttrium oxide, cerium oxide.
The metal oxygen rate of described zirconium white, yttrium oxide, cerium oxide is greater than 99.5%.
The preparation method who is used for the platinum rhodium thermocouple microfilament material of quick temperature measurement, has following steps:
1) according to the proportion ingredient of above-mentioned each material of positive and negative electrode;
2) high vacuum intermediate frequency (IF) smelting:
Step 1) described by each proportioning materials of positive pole under argon shield condition, vacuum tightness is 1 * 10
-3～1 * 10
-5pa, smelting temperature is 1900～1980 ℃, melting, after each material melts completely, magnetic stirs and is incubated 2～5 minutes, and casting obtains anodal ingot casting fast;
Step 1) described by each material of negative pole batching under argon shield condition, vacuum tightness is 1 * 10
-3～1 * 10
-5pa, smelting temperature is 1800～1880 ℃, and melting is carried out intermediate frequency magnetic after material melts completely and is stirred and be incubated 2～5 minutes, and casting obtains negative pole ingot casting fast;
3) hot-work:
Step 2) described anodal ingot casting is placed in heat treatment furnace, and anneal is 30～60 minutes at 1350～1500 ℃; Forge hot, initial forging temperature is 1350～1500 ℃, begins to forge 5～10 times, final forging temperature is 1300～1400 ℃, finish-forging 5～10 times; Homogenizing thermal treatment 0.5～2 hour at 1250～1350 ℃ subsequently, repeatedly rolling obtains
alloy preform bar; At 1250～1350 ℃, homogenizing thermal treatment is 15～30 minutes, stress relief annealing;
By step 2) gained negative pole ingot casting is placed in heat treatment furnace, at 1250～1350 ℃, anneal is 30～60 minutes, forge hot, initial forging temperature is 1250～1350 ℃, begin to forge 5～10 times, final forging temperature is 1100～1250 ℃, finish-forging 5～10 times, homogenizing thermal treatment 0.5～2 hour at 1100～1250 ℃ subsequently, repeatedly rolling obtains
alloy preform bar, at 1000～1100 ℃, carry out 15～30 minutes stress relief annealings of homogenizing thermal treatment;
4) just silk drawing:
By step 3) described positive and negative electrode alloy preform bar drawing respectively, every time deflection is 5%～12%, is drawn to
obtain positive and negative polar filament material;
5) positive and negative polar filament material high temperature oxidation process:
High temperature oxidation temperature is 700～1000 ℃; It is 10 that oxygen is pressed
2～10
5pa; During silk material string diameter Φ 2mm, high temperature oxidation is 5～10 hours, during string diameter Φ 0.2mm, and high temperature oxidation 8～40 hours;
6) fine drawing:
Through the positive and negative polar filament material drawing of high temperature oxidation process, according to pass deformation, be 5%～10%, be drawn to minimum diameter and reach
microfilament, obtains the positive and negative polar filament material of rolling;
7) microfilament stress relief annealing:
Step 6) the positive polar filament material annealing of described rolling, 500～700 ℃ of temperature, threading speed is 30～70r/m, the annealing of rolling negative electrode filament material, 350～500 ℃ of temperature, threading speed is 30～70r/m.
In step 7) stress relief annealing process in apply a backward pull device and make a material exceptionally straight, its effect is both to have reduced annealing temperature, can guarantee again good intensity and planeness preferably simultaneously, is convenient to fast even processing and fabricating.The backward pull that positive polar filament material applies is 3～20N, and the backward pull that negative electrode filament material applies is 3～15N.
Material of the present invention is compared with Platinum-30Rhodium-Platinum-6Rhodium thermocouple microfilament of the prior art, by adding trace zirconium, yttrium, cerium one or several, carry out high temperature oxidation process, make zirconium, yttrium, cerium in high temperature oxidation process process, form the strengthening phase zirconium white that is evenly distributed in platinum rhodium or/and yttrium oxide or/and cerium oxide, tensile strength and the processing characteristics of material have greatly been improved, significantly improve material miniaturization simultaneously and prepare yield rate, reduce platinum, the consumption of rhodium noble metal, significantly reduce costs, meet iron and steel, in the industries such as metallurgy, molten steel thermometric is quick, accurately, effectively, stablize and wait requirement.
When material of the present invention is prepared into platinum rhodium thermo wires, its diameter can reach
use range is
there is high reliability, high-intensity performance.
The unit of weight part of the present invention is gram, kilogram.
The metal content of platinum, rhodium, zirconium, yttrium, cerium is 99.99%.
Embodiment
Below in conjunction with embodiment, the present invention is further illustrated, but therefore do not limit the present invention among described scope of embodiments.
The proportioning of each component of platinum rhodium thermocouple microfilament material for quick temperature measurement of embodiment 1 to 3 is in Table 1
Table 1 Platinum-30Rhodium-Platinum-6Rhodium thermocouple material component table
Get each material described in table 1 embodiment 1-3, respectively by the following method for the preparation of the platinum rhodium thermocouple microfilament material of quick temperature measurement:
(1), high vacuum intermediate frequency (IF) smelting:
Each component raw material of the positive pole preparing in step 1 is put into high vacuum intermediate frequency, in vacuum tightness, is 1 * 10
-3～1 * 10
-5pa, smelting temperature is 1900～1980 ℃, is filled with argon shield simultaneously, carries out intermediate frequency magnetic and stir and be incubated 2～5 minutes after material melts completely, the liquid metal of acquisition waters fast to cast from and in water cooled copper mould, obtains anodal ingot casting.
Each component raw material of the negative pole that step 1 prepares is put into high vacuum intermediate frequency, in vacuum tightness, is 1 * 10
-3～1 * 10
-5pa, smelting temperature is 1800～1880 ℃, is filled with argon shield simultaneously, carries out intermediate frequency magnetic and stir and be incubated 2～5 minutes after material melts completely, the liquid metal of acquisition waters fast to cast from and in water cooled copper mould, obtains negative pole ingot casting;
(2), hot-work: the middle anodal ingot casting described in step 1 is placed in heat treatment furnace, and anneal is 30～60 minutes at 1350～1500 ℃; Forge hot, initial forging temperature is 1350～1500 ℃, begins to forge 5～10 times, final forging temperature is 1300～1400 ℃, finish-forging 5～10 times; Homogenizing thermal treatment 0.5～2 hour at 1250～1350 ℃ subsequently, repeatedly rolling obtains
alloy preform bar; At 1250～1350 ℃, homogenizing thermal treatment is 15～30 minutes, stress relief annealing; Negative pole ingot casting in step 1 is placed in heat treatment furnace, at 1250～1350 ℃, anneal is 30～60 minutes, then on the air hammer of 250Kg, carry out forge hot, initial forging temperature is 1250～1350 ℃, begin to forge 5～10 times, final forging temperature is 1100～1250 ℃, finish-forging 5～10 times, platinum rhodium ingot after forge hot carries out homogenizing thermal treatment 0.5～2 hour at 1100～1250 ℃, and on bar mill, repeatedly homogeneous deformation rolling obtains
alloy preform bar, at 1000～1100 ℃, carry out 15～30 minutes stress relief annealings of homogenizing thermal treatment;
(3), just silk drawing: the alloy preform bar of step 2 is carried out to cold deformation drawing processing on rope formula cold drawing bench, is 5%～12% according to pass deformation, is drawn to
obtain into curled hair material;
(4), high temperature oxidation process: high temperature oxidation temperature is 700～1000 ℃; It is 10 that oxygen is pressed
2～10
5pa; During silk material string diameter Φ 2mm, high temperature oxidation is 5～10 hours, during string diameter Φ 0.2mm, and high temperature oxidation 8～40 hours;
(5), filament draws: the silk material through high temperature oxidation process draws on water tank drawbench, according to pass deformation, is 5%～10%, is drawn to minimum diameter and reaches
microfilament, obtains monotubular weight and reaches one-tenth curled hair material more than 100g;
(6), microfilament stress relief annealing: described quick temperature measurement carries out filament annealing with the positive polar filament material of novel platinum rhodium thermocouple microfilament on rewinder, 500～700 ℃ of temperature, threading speed is 30～70r/m, negative electrode filament material carries out filament annealing on rewinder, 350～500 ℃ of temperature, threading speed is 30～70r/m.The backward pull that positive polar filament material applies is 3～20N, and the backward pull that negative electrode filament material applies is 3～15N, obtains the Platinum-30Rhodium-Platinum-6Rhodium thermocouple microfilament material for quick temperature measurement.
Performance test:
After testing, the material room temperature tensile strength values described in embodiment 1 to 3 and the more common thermo wires of high temperature endurance performance have improved more than 30%.Hot potential test, is tested its Hot electromotive force and is met GB requirement for the requirement of Type B PtRh30-PtRh6 thermocouple wire thermoelectric force according to GB GB/T1598-2010 under differing temps.More than show and described ultimate principle of the present invention, principal character and advantage of the present invention.The technician of the industry should understand; the present invention is not restricted to the described embodiments; that in above-described embodiment and specification sheets, describes just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention.The claimed scope of the present invention is defined by appending claims and equivalent thereof.
Claims (4)
1. for a platinum rhodium thermocouple microfilament material for quick temperature measurement, it is characterized in that: comprise anodal PtRh30 material and negative pole PtRh6 material,
The weight part of described anodal its each component of PtRh30 is:
The weight part of described each component of negative pole PtRh6 material is:
Yttrium in positive and negative electrode, zirconium, cerium are distributed in material matrix with the fine oxide dispersion obtaining through high temperature oxidation process, and all with it, the weight part containing zirconium, yttrium or cerium represents for zirconium white, yttrium oxide, cerium oxide.
2. material according to claim 1, is characterized in that: the metal oxygen rate of zirconium white, yttrium oxide, cerium oxide is greater than 99.5%.
3. the preparation method of material described in claim 1 or 2, is characterized in that there are following steps:
1) according to the proportion ingredient of each material of positive and negative electrode described in claim 1;
2) high vacuum intermediate frequency (IF) smelting:
Step 1) described by each proportioning materials of positive pole under argon shield condition, vacuum tightness is 1 * 10
-3～1 * 10
-5pa, smelting temperature is 1900～1980 ℃, melting, after each material melts completely, magnetic stirs and is incubated 2～5 minutes, and casting obtains anodal ingot casting fast;
Step 2) described by each material of negative pole batching under argon shield condition, vacuum tightness is 1 * 10
-3～1 * 10
-5pa, smelting temperature is 1800～1880 ℃, and melting is carried out intermediate frequency magnetic after material melts completely and is stirred and be incubated 2～5 minutes, and casting obtains negative pole ingot casting fast;
3) hot-work:
Step 2) described anodal ingot casting is placed in heat treatment furnace, and anneal is 30～60 minutes at 1350～1500 ℃; Forge hot, initial forging temperature is 1350～1500 ℃, begins to forge 5～10 times, final forging temperature is 1300～1400 ℃, finish-forging 5～10 times; Homogenizing thermal treatment 0.5～2 hour at 1250～1350 ℃ subsequently, repeatedly rolling obtains
alloy preform bar; At 1250～1350 ℃, homogenizing thermal treatment is 15～30 minutes, stress relief annealing;
By step 2) gained negative pole ingot casting is placed in heat treatment furnace, at 1250～1350 ℃, anneal is 30～60 minutes, forge hot, initial forging temperature is 1250～1350 ℃, begin to forge 5～10 times, final forging temperature is 1100～1250 ℃, finish-forging 5～10 times, homogenizing thermal treatment 0.5～2 hour at 1100～1250 ℃ subsequently, repeatedly rolling obtains
alloy preform bar, at 1000～1100 ℃, carry out 15～30 minutes stress relief annealings of homogenizing thermal treatment;
4) just silk drawing:
By step 3) described positive and negative electrode alloy preform bar drawing respectively, every time deflection is 5%～12%, is drawn to
obtain positive and negative polar filament material;
5) positive and negative polar filament material high temperature oxidation process:
High temperature oxidation temperature is 700～1000 ℃; It is 10 that oxygen is pressed
2～10
5pa; During silk material string diameter Φ 2mm, high temperature oxidation is 5～10 hours, during string diameter Φ 0.2mm, and high temperature oxidation 8～40 hours;
6) fine drawing:
Through the positive and negative polar filament material drawing of high temperature oxidation process, according to pass deformation, be 5%～10%, be drawn to minimum diameter and reach
microfilament, obtains the positive and negative polar filament material of rolling;
7) microfilament stress relief annealing:
Step 6) the positive polar filament material annealing of described rolling, 500～700 ℃ of temperature, threading speed is 30～70r/m, the annealing of rolling negative electrode filament material, 350～500 ℃ of temperature, threading speed is 30～70r/m.
4. preparation method according to claim 3, is characterized in that: step 7) stress relief annealing process in to apply backward pull exceptionally straight by silk material, the backward pull that its positive polar filament material applies is 3～20N, the backward pull that negative electrode filament material applies is 3～15N.
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| CN109916529A (en) * | 2019-02-26 | 2019-06-21 | 重庆材料研究院有限公司 | Platinum resistive element and preparation process for nuclear leve proof armored platinum resistor |
| WO2021259135A1 (en) * | 2020-06-24 | 2021-12-30 | 重庆材料研究院有限公司 | High-purity fine platinum wire and preparation method |
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| CN109916529A (en) * | 2019-02-26 | 2019-06-21 | 重庆材料研究院有限公司 | Platinum resistive element and preparation process for nuclear leve proof armored platinum resistor |
| WO2021259135A1 (en) * | 2020-06-24 | 2021-12-30 | 重庆材料研究院有限公司 | High-purity fine platinum wire and preparation method |
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