CN111910099A - Fine platinum wire for nuclear grade platinum resistance thermometer and preparation method thereof - Google Patents
Fine platinum wire for nuclear grade platinum resistance thermometer and preparation method thereof Download PDFInfo
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- 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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- B21C37/04—Manufacture of metal sheets, bars, wire, tubes or like semi-manufactured products, not otherwise provided for; Manufacture of tubes of special shape of bars or wire
- B21C37/047—Manufacture of metal sheets, bars, wire, tubes or like semi-manufactured products, not otherwise provided for; Manufacture of tubes of special shape of bars or wire of fine wires
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- C22C1/03—Making non-ferrous alloys by melting using master alloys
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- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/14—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of noble metals or alloys based thereon
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- G01—MEASURING; TESTING
- G01K—MEASURING TEMPERATURE; MEASURING QUANTITY OF HEAT; THERMALLY-SENSITIVE ELEMENTS NOT OTHERWISE PROVIDED FOR
- G01K7/00—Measuring temperature based on the use of electric or magnetic elements directly sensitive to heat ; Power supply therefor, e.g. using thermoelectric elements
- G01K7/16—Measuring temperature based on the use of electric or magnetic elements directly sensitive to heat ; Power supply therefor, e.g. using thermoelectric elements using resistive elements
- G01K7/18—Measuring temperature based on the use of electric or magnetic elements directly sensitive to heat ; Power supply therefor, e.g. using thermoelectric elements using resistive elements the element being a linear resistance, e.g. platinum resistance thermometer
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Abstract
The invention relates to a micro platinum wire for a nuclear grade platinum resistance thermometer and a preparation method thereof, which adopts high-cleanness vacuum melting and bottom pouring type casting processes to effectively ensure the uniformity of components and remove harmful impurities. The fine platinum wire for the nuclear grade platinum resistance thermometer is obtained by adopting precise fine processing and heat treatment, accurately regulating and controlling the uniformity of the structure, effectively controlling the grain size and eliminating the internal vacancy and other micro defects. The smallest diameter of the fine platinum wire reaches 10 mu m, and the resistance temperature coefficient (alpha) meets 0.003851 +/-0.000003 DEG C‑1The fine platinum wire has high uniformity, high precision and high stabilityThe nuclear grade platinum resistance thermometer has the advantages of long service life, irradiation resistance and the like, can meet the performance requirements of key materials of the nuclear grade platinum resistance thermometer, and can be popularized and applied to other high-tech fields.
Description
Technical Field
The invention belongs to the field of metal materials, and particularly relates to a micro platinum wire for a nuclear grade platinum resistance thermometer and a preparation method thereof.
Background
The nuclear-grade platinum resistance thermometer is an important nuclear-grade temperature sensor, the key basic material of the nuclear-grade platinum resistance thermometer is a high-performance fine platinum wire, and the material components, harmful trace element control, mechanical property and electrical property regulation and control, wire uniformity and tissue uniformity of the nuclear-grade platinum resistance thermometer are key influence factors such as measurement accuracy, stability, radiation resistance and other properties and service life of the nuclear-grade platinum resistance thermometer.
The existing technology adopts induction melting to obtain platinum ingots, and then processes such as forging, rolling, drawing and the like are carried out, so that the problems of poor component uniformity, excessive harmful trace elements, poor mechanical property, difficult control of size precision, poor product consistency and the like of the obtained superfine platinum wire are solved. Therefore, the fine platinum wire prepared by the prior art cannot meet the use requirement of the nuclear grade platinum resistance thermometer, so that the fine platinum wire cannot be applied in engineering.
Disclosure of Invention
The invention aims to provide a micro platinum wire for a nuclear grade platinum resistance thermometer and a preparation method thereof aiming at the defects of the existing micro platinum wire and the manufacturing technology, wherein high-purity platinum powder subjected to purification treatment is adopted as a raw material, beneficial elements are added, and the high-purity smelting, high-uniformity structure control and precision micro machining technology are utilized to accurately regulate and control the material components and the structure uniformity, effectively control the grain size and eliminate the internal vacancy and other micro defects so as to obtain the micro platinum wire with high uniformity, high precision, high stability, long service life, irradiation resistance, resistance temperature coefficient and the like(alpha) satisfying 0.003851 + -0.000003 deg.C-1The high-performance fine platinum wire material meets the use requirement of a key material of a nuclear-grade platinum resistance thermometer.
The invention aims to realize the purpose by adopting the following scheme that the micro platinum wire for the nuclear grade platinum resistance thermometer comprises the following components in percentage by weight: the beneficial elements are 0.02-0.08%, the content of harmful elements is less than 30ppm, the balance is platinum, and the purity of the platinum raw material is more than or equal to 99.998%.
The beneficial elements are the combination of two or more of Rh, Ir, Pd and rare earth elements, and the rare earth elements are the combination of two or more of Hf, La, Ce, Gd and Yb.
The better technical scheme is that the weight percentage of each component is as follows: rh: 0.005-0.02%, Ir: 0.001-0.02%, rare earth elements: 0.001-0.01%, and the balance of Pt, wherein the content of harmful elements is less than 30 ppm.
The better technical scheme is that the weight percentage of each component is as follows: rh: 0.008-0.015%, Pd: 0.005-0.008%, rare earth elements: 0.001-0.01%, and the balance of Pt, wherein the content of harmful elements is less than 30 ppm.
The better technical scheme is that the weight percentage of each component is as follows: pd: 0.005-0.008%, Ir: 0.005-0.01%, rare earth elements: 0.003-0.01 percent, and the balance of Pt, wherein the content of harmful elements is less than 30 ppm.
The main harmful elements affecting the radiation resistance are: co, Cu, B, Si, Cd, etc., require strict control and reduction of harmful element content in raw material purity, smelting and processing.
The preparation method of the fine platinum wire for the nuclear grade platinum resistance thermometer comprises the following steps:
1) taking the components of the superfine platinum wire for the nuclear-grade platinum resistance thermometer according to the proportion, wherein the platinum is prepared by coating beneficial elements by 70-80% of the total amount of the platinum, and adopting high-cleanness vacuum induction melting with the vacuum degree of 1 multiplied by 10-2～1×10-3Pa, argon protection, heat preservation for 5-10min after the materials are completely melted, and bottom leakage casting to obtain the intermediate solid solution alloy. The intermediate solid solution alloy and the rest platinum are placed in a crucible by adopting a high crucibleClean vacuum induction melting with vacuum degree of 1 × 10-2～1×10-3Pa, argon protection, heat preservation for 5-10min, bottom leakage casting to obtain final solid alloy;
2) hot forging: carrying out homogenization heat treatment on the final solid alloy obtained in the step 1) at 800-1100 ℃ for 0.5-1 hour, then carrying out hot die forging and pressing to obtain a bar, and carrying out heat treatment on the obtained bar at 500-800 ℃ for 15-30 minutes;
3) wire processing: and (3) carrying out rough drawing with the deformation not more than 15%, medium drawing with the deformation not more than 10% and fine drawing with the deformation not more than 6% on the bar subjected to heat treatment obtained in the step 2) on a wire drawing machine in sequence, wherein the total deformation of drawing is not more than 80%, carrying out heat treatment, namely carrying out heat treatment at the temperature of 400-700 ℃ for 10-30 min, drawing into a finished product of fine platinum wire, and cleaning to obtain the finished product of wire.
The method for coating beneficial elements by using platinum accounting for 70-80% of the total amount in the step 1) comprises the following steps of coating in layers: the bottom layer and the top layer are made of platinum powder, the middle layer is arranged between the bottom layer and the top layer and is beneficial elements, and the beneficial elements are completely wrapped and compacted by the platinum powder.
In the step 2), the bar is a round bar with the size of phi 4 +/-1 mm.
Performing alkaline cooking treatment after the rough drawing stage in the step 3), and performing acid cooking treatment; in the middle pulling stage, alkali cooking treatment is firstly carried out, and then acid cooking treatment is carried out; in the fine drawing stage, firstly, ultrasonic cleaning with absolute ethyl alcohol as a medium is adopted to carry out online continuous cleaning on the drawn finished fine platinum wire, and then ultrasonic cleaning with deionized water as a medium is adopted to carry out online continuous cleaning on the drawn finished fine platinum wire. The method comprises the steps of alkaline boiling, acid boiling, on-line continuous cleaning and the like, and the method can be used for removing foreign matters such as ceramic, foreign metal impurities (such as iron, copper, silicon, calcium, aluminum and the like), micro-particles, oil stains and the like (the same below) attached to the surface.
The alkali boiling, namely washing by using a boiling alkali solution: the volume fraction of deionized water and sodium hydroxide was 1: 1.
The acid digestion, i.e. washing with boiling acid solution: the volume fraction of the deionized water and the concentrated hydrochloric acid is 1: 1.
The effect of adding each beneficial element with the content is as follows:
1. the addition of rhodium, palladium and iridium plays roles in solid solution strengthening and resistance ratio and resistance temperature coefficient adjustment:
rhodium: the resistance temperature coefficient is adjusted while the solid solution strengthening effect is achieved, the volatilization characteristic of the high-temperature oxide is close to that of Pt, and the long-term stability of the resistance temperature coefficient is ensured;
iridium: the alloy has high solid solution strengthening effect in platinum, can obviously improve the hardness and improve the high-temperature durable strength of the alloy;
palladium: the additive is added together with rhodium and iridium to enhance the solid solution strengthening effect and improve the temperature coefficient of resistance;
2. adding rare earth elements: two or more than two combinations of rare earth elements Hf, La, Ce, Gd and Yb are added in the smelting process, so that impurities can be removed, crystal grains can be obviously refined, the recrystallization temperature is increased, the toughness is improved, the processing performance is improved, the dispersion strengthening effect can be realized by oxidation in the processing, in addition, the resistance temperature coefficient can be adjusted, the electrical property, the structure, the mechanical property and the like of the platinum wire can be effectively adjusted and controlled, and the comprehensive performance of the alloy is improved.
By reasonably matching the added beneficial elements, the temperature coefficient of resistance (alpha) of the material is ensured to be 0.003851 +/-0.000003 DEG C-1And the micro-processing is carried out, so that the use of key materials of the nuclear-grade platinum resistance thermometer is met.
By adopting the technical scheme, the beneficial elements are wrapped by the platinum material, so that volatilization, burning loss and oxidation of the beneficial elements are reduced in the smelting process; the intermediate solid solution alloy is prepared firstly, and then the final solid alloy is prepared, so that the precise regulation and control of beneficial elements are facilitated; argon is introduced in the smelting process, so that the phenomenon of air suction of the alloy in the smelting process can be effectively solved, and refining and tissue homogenization are facilitated.
The final solid alloy obtained in the step 1) in the preparation method is subjected to homogenization heat treatment for 0.5-1 hour at 800-1100 ℃ by adopting a hot forging technology, then is subjected to hot forging by adopting a circular die forging to obtain an alloy round bar with the size of phi 4 +/-1 mm, is subjected to heat treatment for 15-30 minutes at 500-800 ℃, and is subjected to surface rounding and smooth finishing after forging, so that the defects of loose structure, holes and the like on the surface layer of an ingot are removed, the surface quality is ensured, and the material micronization processing is facilitated.
Carrying out wire processing on the alloy round bar material, sequentially carrying out rough drawing with the deformation of less than or equal to 15%, medium drawing with the deformation of less than or equal to 10% and fine drawing with the deformation of less than or equal to 6% on the alloy round bar material obtained in the step 2) on a wire drawing machine, keeping the total deformation of less than or equal to 80% in each stage, carrying out heat treatment at the temperature of 400-700 ℃ for 10-30 min, drawing to obtain a finished product of fine platinum wires, and rewinding the cleaned wire material on a finished product take-up drum through a rewinding device to obtain a finished product wire material.
For the materials, reasonable heat treatment and deformation processing technologies are adopted, fibrous tissues can be effectively generated in the wire processing process, adverse factors of surface damage of the wire caused by too fast processing hardening and further influence on surface quality and yield are reduced, the processing performance is greatly improved, and the quality of the wire is improved. The tension device is adopted, so that the wire can be ensured to have little or no sliding in the deformation process, and the consistency and the high surface quality of the wire are improved.
Too high heat treatment temperature or too long heating time leads to coarse grains and inconsistent recrystallization in the heating process of the material, and internal vacancies and dislocations are generated, which are one of the key factors for reducing the temperature measurement stability and the temperature measurement precision. If the temperature is too low or the heating time is too short, the stress relief effect cannot be achieved, and the phenomena that the surface of the wire is easy to damage and the wire is broken in the drawing process can be caused seriously. Similarly, too large deformation tends to cause too rapid work hardening, and too small deformation does not maintain a good rigidity of the material, which is not favorable for microfabrication. As described above, the microalloyed material formed by the beneficial elements has a solid solution strengthening effect by itself, and is advantageous in improving the fine grain yield by an appropriate work hardening action.
In the rough drawing stage and the intermediate heat treatment, foreign matters such as ceramic, foreign metal impurities, microparticles, oil stains and the like attached to the surface are mainly removed, boiling alkali and acid solution are selected for cleaning in sequence, namely, alkali boiling is firstly carried out (the volume fraction of deionized water and sodium hydroxide is 1:1), and then acid boiling is carried out (the volume fraction of deionized water and concentrated hydrochloric acid is 1: 1).
In the middle drawing stage, surface micro-particle inclusion and oil stain are mainly removed, and a water-based emulsion lubricant is selected, so that the lubricating effect can be well played, and the drawing of the micro-wire is facilitated. And in the fine drawing stage, firstly, ultrasonic cleaning by using absolute ethyl alcohol as a medium is adopted to carry out online continuous cleaning on the drawn finished product fine platinum wire, and then ultrasonic cleaning by using deionized water as a medium is adopted to carry out online continuous cleaning on the drawn finished product fine platinum wire so as to remove foreign matters such as ceramic, foreign metal impurities, micro particles, oil stains and the like attached to the surface.
The superfine platinum wire for the nuclear grade platinum resistance thermometer obtained by the preparation method has a series of advantages of high uniformity, high precision, high stability, long service life, irradiation resistance and the like, and is wide in application field. The problems of matching and consistency of the electrical property and the mechanical property of the material are solved, and the use of the key material of the nuclear-grade platinum resistance thermometer is met. The performance detection proves that the smallest wire diameter of the superfine platinum wire for the nuclear grade platinum resistance thermometer can reach 10 mu m, the precision is +/-0.2 mu m, and the resistance temperature coefficient (alpha) meets 0.003851 +/-0.000003 DEG C-1The standard requirement of the nuclear grade platinum resistance. The platinum resistance temperature sensing element made of the platinum wire has good stability, and the maximum temperature of long-term use can reach 800 ℃. The micro platinum wire can also be popularized and applied to advanced sensors in other high-technology fields with extremely high micronization degree and extremely high requirement on temperature measurement precision.
Detailed Description
The invention relates to a micro platinum wire for a nuclear grade platinum resistance thermometer, which is prepared by the preparation method and comprises the following components in percentage by weight: the beneficial elements are 0.02-0.08%, the content of harmful elements is less than 30ppm, and the balance is Pt. The beneficial elements are the combination of two or more of Rh, Ir, Pd and rare earth elements, and the rare earth elements are the combination of two or more of Hf, La, Ce, Gd and Yb. The harmful elements are: co, Cu, B, Si, Cd.
The technical solution of the present invention is described in the form of steps in conjunction with the following examples 1-3.
The platinum raw material is prepared by the following method:
(ii) hydrolysis
Weighing commercially available spongy platinum with a purity of 99.95%, dissolving with dilute aqua regia under heating, concentrating, removing nitric acid with concentrated hydrochloric acid, adding sodium chloride solid, and evaporating to dryness. Dissolving in water to obtain platinum solution, boiling, adjusting pH to 8-10 with 10% chlor-alkali (same as chlorine-alkali concentration), standing at room temperature for 10-20 hr, filtering to obtain filtrate 1, and recovering precipitate.
Concentrating the filtrate to 300-500 ml, adding 100-200 ml concentrated hydrochloric acid, evaporating to dryness, dissolving in deionized water, boiling, adjusting pH to 8-10 with chlor-alkali, maintaining at constant temperature for 30-60min, standing at normal temperature for 3-4h, filtering to obtain filtrate 2, precipitating, and recovering.
Adding a cerous chloride solution with the mass concentration of 1-5% into the filtrate 2, boiling, adjusting the pH value of the solution to 8-10, keeping the temperature for 30min, standing at normal temperature for 10-20 h, filtering to obtain a filtrate 3, and precipitating and recovering; and 3-5 times of hydrolysis is carried out according to the steps to obtain filtrate after multiple times of hydrolysis.
Through the process steps, harmful impurities are effectively removed, and the purity of the platinum powder is obviously improved.
Reduction of hydrazine hydrate
Heating the filtrate obtained after the multiple hydrolysis to boil, slowly adding hydrazine hydrate in the slightly cooled filtrate until the supernatant is clear, and boiling until no alkali vacuole exists.
③ filtering and calcining
Filtering to obtain platinum powder, washing with boiling water for multiple times until the pH value is neutral, calcining with a muffle furnace, keeping the temperature at 800 ℃ for 30min, cooling to room temperature, taking out high-purity platinum powder with the Pt content of 99.998%, and obtaining the platinum raw material.
Material purity: the beneficial elements are more than or equal to 99.95 percent (sold in the market).
The weight percentage of each component in the embodiment 1 is as follows: rh: 0.008%, Ir: 0.006%, Hf: 0.001%, La: 0.001%, Ce: 0.001%, the contents of Co, Cu, B, Si and Cd are all less than 30ppm, and the balance is Pt (platinum raw material, the same below).
The weight percentage of each component in the embodiment 2 is as follows: rh: 0.02%, Pd: 0.005%, Gd: 0.0008%, Yb: 0.0008 percent, less than 30ppm of Co, Cu, B, Si and Cd and the balance of Pt.
Example 3 the components are in weight percent: pd: 0.005%, Ir: 0.008%, La: 0.002%, Ce: 0.001%, Gd: 0.001%, Yb: 0.001 percent, the contents of Co, Cu, B, Si and Cd are all less than 30ppm, and the balance is Pt.
Taking the components described in the embodiments 1-3, respectively preparing the fine platinum wire material for the nuclear grade platinum resistance thermometer according to the steps of the preparation method of the invention:
1) taking the components of the fine platinum wire for the nuclear-grade platinum resistance thermometer according to the proportion of the embodiments 1-3, wherein the platinum is prepared by wrapping beneficial elements accounting for 0.5 percent of the total weight by 70-80 percent of the total weight, and in the actual operation process, the components are wrapped by layers: firstly, placing platinum powder on the bottom layer, placing beneficial element in the middle, adding platinum powder on the beneficial element, completely wrapping the beneficial element with platinum powder, compacting, placing in a vacuum induction smelting furnace to make smelting, and making vacuum degree be 1X 10-2～1×10- 3Pa, filling argon for protection, preserving heat for 5-10min after the materials are completely melted, and casting the materials into a water-cooled copper mold in a rapid bottom leakage manner to obtain an intermediate solid solution alloy;
placing the intermediate solid solution alloy and the rest platinum in a melting crucible using high-purity zirconium oxide with the purity of more than 99.9%, and vacuum induction melting in a degree of vacuum of 1 × 10-2～1×10-3Pa, introducing argon for protection, after the materials are completely melted, keeping the temperature for 5-10min, and performing quick bottom leakage casting to obtain the alloy with the resistance temperature coefficient (alpha) of 0.003851 +/-0.000003 DEG C-1The final solid alloy of (a);
2) hot forging: carrying out homogenizing heat treatment on the final solid alloy obtained in the step 1) at 800-1100 ℃ for 0.5-1 h, carrying out hot die forging and pressing on the final solid alloy by adopting round die forging to obtain a round bar material with phi of 4 +/-1 mm, and carrying out heat treatment on the round bar material at 500-800 ℃ for 15-30 min;
3) wire processing: carrying out rough drawing with the deformation amount of less than or equal to 15%, medium drawing with the deformation amount of less than or equal to 10% and fine drawing with the deformation amount of less than or equal to 6% on the round bar obtained in the step 2) on a wire drawing machine in sequence, keeping the total deformation amount of the bar of less than or equal to 80%, carrying out intermediate heat treatment at the temperature of 400-700 ℃, carrying out the intermediate heat treatment for 10-30 min, drawing to obtain a finished product of fine platinum wire, carrying out alkaline boiling treatment by using deionized water and an alkaline solution with the volume fraction of 1:1 of sodium hydroxide after the rough drawing stage, and then carrying out acid boiling treatment by using deionized water and an acid solution with the volume fraction of 1:1 of concentrated hydrochloric; after the middle pulling stage, firstly, carrying out alkali boiling treatment by using deionized water and an alkali solution with the volume fraction of sodium hydroxide being 1:1, and then carrying out acid boiling treatment by using deionized water and an acid solution with the volume fraction of concentrated hydrochloric acid being 1: 1; after the fine drawing stage, firstly, the finished fine platinum wire is continuously cleaned on line by adopting ultrasonic cleaning with absolute ethyl alcohol as a medium, then, the finished fine platinum wire is continuously cleaned on line by adopting ultrasonic cleaning with deionized water as a medium to remove foreign matters such as ceramic, foreign metal impurities, micro-particles and oil stains attached to the surface, and the cleaned wire is rewound on a finished product take-up drum by a rewinding device to obtain the finished wire.
Finally, the performance of the obtained micro platinum wire for the nuclear grade platinum resistance thermometer is detected to obtain the following results:
the smallest diameter of the superfine platinum wire for the nuclear grade platinum resistance thermometer obtained by the preparation method is 10 mu m, the precision is +/-0.2 mu m, and the resistance temperature coefficient (alpha) meets 0.003851 +/-0.000003 DEG C-1The standard requirement of the nuclear grade platinum resistor is that after the standard requirement is manufactured into a wire-wound platinum resistor temperature sensing element, the resistance change values R of the wire-wound platinum resistor temperature sensing element before and after the temperature is respectively preserved for 250 hours at 850 ℃ and 0 ℃ are tested0And converting the resistance change value into a temperature value, so that the temperature change value of the wire-wound platinum resistance temperature sensing element is not more than 0.02 ℃, and the maximum service temperature can reach 900 ℃.
Claims (10)
1. The fine platinum wire for the nuclear grade platinum resistance thermometer is characterized by comprising the following components in percentage by weight: the beneficial elements are 0.02-0.08%, the content of harmful elements is less than 30ppm, and the balance is Pt.
2. The material of claim 1, wherein: the beneficial elements are the combination of at least two of Rh, Ir, Pd and rare earth elements, and the rare earth elements are the combination of at least two of Hf, La, Ce, Gd and Yb.
3. The material according to claim 1, wherein the weight percentage of each component is as follows: rh: 0.005-0.02%, Ir: 0.001-0.02%, rare earth elements: 0.001-0.01%, and the balance of Pt, wherein the content of harmful elements is less than 30 ppm.
4. The material according to claim 1, wherein the weight percentage of each component is as follows: rh: 0.008-0.015%, Pd: 0.005-0.008%, rare earth elements: 0.001-0.01%, and the balance of Pt, wherein the content of harmful elements is less than 30 ppm.
5. The material according to claim 1, wherein the weight percentage of each component is as follows: pd: 0.005-0.008%, Ir: 0.005-0.01%, rare earth elements: 0.003-0.01 percent, and the balance of Pt, wherein the content of harmful elements is less than 30 ppm.
6. A material according to any one of claims 1 to 5, wherein the detrimental elements are: co, Cu, B, Si, Cd.
7. The preparation method of the fine platinum wire for the nuclear grade platinum resistance thermometer is characterized by comprising the following steps:
1) smelting:
vacuum induction melting is adopted, and the vacuum degree is 1 multiplied by 10-2～1×10-3Pa, argon protection;
taking the components of the fine platinum wire for the nuclear-grade platinum resistance thermometer according to the proportion of claim 1, wherein the platinum is used for coating beneficial elements by 70-80% of the total amount of the platinum, and after the materials are completely melted, the temperature is kept for 5-10min, and the intermediate solid solution alloy is obtained by bottom leakage casting; placing the intermediate solid solution alloy and the rest platinum in a crucible, completely melting, keeping the temperature for 5-10min, and casting at the bottom to obtain the final solid alloy;
2) hot forging:
carrying out homogenization heat treatment on the final solid alloy obtained in the step 1) at 800-1100 ℃ for 0.5-1 hour, then carrying out hot die forging and pressing to obtain a bar, and carrying out heat treatment on the obtained bar at 500-800 ℃ for 15-30 minutes;
3) wire processing:
and (3) carrying out rough drawing with the deformation not more than 15%, medium drawing with the deformation not more than 10% and fine drawing with the deformation not more than 6% on the bar subjected to heat treatment obtained in the step 2) on a wire drawing machine in sequence, wherein the total deformation of drawing is not more than 80%, carrying out heat treatment, namely carrying out heat treatment at the temperature of 400-700 ℃ for 10-30 min, drawing into a finished product of fine platinum wire, and cleaning to obtain the finished product of wire.
8. The method of claim 7, wherein: the method for coating beneficial elements by using platinum accounting for 70-80% of the total amount in the step 1) comprises the following steps of coating in layers: the bottom layer and the top layer are made of platinum powder, the middle layer is arranged between the bottom layer and the top layer and is beneficial elements, and the beneficial elements are completely wrapped and compacted by the platinum powder.
9. The method of claim 7, wherein: in the step 2), the bar is a round bar with the size of phi 4 +/-1 mm.
10. The method of claim 7, wherein: performing alkaline cooking treatment after the rough drawing stage in the step 3), and performing acid cooking treatment; in the middle pulling stage, alkali cooking treatment is firstly carried out, and then acid cooking treatment is carried out; in the fine drawing stage, firstly, ultrasonic cleaning with absolute ethyl alcohol as a medium is adopted to carry out online continuous cleaning on the drawn finished fine platinum wire, and then ultrasonic cleaning with deionized water as a medium is adopted to carry out online continuous cleaning on the drawn finished fine platinum wire.
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| CN202010589765.9A CN111910099B (en) | 2020-06-24 | 2020-06-24 | Fine platinum wire for nuclear grade platinum resistance thermometer and preparation method thereof |
| PCT/CN2021/100695 WO2021259139A1 (en) | 2020-06-24 | 2021-06-17 | Micro-fine platinum wire for nuclear-grade platinum resistance thermometer, and preparation method |
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| WO2021259139A1 (en) * | 2020-06-24 | 2021-12-30 | 重庆材料研究院有限公司 | Micro-fine platinum wire for nuclear-grade platinum resistance thermometer, and preparation method |
| 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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| CN115927904A (en) * | 2022-12-14 | 2023-04-07 | 英特派铂业股份有限公司 | Trace substance doped high-purity platinum material and preparation method thereof |
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| CN104439274A (en) * | 2014-11-13 | 2015-03-25 | 重庆材料研究院有限公司 | Method for preparing platinum material for dispersion strengthened thermoelectric couple negative electrode fine wire |
| JP2020193370A (en) * | 2019-05-28 | 2020-12-03 | 石福金属興業株式会社 | High-strength Pt alloy |
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| 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 |
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| JPS6439335A (en) * | 1987-08-05 | 1989-02-09 | Tanaka Precious Metal Ind | Material for pure platinum extra fine wire |
| CN101235446A (en) * | 2008-03-06 | 2008-08-06 | 沐嘉龙 | Dispersion strengthening platinum-base composite material |
| CN101561322A (en) * | 2009-05-18 | 2009-10-21 | 无锡英特派金属制品有限公司 | Dispersion strengthening platinum/rhodium13-platinum thermocouple wires and production method thereof |
| CN104439274A (en) * | 2014-11-13 | 2015-03-25 | 重庆材料研究院有限公司 | Method for preparing platinum material for dispersion strengthened thermoelectric couple negative electrode fine wire |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2021259139A1 (en) * | 2020-06-24 | 2021-12-30 | 重庆材料研究院有限公司 | Micro-fine platinum wire for nuclear-grade platinum resistance thermometer, and preparation method |
| 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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| WO2021259139A1 (en) | 2021-12-30 |
| CN111910099B (en) | 2022-03-08 |
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