CN111922114A - High-purity fine platinum wire and preparation method thereof - Google Patents
High-purity fine platinum wire and preparation method thereof Download PDFInfo
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- CN111922114A CN111922114A CN202010589771.4A CN202010589771A CN111922114A CN 111922114 A CN111922114 A CN 111922114A CN 202010589771 A CN202010589771 A CN 202010589771A CN 111922114 A CN111922114 A CN 111922114A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C5/00—Alloys based on noble metals
- C22C5/04—Alloys based on a platinum group metal
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21C—MANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
- B21C37/00—Manufacture of metal sheets, bars, wire, tubes or like semi-manufactured products, not otherwise provided for; Manufacture of tubes of special shape
- 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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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/03—Making non-ferrous alloys by melting using master alloys
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- 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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- G—PHYSICS
- 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 preparation method of a high-purity fine platinum wire, which is used for obtaining a fine platinum wire material with high uniformity, high precision and high stability by casting, hot forging and wire processing, and solves the problems of matching and consistency of electrical property and mechanical property of the material. The applicant verifies that the minimum wire diameter of the high-purity fine platinum wire can reach 10 mu m, the precision is +/-0.2 mu m, and the standard requirement that the resistance ratio (W100) is more than or equal to 1.39254 is met, so that the high-purity fine platinum wire meets the requirements of standard-grade and high-sensitivity standard platinum resistance thermometers, industrial platinum resistance temperature sensors and other advanced sensors such as other instruments and meters. The material obtained by the method has the advantages of high uniformity, high precision, high stability, long service life and the like, and is wide in application field.
Description
Technical Field
The invention belongs to the field of noble metal materials, and particularly relates to a high-purity fine platinum wire and a preparation method thereof.
Background
The platinum wire has the characteristics of high melting point, high sensitivity, quick response time, good stability and the like, and has excellent physical and chemical stability, so that the platinum wire is widely applied to a platinum resistance thermometer for accurate temperature measurement.
For the application of standard platinum resistance thermometer, industrial platinum resistance and other temperature sensors and other advanced sensors of instruments and meters with standard grade and high sensitivity, a large amount of high-purity platinum wires are required to be used, and the platinum wires need to meet the resistance ratio W100Not less than 1.39254. The purity, trace elements, mechanical property, structure and internal defects of the platinum wire, uniformity and uniformity of the wire and the like directly influence the measurement accuracy, stability, service life and other properties of the sensor.
In the existing preparation process of the platinum filament, the platinum raw material is commercially available spongy platinum, the purity is up to 99.99%, the platinum ingot is obtained by induction melting, and the platinum filament is obtained by forging, rolling, drawing and other processing, and has the advantages of low purity, poor mechanical property, high micronization processing difficulty and resistance ratio W100About 1.3922, the diameter of the obtained industrial grade platinum wire is more than 25 μm, a small amount of experimental grade samples can be made to be 20 μm, the precision is +/-1 μm, the precision of the platinum wire is not easy to control, the consistency of products is poor, and the like, so that the temperature coefficient of resistance of the platinum wire is deviated, and the performances of temperature measurement precision, stability, service life and the like of the platinum wire are greatly reduced.
Therefore, the fine platinum wire prepared by the prior art is greatly limited in engineering application in the high-tech fields of instruments, energy, aviation, aerospace and the like.
Technical content
The invention aims to provide a high-purity fine platinum wire and a preparation method thereof, and the platinum wire prepared by the methodThe diameter of the platinum wire can reach 10 μm, the precision is +/-0.2 μm, and the resistance ratio W is100Not less than 1.39254, and can meet the performance requirements of standard platinum resistance thermometer, industrial platinum resistance temperature sensor, and other instruments.
The technical scheme of the invention is as follows:
the preparation method of the high-purity fine platinum wire comprises the following steps:
1) casting
Placing the platinum material in a vacuum induction melting furnace, protecting with argon, preserving heat for 5-10min after completely melting, and performing rapid bottom leakage casting to obtain a platinum ingot;
2) hot forging
Carrying out homogenization heat treatment on the platinum ingot obtained in the step 1) at 800-1100 ℃ for 0.5-1 hour; hot forging at 800-1100 ℃ into a round bar, and finishing the surface of the round bar;
3) wire processing
Carrying out rough drawing, medium drawing, fine drawing and superfine drawing on the round bar obtained in the step 2) on a wire drawing machine, wherein the total deformation amount of each stage is less than or equal to 90%;
wire processing: and (3) 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 obtained in the step 2) on a wire drawing machine in sequence, 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, and drawing into the fine platinum wire.
The content of the platinum raw material selected in the prepared high-purity fine platinum wire is more than or equal to 99.999 percent.
Step 1) the vacuum degree of the vacuum is 1 x 10-2～1×10-3Pa。
The round bar obtained in the step 2) needs to be subjected to heat treatment, and the heat treatment method is that the round bar is subjected to heat preservation for 15-30 minutes at 500-800 ℃.
And 2) the diameter of the round rod is 4 +/-1 mm, and the surface of the round rod is trimmed and smoothed by preferably adopting turning.
Step 3), adding front and rear tension devices for middle drawing and micro drawing, namely adding tension devices at two ends (paying off and taking up) of a wire drawing machine to ensure stability and no sliding in the wire drawing process and ensure the size precision and the surface quality of wires;
step 3) the heat treatment system of the rough drawing and the medium drawing is as follows: and keeping the temperature for 10-30 min at 400-700 ℃.
And 3) cleaning after rough drawing, namely performing alkali cooking and then performing acid cooking, wherein the alkali cooking is performed by using a solution with the volume fraction of deionized water and sodium hydroxide being 1:1, and the acid cooking is performed by using a solution with the volume fraction of deionized water and concentrated hydrochloric acid being 1: 1.
And 3) cleaning after the intermediate drawing, namely cleaning by adopting a wire drawing water-based emulsion lubricant.
And 3) cleaning the fine wire by adopting ultrasonic online continuous cleaning, wherein preferably, the medium for continuous cleaning is deionized water and absolute ethyl alcohol.
When the method is used for smelting, a high-cleanness induction smelting bottom-pouring type casting process is adopted, and a smelting crucible is made of high-purity zirconia or magnesia ceramic which is subjected to high-temperature re-sintering, so that the pollution caused by foreign impurities is avoided, and the refining effect is achieved. The re-sintering function is to effectively remove impurities in the crucible at high temperature.
The hot forging of the invention can improve the crystal structure, lead the crystal grains to be crushed and rearranged, improve the density of the matrix, round and smooth the surface of the forged round bar, remove the defects of loose surface structure, holes and the like caused by smelting of the cast ingot, ensure the surface quality and be beneficial to the subsequent fine wire drawing.
Reasonable heat treatment and deformation processing technologies are adopted in the wire processing process, 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 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.
Cleaning and lubricating: in the rough drawing stage, respectively adopting boiling alkali and boiling acid solution to clean so as to remove foreign matters such as ceramic, foreign metal impurities, micro-particles, oil stains and the like attached to the surface; in the middle drawing stage, a water-based emulsion lubricant is selected to remove surface microparticle impurities and oil stains, has a good lubricating effect and is beneficial to drawing of micro-wires; and in the fine drawing stage, deionized water, absolute ethyl alcohol or acetone is used for ultrasonic continuous cleaning, and the surface of the micro-wire is cleaned by decontamination and impurity removal so as to ensure the clean surface, excellent surface quality and wire consistency of the wire.
The superfine platinum wire material with high uniformity, high precision and high stability, which is obtained by the method of the invention, solves the problems of matching and consistency of the electrical property and the mechanical property of the material. The applicant verifies that the content of platinum in the high-purity fine platinum wire is more than 99.995 percent, the minimum wire diameter can reach 10 mu m, the precision is +/-0.2 mu m, and the resistance ratio W is100The standard requirement of not less than 1.39254 meets the requirements of standard grade and high-sensitivity standard platinum resistance thermometers, industrial platinum resistance temperature sensors and other instruments and meters. The material obtained by the method has the advantages of high uniformity, high precision, high stability, long service life, irradiation resistance and the like, and is widely applied to the fields of instruments, aviation, aerospace, energy sources and the like.
Detailed Description
The technical solution of the present invention is described below in the form of steps with reference to examples.
The platinum raw material is prepared by the following method:
1. 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, the contents of elements such as Pd, Rh, Ir, Au, Fe, Ni, Cu, Mg, Al, Pb, Si, Co, Ag, Cd and the like in the platinum powder can be greatly reduced, and the purity of the platinum powder is improved.
2. 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, and taking out the high-purity platinum powder to obtain the platinum raw material.
Other reagents used in this example were commercially available analytical grade reagents.
Example (b):
vacuum smelting: smelting platinum raw material in a vacuum induction smelting furnace with the vacuum degree of 1 multiplied by 10-2～1×10- 3And Pa, introducing argon for protection, preserving the heat for more than 3min after the materials are completely melted, and casting the materials into a water-cooled copper mould in a rapid bottom leakage manner to obtain a platinum ingot.
Hot forging: carrying out homogenization heat treatment at 800-1100 ℃ for 0.5-1 hour; and (3) carrying out hot forging at 800-1100 ℃, wherein the round die forging is adopted for forging, and the round bar with the size phi of 4 +/-1 mm is forged. Heat treatment is carried out for 15-30 minutes at 500-800 ℃.
Wire processing: the alloy round bar is roughly drawn, drawn in and drawn minutely on a wire drawing machine, and tension devices before and after the addition of the drawing in the drawing process and the drawing minutely, namely tension devices are added at two ends (paying off and taking up) of the drawn wire, so that the stability and the non-slip performance of the drawn wire are ensured, and the size precision and the surface quality of the wire are ensured. The deformation of the rough drawing pass is less than or equal to 18 percent; the medium tensile deformation is less than or equal to 15 percent, and the fine tensile deformation is less than or equal to 8 percent; the superfine drawing deformation is less than or equal to 4 percent. The total deformation of wire drawing in each stage is less than or equal to 90%, when the stage deformation reaches about 80%, intermediate heat treatment is carried out, the heat treatment system is 400-700 ℃, and the time is 10-30 min, so that the internal stress of the wire is eliminated, the crystal grains in the material are more uniform, and the subsequent drawing is facilitated. Can be drawn to fine platinum wire with wire diameter of 10 μm.
Cleaning and lubricating: in the rough drawing stage and the intermediate heat treatment, foreign matters such as ceramic, foreign metal impurities, micro-particles, oil stains and the like attached to the surface are mainly removed, boiling alkali and acid solution are selected for cleaning, 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. The fine drawing stage is a key stage for ensuring the cleanness of the surface of the wire, excellent surface quality and consistency of the wire, and ultrasonic cleaning is adopted for online continuous cleaning, and deionized water and absolute ethyl alcohol are used as media for performing decontamination and impurity removal cleaning on the surface of the micro-wire.
Fine platinum wires of different wire diameters (examples 1, 2, 3) were obtained by the above method and subjected to relevant performance tests as shown in the following table:
| performance parameter | Silk diameter (mum) | Tolerance (mum) | Resistance ratio (W)100) | Breaking force (cN) | Elongation (%) |
| Example 1 | 10 | ≤0.2 | ≥1.39254 | ≥4 | ≥1.5 |
| Example 2 | 15 | ≤0.12 | ≥1.39254 | ≥8 | ≥3.0 |
| Example 3 | 20 | ≤0.15 | ≥1.39254 | ≥10 | ≥5.0 |
The method solves the matching problem of high obdurability, electrical property and processability of the material, the obtained material has a series of advantages of high purity, high uniformity, high precision, high stability, excellent mechanical property and the like, and the material is used as an advanced sensor key material, is applied to the fields of instruments, measurement and control, aviation, aerospace and the like, and has a wide application field.
Claims (10)
1. The preparation method of the high-purity fine platinum wire is characterized by comprising the following steps of:
1) casting
Placing the platinum material in a vacuum induction melting furnace, protecting with argon, preserving heat for 5-10min after completely melting, and performing rapid bottom leakage casting to obtain a platinum ingot;
2) hot forging
Carrying out homogenization heat treatment on the platinum ingot obtained in the step 1) at 800-1100 ℃ for 0.5-1 hour; hot forging at 800-1100 ℃ into a round bar, and finishing the surface of the round bar;
3) wire processing
Carrying out rough drawing, medium drawing, fine drawing and superfine drawing on the round bar obtained in the step 2) on a wire drawing machine, wherein the total deformation amount of each stage is less than or equal to 90%;
wire processing: and (3) 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 obtained in the step 2) on a wire drawing machine in sequence, carrying out heat treatment at the temperature of 400-700 ℃ for 10-30 min at the total deformation of less than or equal to 80% in each stage, and drawing into the fine platinum wire.
2. The method of claim 1, wherein: the platinum content in the high-purity fine platinum wire is more than 99.995 percent.
3. The method of claim 1, wherein: step 1) the vacuum degree of the vacuum is 1 x 10-2～1×10-3Pa。
4. The method of claim 1, wherein: the round bar obtained in the step 2) needs to be subjected to heat treatment, and the heat treatment method is that the round bar is subjected to heat preservation for 15-30 minutes at 500-800 ℃.
5. The method of claim 1, wherein: and 2) the diameter of the round rod is 4 +/-1 mm, and the surface of the round rod is trimmed and smoothed by preferably adopting turning.
6. The method of claim 1, wherein: and 3) controlling the stability of the drawn wire by using a tension device for middle drawing and micro drawing.
7. The method of claim 1, wherein: step 3) the heat treatment system of the rough drawing and the medium drawing is as follows: and keeping the temperature for 10-30 min at 400-700 ℃.
8. The method of claim 1, wherein: and 3) cleaning after rough drawing, namely performing alkali cooking and then performing acid cooking, wherein the alkali cooking is performed by using a solution with the volume fraction of deionized water and sodium hydroxide being 1:1, and the acid cooking is performed by using a solution with the volume fraction of deionized water and concentrated hydrochloric acid being 1: 1.
9. The method of claim 1, wherein: and 3) cleaning after the intermediate drawing, namely cleaning by adopting a wire drawing water-based emulsion lubricant.
10. The method of claim 1, wherein: and 3) cleaning the fine wire by adopting ultrasonic online continuous cleaning, wherein preferably, the medium for continuous cleaning is deionized water and absolute ethyl alcohol.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010589771.4A CN111922114B (en) | 2020-06-24 | 2020-06-24 | High-purity fine platinum wire and preparation method thereof |
| PCT/CN2021/100628 WO2021259135A1 (en) | 2020-06-24 | 2021-06-17 | High-purity fine platinum wire and preparation method |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113578996A (en) * | 2021-07-08 | 2021-11-02 | 英特派铂业股份有限公司 | Preparation method of platinum heating wire |
| 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 |
| CN114592159A (en) * | 2022-03-22 | 2022-06-07 | 重庆材料研究院有限公司 | Palladium alloy reinforced composite bonding wire and preparation method thereof |
| CN116618464A (en) * | 2023-03-13 | 2023-08-22 | 河北冀伽康新材料科技有限公司 | Production process of quantum platinum cobalt alloy fiber yarn |
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| CN114592159A (en) * | 2022-03-22 | 2022-06-07 | 重庆材料研究院有限公司 | Palladium alloy reinforced composite bonding wire and preparation method thereof |
| CN116618464A (en) * | 2023-03-13 | 2023-08-22 | 河北冀伽康新材料科技有限公司 | Production process of quantum platinum cobalt alloy fiber yarn |
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| Publication number | Publication date |
|---|---|
| CN111922114B (en) | 2022-08-02 |
| WO2021259135A1 (en) | 2021-12-30 |
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