A method for preparing a fast-response sensitive element emitter body fiber

Abstract

The present application relates to a kind of preparation methods for fast response sensitive element emitter erbium wire, the method is prepared by using erbium powder pretreatment, cold isostatic pressing, microwave vacuum sintering, vacuum electron beam melting, hot forging cold drawing, wire post-processing etc., emitter erbium wire purity ≥99.95%, B, Cd, Si, Cr, Cu, Co impurity element content≤30ppm, O, N, H content≤100ppm, erbium wire diameter is 0.50~1.00mm, wire diameter precision reaches ±0.005mm, surface roughness Ra≤1.5 μm, tensile strength≥620MPa, elongation≥7%, meter resistance uniformity±1.5%, with high purity, high precision, the stability of mechanical properties and surface quality is good, can satisfy the performance requirements of fast response sensitive element emitter erbium wire.

Description

TECHNICAL FIELD

[0001] The present application belongs to the field of material processing, and particularly relates to a preparation method of a emitter erbium wire for a fast response sensitive element. BACKGROUND

[0002] Metal erbium is a strategic functional material of rare earth, and is widely used in nuclear industry, electronic information, medical devices, laser and many other fields. In the nuclear industry, high-purity erbium has high thermal stability and helium release threshold, and has low neutron irradiation activity and low thermal expansion coefficient, and is one of the ideal candidate materials for the emitter of the fast response neutron sensitive element. Since metal erbium belongs to the close-packed hexagonal structure, there is a plastic-brittle transition phenomenon in the deformation process, and the high-temperature oxidation and gas absorption show brittleness, which makes the high-temperature deformation processing of erbium extremely difficult, and the hardness increases sharply during cold processing, which easily causes the surface quality to be damaged and broken, and it is difficult to ensure the high strength and high toughness of the processed erbium finished material, and the performance requirements of the emitter cannot be met.

[0003] The emitter erbium wire is usually prepared for the emitter material of the fast response sensitive element, and the purity, control of trace impurity elements, consistency of wire diameter and stability of surface quality of the emitter erbium wire are directly related to the sensitivity, measurement accuracy and service life of the sensitive element, so the preparation and processing performance of the emitter erbium wire are of great significance to the preparation of the fast response sensitive element for nuclear industry. However, the preparation research of high-purity metal erbium carried out at home and abroad focuses on the purification of metal erbium and the preparation of erbium target material, and there are few reports on the research of the emitter erbium wire. SUMMARY

[0004] The purpose of the present application is to provide a preparation method of an emitter erbium wire for a fast response sensitive element, and the emitter erbium wire prepared by the method has high purity, less impurity elements, high wire diameter precision, good mechanical properties, and high surface quality stability, and can meet the performance requirements of the emitter material of the fast response sensitive element for nuclear industry.

[0005] The flow of the preparation method of the emitter erbium wire for a fast response sensitive element is: erbium powder pretreatment, cold isostatic pressing, microwave vacuum sintering, vacuum electron beam melting, hot forging, drawing and surface post-treatment, and the specific steps of the method are as follows:

[0006] 1) erbium powder pretreatment

[0007] The erbium powder is added into a hydrochloric acid solution, stirred uniformly to a slurry, ultrasonically cleaned for 15-30 min, then deionized water is added and repeatedly stirred and rinsed to neutral, and dried under vacuum to obtain the pretreated erbium powder;

[0008] Step 1) By using the vibration of ultrasonic waves, strong liquid flow force is generated to achieve good cleaning effect. After cleaning treatment, deionized water is added for repeated stirring and rinsing, and the addition of deionized water is stopped when the PH test paper is tested to be neutral.

[0009] Through pretreatment, the dirt and impurities on the surface of the erbium powder can be effectively cleaned, thereby improving the quality and forming performance of the erbium powder.

[0010] 2) Cold isostatic pressing

[0011] The pre-processed erbium powder is pressed into an erbium rod by cold isostatic pressing. The forming pressure of the erbium rod is uniform when the erbium powder is pressed by cold isostatic pressing, which can improve the forming ability of the erbium rod.

[0012] 3) Microwave vacuum sintering

[0013] The erbium rod is placed in a microwave vacuum heating furnace for sintering, the vacuum degree is ≥10 -2 Pa, sintering is carried out by using two-step gradient heat preservation method, and the furnace is cooled down to obtain a sintered erbium rod; the two-step gradient microwave sintering can reduce the sintering activation energy, speed up the sintering process, shorten the sintering time, inhibit the grain growth, and obtain a sintered erbium rod with uniform structure.

[0014] 4) Vacuum electron beam melting

[0015] Electron beam melting: the sintered erbium rod is melted under vacuum condition, the sintered erbium rod is melted in the electron beam bombardment area, and the molten erbium metal liquid is drawn into an erbium ingot by spiral downward pulling, and the melting is completed; the surface of the erbium ingot is turned; the electron beam melting and turning are repeated once again to obtain a high-purity erbium ingot;

[0016] Step 4) Two times of vacuum electron beam melting can greatly reduce the content of impurity elements in erbium, so that the content of B, Cd, Si, Cr, Cu and Co is ≤30ppm, the content of O, N and H is ≤100ppm, the purity of the erbium ingot reaches more than 99.99%, and the purity of the erbium ingot is improved.

[0017] 5) Hot forging

[0018] A layer of high-temperature resistant and oxidation resistant silicone lubricating paint is coated on the surface of the erbium ingot to avoid oxidation and air absorption of the erbium ingot during heating; drying is performed to ensure that the paint effectively covers the surface of the erbium ingot. Then, the erbium ingot is subjected to homogenization annealing treatment and is forged into an erbium metal rod; the erbium rod is subjected to hot rotary forging by a six-jaw die rotary forging machine to obtain an erbium metal rod;

[0019] Step 5) By coating and hot forging, the erbium rod is prevented from being polluted by oxidation and air absorption, and the erbium rod is deformed by six-jaw die rotary forging, which refines the grain and improves the uniformity of the grain structure, so that the erbium rod with an average grain size of 5-10μm is obtained.

[0020] 6) Drawing

[0021] The erbium metal rod is subjected to low-temperature oxidation surface pretreatment at a temperature of 280-350 ℃ and a treatment time of 20-30 min, and then is drawn into an erbium wire with a drawing pass deformation of ≤8%, a lubricant being chlorinated paraffin. When the cumulative deformation reaches 70-80%, the erbium wire is subjected to intermediate annealing treatment to eliminate deformation processing stress. Before annealing, the erbium wire surface is subjected to pickling to remove the chlorinated paraffin attached to the surface of the erbium wire, so as to obtain an erbium wire with a wire diameter of 0.50-1.00 mm (±0.005 mm).

[0022] Step 6) The low-temperature oxidation surface pretreatment makes the lubricant easily adhere to the surface of the erbium rod, improves the drawing lubrication, and reduces the generation of burrs and defects in the drawing process of the erbium wire.

[0023] 7) Surface post-treatment

[0024] The erbium wire is subjected to continuous electrolytic polishing and cleaning, electrolytic current being 3-6 A, alkali concentration being 5-15%wt of NaOH solution, and wire collecting speed being 3-5 m / min. The low-temperature oxidation surface pretreatment makes the lubricant easily adhere to the surface of the erbium rod, improves the drawing lubrication, and reduces the generation of burrs and defects in the drawing process of the erbium wire. After cleaning, the erbium wire is subjected to vacuum annealing.

[0025] Step 1) The erbium powder has Er≥99.95%, Fisher particle size of 5-45 μm, and normal distribution of particle size, and the weight ratio of the erbium powder to hydrochloric acid is 1:3.

[0026] The ultrasonic cleaning has an ultrasonic vibration frequency of 30-50 KHz.

[0027] Step 1) The vacuum drying has a temperature of 40-60 ℃, a drying time of 24-36 h, and a vacuum degree of ≥10 -2 Pa.

[0028] Step 2) The cold isostatic pressing has a pressing pressure of 160-200 MPa and a pressure holding time of 60-150 s.

[0029] Step 3) The two-step gradient heat preservation method is 300-350 ℃ for 60-90 min and 800-1000 ℃ for 60-90 min.

[0030] Step 4) The vacuum is ≥1.0×10 -4 Pa, and the emission current is 300-400 mA.

[0031] Step 5) The drying has a temperature of 160-200 ℃ and a heat preservation time of 18-24 h; and the homogenization heat treatment has a heating temperature of 700-800 ℃ and a heat preservation time of 1.5-2 h.

[0032] Step 5) the forging initial forging temperature is 700-800 DEG C, and the final forging temperature is 400-500 DEG C;

[0033] Step 5) the hot rotary section is deformed at a rate of 7-10%, the heating temperature is 700-800 DEG C, and the heating time is 10-20 min;

[0034] The erbium metal thin rod is phi 4mm-phi 6mm, and the average grain size is 5-10 mu m.

[0035] Step 6) the intermediate annealing treatment is under vacuum, the temperature is 520-820 DEG C, the holding time is 30-40 min, and the vacuum degree is greater than or equal to 10 -3 Pa.

[0036] Step 7) the vacuum annealing is at a temperature of 520-720 DEG C, a holding time of 30-40 min, and a vacuum degree of greater than or equal to 10 -3 Pa, and the furnace is cooled.

[0037] The method of the application, by adopting erbium powder pretreatment, cold isostatic pressing, microwave vacuum sintering, vacuum electron beam melting, hot forging and cold drawing, wire post-processing and other technologies, the emitter erbium wire prepared by the method has a purity of greater than or equal to 99.95%, the content of impurity elements B, Cd, Si, Cr, Cu and Co is less than or equal to 30 ppm, the content of O, N and H is less than or equal to 100 ppm, the erbium wire diameter is 0.50-1.00 mm, the wire diameter precision is plus or minus 0.005 mm, the surface roughness Ra is less than or equal to 1.5 mu m, the tensile strength is greater than or equal to 620 MPa, the elongation is greater than or equal to 7%, and the meter resistance uniformity is plus or minus 1.5%, and the method has high purity, high precision, good stability of mechanical properties and surface quality, and can meet the performance requirements of the emitter erbium wire of the fast-response sensitive element.

[0038] (1) The patent pretreats and cold isostatic presses the erbium powder, adopts a mixed solution of hydrochloric acid and deionized water to ultrasonically clean the erbium powder, can effectively clean the dirt and impurities on the surface of the erbium powder, and improves the quality and forming performance of the erbium powder.

[0039] (2) The combined process of microwave vacuum sintering and vacuum electron beam melting is adopted, two-step gradient microwave holding sintering can reduce the sintering activation energy, accelerate the sintering process, shorten the sintering time, inhibit the grain growth, and obtain a sintered erbium rod with uniform structure. The twice vacuum electron beam melting can greatly reduce the content of impurity elements in erbium, so that the content of B, Cd, Si, Cr, Cu and Co is less than or equal to 30 ppm, the content of O, N and H is less than or equal to 100 ppm, the purity of the erbium ingot is more than 99.99%, and the purity of the erbium ingot is improved.

[0040] (3) Through hot forging processing, the oxidation and air absorption of the rod is avoided, and the rod is deformed by six die rotary swaging, so that the crystal grains are refined and the uniformity of the crystal structure is improved. The average grain size of the rod is 5-10 μm.

[0041] (4) Through low-temperature oxidation surface pretreatment, the lubricant is easily attached to the surface of the rod, the drawing lubrication is improved, the burr and defects in the drawing process are reduced, the wire is post-treated, electrolytic polishing cleaning is adopted, the surface of the wire is smooth, the surface burr is reduced, the surface roughness is reduced, and the surface quality of the wire is greatly improved. BRIEF DESCRIPTION OF DRAWINGS

[0042] Figure 1 High-purity erbium wire prepared by the method. DETAILED DESCRIPTION

[0043] The reagents used in the application are all commercial products.

[0044] Example 1

[0045] 2000 g of erbium powder is weighed, the erbium powder is added into a 5wt% solution prepared from hydrochloric acid and deionized water and stirred into a slurry, and the weight ratio of the erbium powder to the hydrochloric acid is 1:3. Then it is put into an ultrasonic cleaning machine for cleaning for 15 min, and the vibration frequency is 30 KHz. After the cleaning treatment, deionized water is added for repeated stirring and rinsing, and the addition of deionized water is stopped when the PH test paper is tested to be neutral. After completion, it is put into a vacuum drying box for drying, the temperature is controlled at 60℃, the drying time is 24 h, the vacuum degree is 1.4×10 -2 Pa or above, until the erbium powder is completely dried. The erbium powder is loaded into a 304 stainless steel hole net fixed rubber mold sleeve, sealed and put into a cold isostatic pressing machine, the pressing pressure is 160 MPa, and the pressure holding time is 120 s. After cold isostatic pressing, the rubber mold sleeve is taken out, and the formed rod is φ15 mm in diameter. The pressed and formed rod is put into a microwave vacuum sintering furnace for sintering, the vacuum degree is 1.2×10 -2 Pa, a two-step gradient heat preservation sintering method is adopted, 300℃ is preserved for 90 min, 800℃ is preserved for 90 min, and the furnace is cooled down. A 250KW electron beam melting furnace is used, the microwave sintered rod is loaded and clamped in the furnace through the inlet valve, vacuum is extracted to 1.3×10 -4 Pa, the electron gun is moved to the place near the bottom of the rod to start melting, the emission current is gradually increased to 300 mA, the rod is melted in the electron beam bombardment area, and the molten erbium liquid drops into a water-cooled copper crucible. The erbium liquid drops into the crucible to slowly spiral down the bottom pad to draw a φ30 mm erbium ingot. After the melting is completed, the erbium ingot is surface turned to remove the surface inclusions. After one more electron beam melting and turning process, a high-purity erbium ingot is obtained.

[0046] A layer of high-temperature resistant and oxidation resistant silicone lubricating paint is coated on the surface of the erbium ingot to avoid oxidation and air absorption when the erbium ingot is heated, the drying temperature is 200°C, and the holding time is 18h to ensure that the paint effectively covers the surface of the erbium ingot. Then, the erbium ingot is subjected to homogenization annealing treatment, the heating temperature is 800°C, and the holding time is 2h. The erbium ingot is forged by a 500kg air hammer, the initial forging temperature is 800°C, and the final forging temperature is 450°C, and the erbium ingot is processed into an erbium metal rod with a diameter of φ13mm. After the air hammer forging is completed, the erbium rod is subjected to hot rotary forging by a six-pinch die rotary forging machine, the deformation processing rate is 7%, the heating temperature is 800°C, and the heating time is 15min. After rotary forging, an erbium metal thin rod with a diameter of φ4mm is obtained. The erbium thin rod is subjected to low-temperature oxidation surface pretreatment, the heating temperature is 320°C, and the treatment time is 30min. After the treatment is completed, the erbium wire is subjected to cold drawing, the drawing pass deformation is 7%, the lubricant is chlorinated paraffin, the drawing die is a diamond drawing die, and when the cumulative deformation reaches 70%, the erbium wire is subjected to intermediate annealing treatment, the annealing temperature is 750°C, the holding time is 30min, the vacuum degree is 2.4×10 -3 Pa, the surface of the erbium wire is pickled before annealing to remove the chlorinated paraffin attached to the surface of the erbium wire, and the final drawing diameter of the erbium wire is 0.50±0.005mm. The wire is cleaned by continuous electrolytic polishing, the electrolytic current is 4A, the alkali solution concentration is 5%wt NaOH solution, and the wire collection speed is 5m / min. After cleaning, the erbium wire is subjected to vacuum annealing, the vacuum degree is 2.2×10 -3 Pa, the annealing temperature is 550°C, the holding time is 30min, and the furnace cooling is performed.

[0047] The erbium wire prepared by the method of the embodiment is detected by inductively coupled plasma mass spectrometer, ICP-AES emission spectrometer and oxygen, nitrogen and hydrogen analyzer, the purity of the erbium wire is 99.96%, the content of B, Cd, Si, Cr, Cu and Co impurity elements is ≤30ppm, and the content of O, N and H is ≤100ppm, as shown in Table 1; the diameter of the erbium wire is 0.50mm, the wire diameter accuracy reaches ±0.005mm, the surface roughness Ra is 1.2μm, the tensile strength is 685MPa, the elongation is 8%, and the meter resistance uniformity is ±1.2%.

[0048] Table 1: Impurity element content of erbium wire

[0049]

[0050] Example 2

[0051] The erbium powder 3000g was weighed, and the erbium powder was added to a 7wt% solution prepared from hydrochloric acid and deionized water and stirred to a slurry, with the weight ratio of erbium powder to hydrochloric acid being 1:3. Then it was put into an ultrasonic cleaner for 20min, with the vibration frequency being 35KHz. After the cleaning treatment, deionized water was added and repeatedly stirred for rinsing, and the addition of deionized water was stopped when the PH test paper was tested to be neutral. After completion, it was put into a vacuum drying oven for drying, with the temperature being controlled at 60℃, the drying time being 24h, and the vacuum degree being 1.2×10 -2 Pa, until the erbium powder was completely dried. The erbium powder was loaded into a 304 stainless steel hole net fixed rubber mold sleeve in the shape of a round rod, sealed well and put into a cold isostatic pressing machine, with the pressing pressure being 180MPa and the pressure holding time being 90s. After cold isostatic pressing, the rubber mold sleeve was taken out, and the formed erbium rod had a diameter of φ20mm. The pressed and formed erbium rod was put into a microwave vacuum sintering furnace for sintering, with the vacuum degree being 1.1×10 -2 Pa, and a two-step gradient heat preservation sintering method was adopted, with the temperature being 350℃ for 90min and 850℃ for 90min, and the furnace was cooled down. A 250KW electron beam melting furnace was used, the erbium rod after microwave sintering was clamped in the furnace through the inlet valve, vacuum was extracted to 1.2×10 -4 Pa, the electron gun was moved to the place near the bottom of the erbium rod to start melting, the emission current was gradually increased to 350mA, the erbium rod was melted in the electron beam bombardment area, and after melting, the erbium liquid droplets fell into the water-cooled copper crucible. The erbium liquid droplets fell into the crucible, slowly pulled the bottom pad into a φ35mm erbium ingot, and after the melting was completed, the erbium ingot was surface turned, and the surface inclusions were removed. After one more time of the above electron beam melting and turning process, a high-purity erbium ingot was obtained.

[0052] A layer of high-temperature resistant and oxidation resistant silicone lubricating paint was coated on the surface of the erbium ingot to avoid oxidation and air absorption when the erbium ingot was heated, the drying temperature was 200℃, the holding time was 24h, and the paint was ensured to effectively cover the surface of the erbium ingot. Then the erbium ingot was subjected to homogenization annealing treatment, with the heating temperature being 800℃ and the holding time being 2h. The erbium ingot was forged by a 500kg air hammer, with the initial forging temperature being 800℃ and the final forging temperature being 500℃, and the erbium ingot was processed into an erbium metal rod with a diameter of φ15mm. After the air hammer forging was completed, the erbium rod was subjected to hot rotary forging by a six-pinch rotary forging machine, with the heating temperature being 800℃, the heating time being 20min, and the rotary forging obtained an erbium metal thin rod with a diameter of φ5mm. The erbium thin rod was subjected to low-temperature oxidation surface pretreatment, with the heating temperature being 320℃ and the treatment time being 30min, and after the treatment was completed, the erbium wire was cold drawn, with the drawing pass deformation being 8%, the lubricant being chlorinated paraffin, the drawing die being a diamond drawing die, and when the cumulative deformation reached 75%, the erbium wire was subjected to intermediate annealing treatment, with the annealing temperature being 700℃, the holding time being 30min, and the vacuum degree being 2.2×10 -3Pa, the annealing temperature is 600 ℃, the holding time is 30 min, and the furnace cooling is performed. The annealing temperature is 600 ℃, the holding time is 30 min, and the furnace cooling is performed. -3 Pa, the annealing temperature is 600 ℃, the holding time is 30 min, and the furnace cooling is performed. The annealing temperature is 600 ℃, the holding time is 30 min, and the furnace cooling is performed.

[0053] The purity of the erbium wire prepared by the method of the embodiment is 99.98%, the content of impurity elements B, Cd, Si, Cr, Cu and Co is ≤30 ppm, and the content of O, N and H is ≤100 ppm, as shown in Table 2; the wire diameter of the erbium wire is 0.80 mm, the wire diameter accuracy reaches ±0.005 mm, the surface roughness Ra is 1.0 μm, the tensile strength is 710 MPa, the elongation is 10.2%, and the uniformity of the meter resistance is ±1.2%,

[0054] Table 2: Impurity element content of erbium wire

[0055]

[0056] Example 3

[0057] 4000 g of erbium powder is weighed, and the erbium powder is added into a solution with a concentration of 8 wt% prepared by hydrochloric acid and deionized water and stirred into a slurry, and the weight ratio of the erbium powder to the hydrochloric acid is 1:3. Then, the solution is placed into an ultrasonic cleaning machine for cleaning for 30 min, and the vibration frequency is 40 KHz. After the cleaning treatment, deionized water is added and repeatedly stirred and rinsed, and the addition of the deionized water is stopped when the pH test paper is tested to be neutral. After completion, the solution is placed into a vacuum drying box for drying, the temperature is controlled at 60 ℃, the drying time is 36 h, and the vacuum degree is 1.1×10 -2 Pa until the erbium powder is completely dried. The erbium powder is loaded into a rubber mold sleeve in the shape of a round bar fixed by a 304 stainless steel mesh, sealed, and placed into a cold isostatic pressing machine, the pressing pressure is 200 MPa, the pressure holding time is 60 s, the rubber mold sleeve is taken out after the cold isostatic pressing, and the diameter of the formed erbium rod is φ25 mm. The pressed and formed erbium rod is placed into a microwave vacuum sintering furnace for sintering, the vacuum degree is 1.4×10 -2 Pa, a two-step gradient holding sintering method is adopted, the holding temperature is 350 ℃ for 90 min, and the holding temperature is 900 ℃ for 90 min, and the furnace cooling is performed. A 250 KW electron beam melting furnace is used, the erbium rod after microwave sintering is clamped in the furnace through an inlet valve, the vacuum is extracted to 1.6×10 -4Pa, move the electron gun to the vicinity of the lower end of the rod, gradually increase the emission current to 400 mA, and melt the rod in the electron beam bombardment zone. After melting, the liquid metal droplets fall into the water-cooled copper crucible. The liquid droplets fall into the crucible and slowly spiral down the bottom pad to draw the ingot to φ40mm. After the melting is completed, the erbium ingot is surface turned to remove the surface inclusions. After the above electron beam melting and turning process, a high purity erbium ingot is obtained.

[0058] A layer of high-temperature resistant and oxidation resistant silicone lubricating paint is coated on the surface of the erbium ingot to avoid oxidation and air absorption when the erbium ingot is heated. The drying temperature is 200℃ and the holding time is 24h to ensure that the paint effectively covers the surface of the ingot. Then the erbium ingot is subjected to homogenization annealing treatment at a heating temperature of 800℃ and a holding time of 2h. The erbium ingot is forged by a 500kg air hammer, the initial forging temperature is 800℃ and the final forging temperature is 450℃, and the erbium ingot is processed into an erbium metal rod with a diameter of φ15mm. After air hammer forging, the erbium rod is hot rotary forged by a six-pinch die rotary forging machine, the deformation rate of each pass is 10%, the heating temperature is 800℃ and the heating time is 20min. After rotary forging, a φ6mm erbium metal rod is obtained. The erbium rod is subjected to low-temperature oxidation surface pretreatment at a heating temperature of 350℃ for 30min, and then cold drawing is performed on the wire. The lubricant is chlorinated paraffin, the drawing die is a diamond drawing die, and when the cumulative deformation reaches 80%, the erbium wire is subjected to intermediate annealing treatment at an annealing temperature of 750℃ for 30min, a vacuum degree of 1.8×10 -3 Pa, the surface of the erbium wire is pickled before annealing to remove the chlorinated paraffin attached to the surface of the erbium wire. The final drawing diameter of the erbium wire is 1.00±0.005mm. The wire is cleaned by continuous electrolytic polishing, the electrolytic current is 6A, the alkali solution concentration is 7%wt NaOH solution, and the wire collection speed is 3m / min. After cleaning, the erbium wire is vacuum annealed at a vacuum degree of 2.5×10 -3 Pa, the annealing temperature is 650℃ and the holding time is 30min, and the furnace is cooled.

[0059] The erbium wire prepared by the method of the embodiment is tested by inductively coupled plasma mass spectrometer, ICP-AES emission spectrometer and oxygen, nitrogen and hydrogen analyzer, the purity of the erbium wire is 99.95%, the content of B, Cd, Si, Cr, Cu and Co impurity elements is ≤30ppm, and the content of O, N and H is ≤100ppm, as shown in Table 3; the diameter of the erbium wire is 1.00mm, the diameter accuracy reaches ±0.005mm, the surface roughness Ra is 1.0μm, the tensile strength is 750MPa, the elongation is 12.6%, and the meter resistance uniformity is ±1.3%.

[0060] Table 3 Impurity element content of erbium wire

[0061]

[0062] The erbium wire prepared by the method has a smooth surface, reduces surface burrs, and reduces surface roughness, and the surface quality of the erbium wire is greatly improved, see Figure 1 .

Claims

1. A method for preparing an erbium filament for a fast-response sensitive element, characterized in that, The steps are as follows: 1) Erbium powder pretreatment Erbium powder was added to hydrochloric acid solution and stirred until it became a slurry. It was then ultrasonically cleaned for 15–30 minutes. After that, deionized water was added and the mixture was repeatedly stirred and rinsed until neutral. The mixture was then dried under vacuum to obtain pretreated erbium powder. The ultrasonic vibration frequency of the ultrasonic cleaning is 30-50KHz. 2) Cold isostatic pressing The pretreated erbium powder was cold isostatically pressed into erbium rods; 3) Microwave vacuum sintering The erbium rod was sintered in a microwave vacuum heating furnace with a vacuum degree ≥10. -2 Pa was sintered using a two-step gradient holding method and cooled in the furnace to obtain sintered erbium rods; The two-step gradient heat preservation method is as follows: heat preservation at 300-350℃ for 60-90 minutes; heat preservation at 800-1000℃ for 60-90 minutes. 4) Vacuum electron beam melting Electron beam melting: The sintered erbium rod is melted under vacuum conditions. The sintered erbium rod is melted in the electron beam bombardment zone. After melting, the molten erbium metal is pulled down by a spiral to form an erbium ingot, and the melting is completed. The surface of the erbium ingot is turned. Electron beam melting and turning are repeated once more to obtain a high-purity erbium ingot. 5) Hot forging A high-temperature resistant and oxidation-resistant silicone lubricating coating is applied to the surface of the erbium ingot, dried, and then the erbium ingot is subjected to homogenization annealing treatment and forged into erbium metal rods; the erbium rods are hot-forged using a six-die rotary forging machine to obtain erbium metal fine rods; 6) Pulling Erbium metal rods were subjected to low-temperature oxidation surface pretreatment at a temperature of 280–350℃ for 20–30 min, and then drawn into erbium wires. The deformation amount per drawing pass was ≤8%. When the cumulative deformation amount reached 70–80%, the erbium wires were subjected to intermediate annealing to obtain erbium wires with a diameter of 0.4950–1.005 mm. 7) Surface post-treatment Erbium wire is continuously electrolytically polished and cleaned with an electrolytic current of 3–6 A, an alkaline solution of 5–15% wt NaOH, and a winding speed of 3–5 m / min. After cleaning, the erbium wire is vacuum annealed.

2. The method according to claim 1, characterized in that: Step 1) The erbium powder has an Er ≥ 99.95%, a Fisher particle size of 5-45 μm, and a normal particle size distribution. The weight ratio of erbium powder to hydrochloric acid is 1:

3.

3. The method according to claim 1, characterized in that: Step 1) The vacuum drying temperature is 40℃~60℃, the drying time is 24~36h, and the vacuum degree is ≥10. -2 Pa.

4. The method according to claim 1, characterized in that: Step 2) The pressing pressure of the cold isostatic pressing is 160MPa to 200MPa, and the holding time is 60s to 150s.

5. The method according to claim 1, characterized in that: Step 4) The vacuum is ≥1.0×10 -4 Pa, emission current 300-400mA.

6. The method according to claim 1, characterized in that: Step 5) The drying temperature is 160℃~200℃, and the holding time is 18~24h; The heating temperature for the homogenization annealing treatment is 700–800℃, and the holding time is 1.5–2 hours.

7. The method according to claim 1, characterized in that: Step 5) The initial forging temperature is 700-800℃, and the final forging temperature is 400-500℃; Step 5) The hot rotary forging has a pass deformation rate of 7-10%, a heating temperature of 700-800℃, and a heating time of 10-20 min; The erbium metal rod has a diameter of φ4mm to φ6mm and an average grain size of 5 to 10μm.

8. The method according to claim 1, characterized in that: Step 6) The intermediate annealing process is carried out under vacuum at a temperature of 520–820°C for 30–40 minutes, with a vacuum degree ≥10. -3 Pa.

9. The method according to claim 1, characterized in that: Step 7) The vacuum annealing is performed at a temperature of 520–720°C for 30–40 minutes, with a vacuum degree ≥10. -3 Pa, cooled with the furnace.

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