CN112958772A - Method for repairing waste WRe/TZM composite rotary anode target disc - Google Patents

Method for repairing waste WRe/TZM composite rotary anode target disc Download PDF

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Publication number
CN112958772A
CN112958772A CN202110140690.0A CN202110140690A CN112958772A CN 112958772 A CN112958772 A CN 112958772A CN 202110140690 A CN202110140690 A CN 202110140690A CN 112958772 A CN112958772 A CN 112958772A
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Prior art keywords
wre
waste
tzm
rotary anode
target disc
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CN202110140690.0A
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Inventor
张久兴
农滨荣
朱俊康
胡子
韩翠柳
潘亚飞
杨新宇
全昕龙
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Hefei Jingsili New Material Technology Co ltd
Hefei University of Technology
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Hefei Jingsili New Material Technology Co ltd
Hefei University of Technology
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Priority to CN202110140690.0A priority Critical patent/CN112958772A/en
Publication of CN112958772A publication Critical patent/CN112958772A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F7/00Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
    • B22F7/06Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite workpieces or articles from parts, e.g. to form tipped tools
    • B22F7/062Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite workpieces or articles from parts, e.g. to form tipped tools involving the connection or repairing of preformed parts
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/02Compacting only
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/12Both compacting and sintering
    • B22F3/14Both compacting and sintering simultaneously
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F7/00Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
    • B22F7/06Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite workpieces or articles from parts, e.g. to form tipped tools
    • B22F7/062Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite workpieces or articles from parts, e.g. to form tipped tools involving the connection or repairing of preformed parts
    • B22F2007/068Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite workpieces or articles from parts, e.g. to form tipped tools involving the connection or repairing of preformed parts repairing articles

Abstract

The invention provides a method for repairing a waste WRe/TZM composite rotary anode target disc, which comprises the following steps: s1) inspecting the surface defects of the waste WRe/TZM composite rotary anode target disc; s2) cutting the surface defects of the waste target disc; s3) processing the surface of the waste target disc, and calculating the mass of the needed WRe alloy powder; s4) placing the waste target disc with the surface treated into a graphite mold, wherein the target surface faces upwards, and adding WRe alloy powder; pre-pressing a graphite die filled with waste target discs and WRe alloy powder by adopting an SPS axial pressure device; s5) wrapping carbon felts with the same height as the graphite mold and the thickness of 4-6 mm on the periphery of the pre-pressed graphite mold, placing the carbon felts in an SPS furnace chamber, vacuumizing to below 5Pa, and carrying out spark plasma sintering connection. The obtained WRe/TZM composite rotary anode target disc has no defect on the surface, fine, uniform and relative tissuesThe density is high, the relative density of the repaired WRe alloy of the WRe/TZM composite rotary anode target disc is 97.0-98.0%, and the Vickers hardness is 430-455 HV0.5

Description

Method for repairing waste WRe/TZM composite rotary anode target disc
Technical Field
The invention relates to the field of rotary anode target materials, in particular to a method for repairing a waste WRe/TZM composite rotary anode target disc.
Background
The X-ray tube is widely applied to modern medical clinical diagnosis equipment, the WRe/TZM composite rotary anode target is one of core components of the X-ray tube, more than 50% of damage of the X-ray tube is caused by the failure of the rotary anode target, and the utilization rate of the rotary anode target product is generally about 70%. The working principle is that when the rotary anode target material runs, the rotary anode target material rotates at a high speed, and high-speed electrons emitted by a cathode bombard a target surface to generate X rays, so that the rotary anode target material is required to have high density, good mechanical property and the like. In the preparation and use processes of the rotary anode target, due to the production process problem, the user use parameter setting problem, the manual operation irregularity and the like, cracks and burn marks are generated on the surface of the target, or the use time is too long, the surface of the target has the defect of unevenness, the roughness of the target surface is increased, the performance of the rotary anode target and the service life of a product are influenced, and finally the target is failed.
Due to the fact that the melting point of WRe alloy is high, WRe/TZM composite rotary anode target materials on the market are generally prepared by a powder metallurgy method, after damage and discarding, serious refractory metal strategic resource waste is caused, and heavy metal pollution is easily caused. If the whole X-ray tube is scrapped, the target material is decomposed into raw materials after recovery, and the metal needs to be recovered through a complex metallurgical process, so that the serious problems of high cost, low production efficiency, low metal purity, environmental pollution and the like exist.
In the prior art, reports about repairing WRe/TZM composite rotary anode targets are not found. The difficulty in repairing the WRe/TZM composite rotary anode target is that high relative density and good processability are difficult to achieve. Because the rotary anode target disk rotates at a high speed when in operation, a repaired welding interface needs to have certain mechanical property to prevent the repairing layer from peeling off, and the WRe alloy has high melting point, so that the repairing layer and the original target surface are well combined, and the repair target material with high density and uniform tissue is difficult to obtain. At present, it is reported that the chemical vapor deposition method can be used for repairing the W-plated film on the surface of the target material, but the repairing temperature is too low, the interface bonding performance is not improved, and toxic gas is emitted. Therefore, the development of a new technology for repairing WRe/TZM composite rotary anode target is urgently needed.
Disclosure of Invention
Technical problem
Aiming at the defects in the prior art and realizing the recycling of the rotary anode target, the invention provides a method for repairing a waste WRe/TZM composite rotary anode target disc.
Technical scheme
According to one aspect of the invention, the method for repairing the waste WRe/TZM composite rotary anode target disc comprises the following steps:
s1: inspecting the surface defects of the waste WRe/TZM composite rotary anode target disc;
s2: cutting the surface defects of the waste target disc to remove the parts with the defects;
s3: performing surface treatment on the waste target disc, and calculating the mass of the needed WRe alloy powder;
s4: placing the waste target disc subjected to surface treatment into a graphite mold, enabling the target surface to face upwards, and adding WRe alloy powder; pre-pressing a graphite die filled with waste target discs and WRe alloy powder by using an SPS axial pressure device, wherein the pressure is 10-15 MPa;
s5: wrapping a carbon felt with the same height as the graphite mold and the thickness of 4-6 mm on the periphery of the pre-pressed graphite mold, placing the graphite mold in an SPS furnace chamber, vacuumizing to below 5Pa, and performing discharge plasma sintering connection on WRe alloy powder and the waste target disk to obtain the repaired WRe/TZM composite rotary anode target disk.
Preferably, the sintering process in step S5 is:
axial pressure: 10-30 MPa; the heating rate is as follows: 10-60 ℃/min; sintering temperature: 1450-1650 ℃; and (3) heat preservation time: 0-10 min; cooling: and (5) cooling along with the furnace.
Further, the diameter of the waste WRe/TZM composite rotary anode target disc is 50-110 mm, the length-diameter ratio is 0.05-1.0, and the rhenium content of the tungsten-rhenium alloy in the WRe/TZM composite rotary anode target disc is 5-15 wt%.
Further, the defect inspection described in step S1 includes a visual inspection for inspecting the target surface for visually observable cracks and burn marks and a non-destructive inspection for inspecting fine cracks.
Further, the surface defect cutting processing of step S2 is to remove the surface defect by machining, check the crack depth and burn degree of the target disc according to step S1, adjust the cutting depth to be greater than the crack depth, and obtain a smoother surface with a roughness Ra of less than 1.6. When the roughness is less than 1.6, good mechanical properties of the joint can be ensured.
Further, the surface treatment in step S3 includes removing an oxide layer by washing with an acid solution, rinsing with clear water, and dehydrating with absolute ethanol; and calculating the mass of the needed WRe alloy powder according to the cutting depth and the repair thickness, wherein the proportion of W to Re in the WRe alloy powder is consistent with the proportion of W to Re contained in the waste WRe/TZM composite rotary anode target disc.
Preferably, the acid solution is an aqueous solution of hydrochloric acid, and more preferably an aqueous solution of hydrochloric acid with a volume fraction of 5%.
Further, the temperature rise rate is 30-60 ℃/min between room temperature and 1300 ℃, and the temperature rise rate is 10-30 ℃/min between 1300 ℃ and the highest sintering temperature; the axial pressure adopts a gradient pressurization mode: when the temperature is lower than 1400 ℃, the axial pressure is 10 MPa; when the temperature is more than or equal to 1400 ℃, the axial pressure is 30 MPa.
The repaired WRe/TZM composite rotary anode target disc obtained by the method has the WRe alloy relative density of 97.0-98.0% and the Vickers hardness of 430-455 HV0.5
Advantageous effects
The method adopts the SPS technology, can completely repair the defects on the surface of the waste WRe/TZM composite rotary anode target disc by selecting proper sintering connection parameters, has fine and uniform tissues after repair, high relative density and equivalent density with a new target material, effectively solves the problem that the existing WRe/TZM composite rotary anode target disc cannot be repaired and reused after the defects are generated on the surface, has simple process, short period and high production efficiency, and can greatly reduce the use cost of the WRe/TZM composite rotary anode target material.
Detailed Description
The present invention will be described in detail with reference to the following examples, which are carried out on the premise of the technical solution of the present invention, and give detailed embodiments and specific procedures, but the scope of the present invention is not limited to the following examples.
The following examples used a discharge plasma sintering furnace of LABOX-6020 series discharge plasma sintering system manufactured by Sinter Land of Japan, whose current type was DC pulse current and whose pulse sequence was 40: 7.
The test method comprises the following steps:
1. relative density: archimedes drainage method
2. Vickers hardness: DHV-1000Z Vickers hardness tester
Example 1
In this embodiment, the waste W5Re/TZM composite rotary anode target disk with a diameter of 100.0mm × 11.5mm is repaired, which includes the following steps:
step 1, performing defect detection on a waste W5Re/TZM composite rotary anode target disc, mainly performing visual inspection and nondestructive inspection, manually inspecting visible cracks and burn groove marks on a target surface by using a high power magnifier, and performing nondestructive inspection for detecting fine cracks to determine that the processing depth is 0.5 mm;
2, selecting a lathe to cut the target surface, wherein the machining depth is 0.5 mm;
step 3, washing by using a hydrochloric acid aqueous solution with the volume fraction of 5% to remove an oxide layer, washing by using clear water, dehydrating by using absolute ethyl alcohol, and carrying out surface treatment; calculating the mass of the required W5Re alloy powder according to the cutting depth and the repair thickness;
weighing W5Re alloy powder with corresponding mass for later use;
step 4, placing the waste target disc subjected to surface treatment into a graphite mold, enabling the target surface to face upwards, adding W5Re powder, and placing a pressure head; pre-pressing a graphite die filled with waste target discs and W5Re alloy powder by using an SPS axial pressure device, wherein the pressure is 10 MPa;
and 5, wrapping a carbon felt with the same height as the graphite mold and the thickness of 4-6 mm on the periphery of the pre-pressed graphite mold, placing the carbon felt in an SPS furnace chamber, vacuumizing to below 5Pa, and performing discharge plasma sintering connection on the W5Re alloy powder and the waste W5Re/TZM composite rotary anode waste target disc. The sintering process comprises the following steps:
axial pressure: adopting a gradient pressurization mode (room temperature to 1400 ℃, 10MPa of pressure, 1400 to 1500 ℃, 30MPa of pressure);
the heating rate is as follows: the temperature is between room temperature and 1300 ℃, the heating rate is 50 ℃/min, the heating rate is between 1300 and 1500 ℃, and the heating rate is 30 ℃/min;
sintering temperature: 1500 ℃;
and (3) heat preservation time: 10 min;
after furnace cooling, rough machining removes carbon paper on the surface of the sample, namely the repair of the waste W5Re/TZM composite rotary anode target disc is completed, the repaired rotary anode target disc with high density of phi 100mm multiplied by 11.5mm is obtained, the relative density of the repaired W5Re alloy is 97.52 percent, and the Vickers hardness is 456.19HV0.5. Whereas the W5Re alloy relative density and hardness of the anode target disk prior to repair were 94.30% and 305HV0.5
Example 2
In this embodiment, the waste W5Re/TZM composite rotary anode target disk with a diameter of 100.0mm × 11.5mm is repaired, which includes the following steps:
step 1, performing defect detection on a waste W5Re/TZM composite rotary anode target disc, mainly performing visual inspection and nondestructive inspection, manually inspecting visible cracks and burn cracks on a target surface by using a high power magnifier, and performing nondestructive inspection for detecting fine cracks to determine the processing depth of 0.6 mm;
2, selecting a lathe to cut the target surface, wherein the machining depth is 0.6 mm; (ii) a
Step 3, washing by using a hydrochloric acid aqueous solution with the volume fraction of 5% to remove an oxide layer, washing by using clear water, dehydrating by using absolute ethyl alcohol, and performing surface treatment on the surface of the target disc to be repaired; calculating the mass of the required W5Re alloy powder according to the cutting depth and the repair thickness;
weighing W5Re alloy powder with corresponding mass for later use;
step 4, placing the waste target disc subjected to surface treatment into a graphite mold, enabling the target surface to face upwards, adding W5Re powder, and placing a pressure head; pre-pressing a graphite die filled with waste target discs and W5Re alloy powder by using an SPS axial pressure device, wherein the pressure is 10 MPa;
and 5, wrapping a carbon felt with the same height as the graphite mold and the thickness of 4-6 mm on the periphery of the pre-pressed graphite mold, placing the carbon felt in an SPS furnace chamber, vacuumizing to below 5Pa, and performing discharge plasma sintering connection on the W5Re powder and the waste W5Re/TZM composite rotary anode target disk. The sintering process comprises the following steps:
axial pressure: adopting a gradient pressurization mode (room temperature to 1400 ℃, 10MPa pressure, 1400 to 1600 ℃, 30MPa pressure);
the heating rate is as follows: the temperature is between room temperature and 1300 ℃, the heating rate is 50 ℃/min, the heating rate is between 1300 and 1600 ℃, and the heating rate is 30 ℃/min;
sintering temperature: 1600 ℃;
and (3) heat preservation time: 10 min;
after furnace cooling, rough machining removes carbon paper on the surface of the sample, namely the repair of the waste W5Re/TZM composite rotary anode target disc is completed, the repaired rotary anode target disc with high density of phi 100mm multiplied by 11.5mm is obtained, the relative density of the repaired W5Re alloy is 98.38 percent, and the Vickers hardness is 445.31HV0.5. Whereas the relative density and hardness of the anode target disk W5Re alloy prior to repair was 94.65% and309HV0.5
example 3
In this embodiment, the waste W5Re/TZM composite rotary anode target disk with a diameter of 90.0mm × 10.5mm is repaired, which includes the following steps:
step 1, performing defect detection on a waste W5Re/TZM composite rotary anode target disc, mainly performing visual inspection and nondestructive inspection, manually inspecting visible cracks and burn groove marks on a target surface by using a high power magnifier, and performing nondestructive inspection for detecting fine cracks to determine that the processing depth is 0.5 mm;
2, selecting a lathe to cut the target surface, wherein the machining depth is 0.5 mm; (ii) a
Step 3, washing by using a hydrochloric acid aqueous solution with the volume fraction of 5% to remove an oxide layer, washing by using clear water, dehydrating by using absolute ethyl alcohol, and carrying out surface treatment; calculating the mass of the required W5Re alloy powder according to the cutting depth and the repair thickness;
weighing W5Re alloy powder with corresponding mass for later use;
step 4, placing the waste target disc subjected to surface treatment into a graphite mold, enabling the target surface to face upwards, adding W5Re powder, and placing a pressure head; pre-pressing a graphite die filled with waste target discs and W5Re alloy powder by using an SPS axial pressure device, wherein the pressure is 10 MPa;
and 5, wrapping a carbon felt with the same height as the graphite mold and the thickness of 4-6 mm on the periphery of the pre-pressed graphite mold, placing the carbon felt in an SPS furnace chamber, vacuumizing to below 5Pa, and performing discharge plasma sintering connection on the W5Re alloy powder and the waste W5Re/TZM composite rotary anode target disk. The sintering process comprises the following steps:
axial pressure: adopting a gradient pressurization mode (room temperature to 1400 ℃, 10MPa of pressure, 1400 to 1500 ℃, 30MPa of pressure);
the heating rate is as follows: the temperature is between room temperature and 1300 ℃, the heating rate is 50 ℃/min, the heating rate is between 1300 and 1500 ℃, and the heating rate is 30 ℃/min;
sintering temperature: 1500 ℃;
and (3) heat preservation time: 10 min;
after cooling along with the furnace, roughly processing and removing carbon paper on the surface of the sample to finish the waste W5Re/TZM compositeRepairing the rotary anode target disc to obtain the high-density repaired rotary anode target disc with phi 90.0mm multiplied by 10.5mm, wherein the relative density of the repaired W5Re alloy is 97.65 percent, and the Vickers hardness is 450.31HV0.5. While the W5Re alloy relative density and hardness of the anode target disk prior to repair were 93.82% and 298HV0.5

Claims (10)

1. A method for repairing a waste WRe/TZM composite rotary anode target disc comprises the following steps:
s1: inspecting the surface defects of the waste WRe/TZM composite rotary anode target disc;
s2: cutting the surface defects of the waste target disc to remove the parts with the defects;
s3: performing surface treatment on the waste target disc, and calculating the mass of the needed WRe alloy powder;
s4: placing the waste target disc subjected to surface treatment into a graphite mold, enabling the target surface to face upwards, and adding WRe alloy powder; pre-pressing a graphite die filled with waste target discs and WRe alloy powder by using an SPS axial pressure device, wherein the pressure is 10-15 MPa;
s5: wrapping a carbon felt with the same height as the graphite mold and the thickness of 4-6 mm on the periphery of the pre-pressed graphite mold, placing the graphite mold in an SPS furnace chamber, vacuumizing to below 5Pa, and performing discharge plasma sintering connection on WRe alloy powder and the waste target disk to obtain the repaired WRe/TZM composite rotary anode target disk.
2. The repair method according to claim 1,
the sintering process in step S5 is:
axial pressure: 10-30 MPa; the heating rate is as follows: 10-60 ℃/min; sintering temperature: 1450-1650 ℃; and (3) heat preservation time: 0-10 min; cooling: and (5) cooling along with the furnace.
3. The repair method according to claim 2,
in step S5, the temperature rise rate is 30-60 ℃/min between room temperature and 1300 ℃, and the temperature rise rate is 10-30 ℃/min between 1300 ℃ and the highest sintering temperature; the axial pressure adopts a gradient pressurization mode: when the temperature is lower than 1400 ℃, the axial pressure is 10 MPa; when the temperature is more than or equal to 1400 ℃, the axial pressure is 30 MPa.
4. The repair method according to any one of claims 1 to 3,
the diameter of the waste WRe/TZM composite rotary anode target disc is 50-110 mm, the length-diameter ratio is 0.05-1.0, and the rhenium content of the tungsten-rhenium alloy in the WRe/TZM composite rotary anode target disc is 5-15 wt%.
5. The repair method according to any one of claims 1 to 4,
the defect inspection described in step S1 includes visual inspection for inspecting the target surface for visually observable cracks and burn scars and non-destructive inspection for inspecting micro cracks.
6. The repair method according to any one of claims 1 to 5,
and the surface defect cutting processing of the step S2 is to remove the surface defects by adopting a mechanical processing method, inspect the crack depth and the burn degree of the target disc according to the step S1, adjust the cutting depth to be larger than the crack depth, obtain a smoother surface, and the roughness Ra is lower than 1.6.
7. The repair method according to any one of claims 1 to 6,
the surface treatment in the step S3 comprises washing with an acid solution, washing with clear water, and dehydrating with absolute ethyl alcohol; and calculating the mass of the required WRe alloy powder according to the cutting depth and the repair thickness, wherein the proportion of W to Re in the WRe alloy powder is consistent with the proportion of W to Re contained in the waste WRe/TZM composite rotary anode target disc.
8. The repair method according to claim 7,
the acid solution is an aqueous solution of hydrochloric acid.
9. The repair method according to claim 8,
the acid solution is a hydrochloric acid aqueous solution with the volume fraction of 5%.
10. The repair method according to any one of claims 1 to 9,
the repaired WRe/TZM composite rotary anode target disc has the WRe alloy relative density of 97.0-98.0% and the Vickers hardness of 430-455 HV0.5
CN202110140690.0A 2021-02-02 2021-02-02 Method for repairing waste WRe/TZM composite rotary anode target disc Pending CN112958772A (en)

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