CN110373642B - Heavy rare earth metal target material repairing method - Google Patents
Heavy rare earth metal target material repairing method Download PDFInfo
- Publication number
- CN110373642B CN110373642B CN201910706295.7A CN201910706295A CN110373642B CN 110373642 B CN110373642 B CN 110373642B CN 201910706295 A CN201910706295 A CN 201910706295A CN 110373642 B CN110373642 B CN 110373642B
- Authority
- CN
- China
- Prior art keywords
- target
- repaired
- repairing
- alloy powder
- rare earth
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/1003—Use of special medium during sintering, e.g. sintering aid
- B22F3/1007—Atmosphere
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C28/00—Alloys based on a metal not provided for in groups C22C5/00 - C22C27/00
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
- C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C24/00—Coating starting from inorganic powder
- C23C24/02—Coating starting from inorganic powder by application of pressure only
- C23C24/04—Impact or kinetic deposition of particles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Manufacturing & Machinery (AREA)
- Powder Metallurgy (AREA)
- Physical Vapour Deposition (AREA)
Abstract
The invention provides a heavy rare earth metal target repairing method, and belongs to the technical field of magnetron sputtering surface treatment. The invention provides a heavy rare earth metal target repairing method, which comprises the following steps: filling alloy powder into a loss area of the target to be repaired, and repairing by adopting a vacuum sintering method or a high-pressure cold spraying method; the alloy powder comprises dysprosium terbium alloy, or one or two of dysprosium terbium and one or two of amphoteric metals. The invention takes the alloy powder as the repairing material, and adopts the vacuum sintering method or the high-pressure cold spraying method for repairing, the alloy powder plays a role of brazing, the sintering temperature in the subsequent target repairing is reduced, the diffusion temperature after the magnetic sheet is coated is reduced, and the repairing difficulty and the repairing cost are reduced. The target tissue repaired by the method effectively solves the problem that the existing target surface cannot be reused after generating defects; and the method has the advantages of simple process, short period, use effect close to that of a new target material and good application value.
Description
Technical Field
The invention relates to the technical field of magnetron sputtering surface treatment, in particular to a heavy rare earth metal target repairing method.
Background
Magnetron sputtering has the characteristics of simple operation, easy and accurate control of process parameters, good film forming quality and the like, becomes one of the most important modern film coating methods, is applied to surface film coating of various materials such as metal, semiconductor, insulator and the like, and has the advantages of easy control of film forming thickness, large film coating area, strong adhesive force and the like. Magnetron sputtering introduces a magnetic field on the surface of a target cathode, improves plasma density by utilizing the confinement of the magnetic field to charged particles so as to increase sputtering rate, and is widely applied to a plurality of technical fields such as electronic information and information industries mainly comprising integrated circuits, information storage, liquid crystal displays, laser memories, electronic controllers and the like at present.
At present, the improvement of the coercive force of a magnet through the surface heavy rare earth metal coating and diffusion becomes the key research point of the industry in recent years. The sintered Nd-Fe-B permanent magnetic material is an advanced functional material, and the coercive force of the sintered Nd-Fe-B permanent magnetic material can be improved by plating a layer of heavy rare earth metal film on the surface of the sintered Nd-Fe-B permanent magnetic material by a magnetron sputtering method and diffusing the heavy rare earth metal film. However, in the magnetron sputtering process, under the influence of the magnetic field structure of the target, the plasma is confined in a local area of the target surface, so that the regional sputtering of the target is caused, and a runway-shaped area is formed after sputtering, so that the utilization rate of the target is low. And the heavy rare earth metal thin film plated on the neodymium iron boron permanent magnet material uses the heavy rare earth metal target material such as dysprosium, terbium and the like with very high price, the target material has high cost and low utilization rate, and the film plating cost is greatly improved.
Disclosure of Invention
The invention aims to provide a heavy rare earth metal target repairing method. The target repaired by the repair method provided by the invention effectively solves the problem that the existing target cannot be reused after the surface of the target has defects; the process is simple, the period is short, the sintered neodymium iron boron magnet is coated and diffused by using the repaired target material, compared with the original target material, the coercive force of the sintered neodymium iron boron magnet is improved by 95-98%, the using effect is close to that of a new target material, but the cost of the target material is only 30-40% of that of the new target material, the cost advantage is very obvious, and the application value is good.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a heavy rare earth metal target repairing method, which comprises the following steps: filling alloy powder into a loss area of the target to be repaired, and repairing by adopting a vacuum sintering method or a high-pressure cold spraying method; the alloy powder comprises dysprosium terbium alloy, or one or two of dysprosium terbium and one or two of amphoteric metals.
Preferably, the target material to be repaired is made of dysprosium terbium alloy and impurities; the total content of dysprosium and terbium in the target material to be repaired is more than or equal to 70 wt%.
Preferably, the content of the heavy rare earth metal in the alloy powder is more than or equal to 70 wt%.
Preferably, the granularity of the alloy powder is 0.1-5 mm.
Preferably, the preparation method of the alloy powder comprises the following steps: smelting and hydrogenating dysprosium terbium alloy or one or two of dysprosium terbium and one or two of amphoteric metals to prepare powder to obtain alloy powder; the temperature of the hydrogenated powder is 400-700 ℃.
Preferably, the method further comprises the step of preprocessing the target to be repaired before the alloy powder is filled in a loss area of the target to be repaired, wherein the preprocessing comprises alkali washing, water washing and ethanol washing which are sequentially carried out.
Preferably, the process parameters of the vacuum sintering method include: vacuum degree is more than or equal to 8 multiplied by 10-3Pa, the heating rate is 5-50 ℃/min, the sintering temperature is 1150-1300 ℃, and the heat preservation time is 60-300 min.
Preferably, before the vacuum sintering method is adopted for repairing, the method further comprises the step of performing pre-pressing treatment on the target to be repaired, wherein the loss area is filled with alloy powder; the pressure of the pre-pressing treatment is 300-500 MPa.
Preferably, the high-pressure cold spraying method is carried out in a protective atmosphere; the technological parameters of the high-pressure cold spraying method comprise: the pressure is 1.5 to 1.8MPa, and the particle impact velocity is 550 to 750 m/s.
Preferably, after the repair is completed, the method further comprises the step of machining the repaired part.
The invention provides a heavy rare earth metal target repairing method, which comprises the following steps: filling alloy powder into a loss area of the target to be repaired, and repairing by adopting a vacuum sintering method or a high-pressure cold spraying method; the alloy powder comprises dysprosium terbium alloy or one or two of dysprosium terbium and amphoteric metal. The alloy powder is used as a repairing material, the repairing material is repaired by a vacuum sintering method or a high-pressure cold spraying method, the repairing material is made of dysprosium terbium alloy or one of the dysprosium terbium alloy and the terbium alloy, and amphoteric metal is added into the repairing material. Meanwhile, the introduced amphoteric material is an indispensable component in the sintered neodymium iron boron component to be coated originally, and has no adverse effect on the magnetic performance. Meanwhile, the repair difficulty and cost are reduced, and the diffusion temperature of the coating film in the subsequent magnetron sputtering process by using the repaired heavy rare earth metal target is reduced. The embodiment result shows that the time for plating the film layer with the same thickness on the repaired target material is not greatly different from that of the new target material, the magnetic performance of the final magnet is almost improved in a similar range, but the cost of each set of target material is obviously reduced. The tensile property of the repaired heavy rare earth metal target material is consistent with that of a new heavy rare earth metal target material, the defects on the surface of the heavy rare earth metal target material are repaired completely, the repaired metal structure is fine, the density is high, and the problem that the existing target material cannot be repaired and reused after the defects are generated on the surface is effectively solved. The target material repaired by the method effectively solves the problem that the existing target material cannot be reused after the surface of the target material has defects; the heavy rare earth metal is hardly lost in the repairing process, the target can be repeatedly used, and the utilization rate of the target is greatly improved; and the process is simple, the period is short, the production efficiency is high, and the cost is low.
Drawings
FIG. 1 is a diagram of a "racetrack" type depletion region formed on the surface of a circular target;
FIG. 2 is a diagram of a "racetrack" type of consumed area formed on the surface of a rectangular target;
FIG. 3 is a diagram of the target before repair of the filler alloy powder;
fig. 4 is a view of the target after repair.
Detailed Description
The invention provides a heavy rare earth metal target repairing method, which comprises the following steps: filling alloy powder into a loss area of the target to be repaired, and repairing by adopting a vacuum sintering method or a high-pressure cold spraying method; the alloy powder includes a heavy rare earth metal and an amphoteric metal.
In the present invention, all the raw material components are commercially available products well known to those skilled in the art unless otherwise specified.
In the present invention, the target to be repaired is preferably any heavy rare earth target that needs to be repaired, and specifically, after the heavy rare earth target customized according to the target configuration requirements of the magnetron sputtering coating equipment is used for a certain period of time, a large "runway" -shaped consumed area (as shown in fig. 1 and fig. 2) is formed on the surface of the target, and the target cannot be reused, needs to be detached from the magnetron sputtering equipment, and is reused after being repaired.
In the invention, the material of the target material to be repaired is preferably dysprosium terbium alloy and impurities, and the total content of dysprosium and terbium in the target material to be repaired is preferably more than or equal to 70 wt%, and more preferably more than or equal to 80 wt%. In the invention, the mass ratio of dysprosium to terbium in the heavy metal target material to be repaired is preferably 1: 1.
In the invention, before the alloy powder is filled in a loss area of the target material to be repaired, the method preferably further comprises the step of pretreating the target material to be repaired, wherein the pretreatment comprises alkali washing, water washing and ethanol washing which are sequentially carried out. In the invention, the alkali liquor used for alkali washing is preferably an inorganic alkali solution, and more preferably a sodium hydroxide solution or a potassium hydroxide solution; the concentration of the sodium hydroxide solution and the concentration of the potassium hydroxide solution are independent, preferably 4-10 wt%, and more preferably 4 wt%. In the invention, the concentration of the inorganic alkali solution is too high, the strong corrosivity of the solution can cause potential safety hazards, and the oil stain cannot be removed completely due to too low concentration. The water used for washing is not particularly limited, and water well known in the art can be used, such as distilled water, deionized water or ultrapure water; the washing frequency is not specially limited, and the alkali can be completely removed. In the invention, the purpose of the ethanol washing is to remove water vapor adsorbed on the surface of the target to be repaired; the ethanol is preferably anhydrous ethanol. In the invention, impurities on the surface of the target to be repaired can be removed through pretreatment, thereby being beneficial to subsequent repair.
In the present invention, the alloy powder preferably includes dysprosium terbium alloy, or one or two kinds of dysprosium terbium and one or two kinds of amphoteric metals. In the invention, the alloy powder is dysprosium terbium binary alloy, or dysprosium gallium binary alloy, or dysprosium aluminum binary alloy, or terbium gallium binary alloy, or terbium aluminum binary alloy, or dysprosium, gallium and aluminum ternary alloy, or terbium, gallium and aluminum ternary alloy, or dysprosium, terbium and gallium ternary alloy, or dysprosium, terbium, gallium and aluminum quaternary alloy, more preferably dysprosium: terbium: aluminum: gallium is formed into a quaternary alloy according to the mass ratio of 4:4:1: 1. In the invention, the content of heavy rare earth metal in the alloy powder is preferably not less than 50 wt%, and more preferably 85-95 wt%. In the invention, the granularity of the alloy powder is preferably 0.1-5 mm. In the invention, the excessive granularity of the alloy powder can cause the specific surface area of the powder to be too small, the activity of the powder particles is poor and the powder particles are difficult to combine with a substrate, the excessive granularity can cause the activity of the powder particles to be too high and easy to oxidize, and the granularity of the alloy powder is controlled within the range, so that the alloy powder can be well combined with the repaired target substrate on the premise of ensuring that the powder particles are not oxidized.
In the invention, the alloy powder is preferably obtained by smelting and hydrogenating dysprosium terbium alloy or one or two kinds of dysprosium terbium and one or two kinds of amphoteric metal to prepare powder. In the invention, the smelting is preferably carried out in a medium-frequency induction smelting furnace to obtain an alloy ingot. The working parameters of the medium-frequency induction smelting furnace are not particularly limited, and the medium-frequency induction smelting furnace known in the field is adopted for smelting. In the present invention, the hydrogenated powder production is preferably carried out in a hydrogen pulverizer. The hydrogen crushing furnace of the present invention is not particularly limited, and a hydrogen crushing furnace known in the art may be used. In the invention, the temperature of the hydrogenated powder is preferably 400-700 ℃, more preferably 450-650 ℃, and most preferably 500-600 ℃. The amphoteric metal in the alloy powder provided by the invention plays roles of fluxing, diffusion and brazing in the repair process, the repair effect is effectively improved, the sintering temperature in the subsequent target repair is reduced, and the repair difficulty and cost are reduced.
According to the invention, the target material to be repaired is preferably placed in a rubber mold, and then the target material is repaired by adopting a vacuum sintering method. The rubber mold of the present invention is not particularly limited, and a rubber mold known in the art may be used. The size of the rubber mold is not particularly required, and the size of the rubber mold is larger than that of the target to be repaired, specifically, the size of the target to be repaired is 350 × 125 × 10mm, and the size of the rubber mold is 352 × 127 × 11 mm. Compared with the graphite mold, the rubber mold adopted by the invention has the advantages of low cost, easy processing and capability of preventing the increase of the carbon content.
In the invention, the process parameters of the vacuum sintering method comprise: the vacuum degree is preferably more than or equal to 8X 10-3Pa, the heating rate is preferably 5-50 ℃/min, more preferably 10-30 ℃/min, and most preferably 17 ℃/min; the sintering temperature is preferably 1150-1300 ℃, more preferably 1200-1300 ℃, and most preferably 1250 ℃; the heat preservation time is preferably 60-300 min, more preferably 90-240 min, and most preferably 120 min. According to the invention, by controlling the technological parameters of pressure, vacuum degree, heating rate, sintering temperature and heat preservation time of the vacuum sintering method, the defects on the surface of the target material to be repaired can be completely repaired, and the repaired metal tissue is fine, high in density and consistent in tensile property with the original target material, so that the problem that the existing target material cannot be repaired and reused after the defects are generated on the surface is effectively solved, the filled heavy rare earth metal powder is dissolved in the region of the target material to be repaired in a solid manner, and the repair of the rare earth metal target material is completed; the method has the advantages of simple process, short period and high production efficiency, and can greatly reduce the use cost of the dysprosium, terbium and other heavy rare earth targets.
In the invention, before the vacuum sintering method is adopted for repairing, the method preferably further comprises the step of performing pre-pressing treatment on the target to be repaired, wherein the loss area is filled with alloy powder; the pressure of the pre-pressing treatment is preferably 300 to 500MPa, more preferably 350 to 450MPa, and most preferably 400 MPa.
In the present invention, the high pressure cold spray method preferably includes the steps of: under the condition of protective atmosphere, high-pressure cold spraying is used for locally melting and stacking alloy powder and the heavy rare earth metal target material, so that the loss area is stacked; specifically, the method comprises the following steps: and (3) performing inert gas protection on the heavy rare earth target by using an upper protective cover positioned above the heavy rare earth target and a bottom protective cover positioned at the bottom of the heavy rare earth target, melting alloy powder and the heavy rare earth target locally by using high-pressure cold spraying, accumulating in a loss area, repeatedly accumulating, gradually flattening the loss area, and finally forming an accumulation state. The protective atmosphere in the present invention is not particularly limited, and a protective atmosphere known in the art may be used, specifically, argon or nitrogen. In the invention, the technological parameters of the high-pressure cold spraying comprise: the pressure is preferably 1.5-1.8 MPa, and more preferably 1.6-1.7 MPa; the particle impact velocity is preferably 550 to 750m/s, more preferably 600 to 700 m/s. The method adopts a high-pressure cold spraying method for repairing, is easy to operate, simple in process, free of pollution and low in cost; in the repairing process, the heavy rare earth materials in the target material and the repairing material are hardly lost, so that the target material can be repeatedly used, and the utilization rate of the target material is greatly improved; and the repaired target material has no cracks and no pores, and the interface of the filled heavy rare earth material and the original sputtering target is in metallurgical bonding in a welding state, so that the phenomena of delamination and the like can not occur.
In the present invention, after the repair is completed, it is preferable to further perform a machining process on the repaired portion. In the present invention, the machining treatment is preferably a polishing and grinding treatment. The polishing treatment of the present invention is not particularly limited, and a polishing treatment known in the art may be used.
In the invention, after the repair of the heavy rare earth metal target is completed, the repaired target is preferably loaded into the target base and can be reused.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
1) Pretreating the target material to be repaired: sequentially adopting 4 wt% sodium hydroxide solution to remove oil, washing with deionized water and dehydrating with absolute ethyl alcohol;
wherein the target to be repaired is a dysprosium terbium alloy target (the mass ratio of dysprosium to terbium is 1:1, and the sum of the contents of dysprosium and terbium is more than 99 wt%); the surface of the target to be repaired is provided with a runway-shaped loss area; the size of the target to be repaired is 350 x 125 x 10 mm;
2) dysprosium, terbium, aluminum and gallium in a mass ratio of 4:4:1:1 are smelted into alloy ingots in a medium-frequency induction smelting furnace, and the alloy ingots are placed in a hydrogen crushing furnace to be hydrogenated and pulverized at the temperature of 650 ℃ to obtain alloy powder;
3) placing the pretreated target material to be repaired into a rubber mold with the size of 352X 127X 11mm, adding alloy powder to make the alloy powder fully distributed on the surface to be repaired of the heavy rare earth metal target material, and repairing by adopting a vacuum sintering method, wherein the technological parameters of the vacuum sintering method are as follows: prepressing by adopting an isostatic pressing process, wherein the pressure is 400 MPa; sintering in a vacuum sintering furnace with vacuum degree higher than 8 × 10-3Pa; the heating rate is 17 ℃/min; the sintering temperature is 1000 ℃; the heat preservation time is 120min, namely the repair of the heavy rare earth metal target material is completed;
4) after the surface of the target material is properly polished and polished, the repaired heavy rare earth metal target material is loaded into a target material base and can be reused.
Fig. 3 is a target material diagram before repair of the filler alloy powder, and fig. 4 is a target material diagram after repair in example 1. As can be seen from fig. 4, the repaired rare earth metal target has complete surface defect repair, fine metal structure and high density, so that the problem that the existing target cannot be repaired and reused after the surface has defects can be effectively solved.
Example 2
1) Pretreating the target material to be repaired: sequentially adopting 4 wt% sodium hydroxide solution to remove oil, washing with deionized water and dehydrating with absolute ethyl alcohol;
wherein the target to be repaired is a dysprosium terbium alloy target (the mass ratio of dysprosium to terbium is 1:1, and the sum of the contents of dysprosium and terbium is more than 99 wt%); the surface of the target to be repaired is provided with a runway-shaped loss area; the specification of the target to be repaired is 350 × 125 × 10 mm;
2) dysprosium, terbium, aluminum and gallium in a mass ratio of 4:4:1:1 are smelted into alloy ingots in a medium-frequency induction smelting furnace, and the alloy ingots are placed in a hydrogen crushing furnace to be hydrogenated and pulverized at the temperature of 650 ℃ to obtain alloy powder;
3) performing inert gas protection on the heavy rare earth metal target by using an upper protective cover positioned on the heavy rare earth metal target and a bottom protective cover positioned at the bottom of the heavy rare earth metal target for the pretreated target to be repaired, melting alloy powder and the heavy rare earth metal target locally by using high-pressure cold spraying, accumulating the alloy powder and the heavy rare earth metal target in a loss area, repeatedly accumulating the alloy powder and the heavy rare earth metal target, gradually leveling the loss area, and finally forming an accumulation state, wherein the technological parameters of the high-pressure cold spraying are as follows: the pressure is 1.6MPa, and the impact velocity of the particles is 680 m/s;
4) after the surface of the target material is properly polished and polished, the repaired heavy rare earth metal target material is loaded into a target material base and can be reused.
The target material diagram before the filling alloy powder is repaired is basically the same as that in the embodiment 1, and the target material diagram after the repair is basically the same as that in the embodiment. The defects on the surface of the repaired rare earth metal target are repaired completely, and the repaired metal has fine structure and high density, so that the problem that the surface of the existing target cannot be repaired and reused after the defects are generated can be effectively solved.
Test example
The comparative use of the target material repaired in examples 1 and 2 with a new target material (i.e., the original target material) is shown in table 1:
TABLE 1 repaired target and New target usage
| Contrast item | Raw target material | Example 1 | Practice ofExample 2 |
| Density (g/cm)3) | 8.5 | 8.2 | 8.3 |
| Utilization (%) | 65 | >90 | >90 |
| Integrated cost (Wan/set) | 4.5 | 1.7 | 1.7 |
| Time (min) for plating a film of 4 μm thickness | 65 | 72 | 73 |
| Coercive force Hcj (KA/m) of coated magnet under the same condition | 638 | 620 | 625 |
As can be seen from Table 1, the time for plating the film layer with the same thickness on the repaired target material is not greatly different from that of the new target material, and finally the magnetic performance of the magnet is improved almost nearly, but the cost of each set of target material is obviously reduced. The tensile property of the repaired heavy rare earth metal target material is consistent with that of a new heavy rare earth metal target material, the defects on the surface of the heavy rare earth metal target material are repaired completely, the repaired metal structure is fine, the density is high, and the problem that the existing target material cannot be repaired and reused after the defects are generated on the surface is effectively solved.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (8)
1. The heavy rare earth metal target repairing method is characterized by comprising the following steps: filling alloy powder into a loss area of the target to be repaired, and repairing by adopting a vacuum sintering method or a high-pressure cold spraying method;
the target to be repaired is made of dysprosium terbium alloy, or one or two of dysprosium terbium and one or two of amphoteric metal;
the alloy powder comprises dysprosium terbium alloy, or one or two of dysprosium terbium and one or two of amphoteric metals;
the sintering temperature of the vacuum sintering method is 900-1100 ℃, the heat preservation time is 60-300 min, and the vacuum degree of the vacuum sintering method is more than or equal to 8 multiplied by 10-3Pa, the heating rate is 5-50 ℃/min;
the high-pressure cold spraying method is carried out in a protective atmosphere; the technological parameters of the high-pressure cold spraying method comprise: the pressure is 1.5 to 1.8MPa, and the particle impact velocity is 550 to 750 m/s.
2. The repairing method according to claim 1, wherein the total content of dysprosium and terbium in the target material to be repaired is not less than 70 wt%.
3. The repair method according to claim 2, wherein the content of the heavy rare earth metal in the alloy powder is not less than 70 wt%.
4. The repair method according to claim 1 or 3, wherein the grain size of the alloy powder is 0.1 to 5 mm.
5. The repair method according to claim 1, wherein the preparation method of the alloy powder comprises: smelting and hydrogenating dysprosium terbium alloy or one or two of dysprosium terbium and one or two of amphoteric metals to prepare powder to obtain alloy powder;
the temperature of the hydrogenated powder is 400-700 ℃.
6. The repair method according to claim 1, wherein before filling the alloy powder into the worn-out area of the target material to be repaired, the method further comprises pretreating the target material to be repaired, wherein the pretreatment comprises alkali washing, water washing and ethanol washing which are sequentially performed.
7. The repair method according to claim 1, further comprising, before the repair by the vacuum sintering method, pre-pressing the target to be repaired, in which the alloy powder is filled in the loss region; the pressure of the pre-pressing treatment is 300-500 MPa.
8. The method of repairing according to claim 1, further comprising machining the repaired site after the repairing is completed.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910706295.7A CN110373642B (en) | 2019-08-01 | 2019-08-01 | Heavy rare earth metal target material repairing method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910706295.7A CN110373642B (en) | 2019-08-01 | 2019-08-01 | Heavy rare earth metal target material repairing method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN110373642A CN110373642A (en) | 2019-10-25 |
| CN110373642B true CN110373642B (en) | 2021-08-10 |
Family
ID=68257546
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910706295.7A Active CN110373642B (en) | 2019-08-01 | 2019-08-01 | Heavy rare earth metal target material repairing method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110373642B (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110983277A (en) * | 2019-12-30 | 2020-04-10 | 广州市尤特新材料有限公司 | Rotary rare earth target material for neodymium iron boron permanent magnet material, and preparation method and repair method thereof |
| CN111362294B (en) * | 2020-04-14 | 2022-06-14 | 开化祥盛磁业有限公司 | Method for treating terbium target material waste, terbium oxide and preparation method thereof |
| CN112725675B (en) * | 2020-12-23 | 2021-11-09 | 苏州希镝瑞新材料科技有限公司 | Method for manufacturing dysprosium/terbium target |
| CN112958772A (en) * | 2021-02-02 | 2021-06-15 | 合肥工业大学 | Method for repairing waste WRe/TZM composite rotary anode target disc |
| CN113174487A (en) * | 2021-04-13 | 2021-07-27 | 新疆众和股份有限公司 | Recovery method of aluminum residual target for liquid crystal panel |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104124052A (en) * | 2014-07-25 | 2014-10-29 | 安徽大地熊新材料股份有限公司 | Preparation method for high-performance rare earth-iron-boron sintered permanent magnet |
| US20150107991A1 (en) * | 2012-10-25 | 2015-04-23 | Jx Nippon Mining & Metals Corporation | Fe-Pt-Based Sputtering Target Having Nonmagnetic Substance Dispersed Therein |
| CN206153033U (en) * | 2016-11-07 | 2017-05-10 | 厦门佰事兴新材料科技有限公司 | Target cold spouts that work piece makes up tool for restoration |
| CN108274009A (en) * | 2018-02-08 | 2018-07-13 | 合肥工业大学 | A kind of restorative procedure of Cr targets |
| CN108389711A (en) * | 2018-01-05 | 2018-08-10 | 宁波招宝磁业有限公司 | A kind of preparation method of the Sintered NdFeB magnet with high-coercive force |
-
2019
- 2019-08-01 CN CN201910706295.7A patent/CN110373642B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20150107991A1 (en) * | 2012-10-25 | 2015-04-23 | Jx Nippon Mining & Metals Corporation | Fe-Pt-Based Sputtering Target Having Nonmagnetic Substance Dispersed Therein |
| CN104124052A (en) * | 2014-07-25 | 2014-10-29 | 安徽大地熊新材料股份有限公司 | Preparation method for high-performance rare earth-iron-boron sintered permanent magnet |
| CN206153033U (en) * | 2016-11-07 | 2017-05-10 | 厦门佰事兴新材料科技有限公司 | Target cold spouts that work piece makes up tool for restoration |
| CN108389711A (en) * | 2018-01-05 | 2018-08-10 | 宁波招宝磁业有限公司 | A kind of preparation method of the Sintered NdFeB magnet with high-coercive force |
| CN108274009A (en) * | 2018-02-08 | 2018-07-13 | 合肥工业大学 | A kind of restorative procedure of Cr targets |
Also Published As
| Publication number | Publication date |
|---|---|
| CN110373642A (en) | 2019-10-25 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110373642B (en) | Heavy rare earth metal target material repairing method | |
| US10526715B2 (en) | Preparation of rare earth permanent magnet | |
| US10179955B2 (en) | Production method for rare earth permanent magnet | |
| US10181377B2 (en) | Production method for rare earth permanent magnet | |
| CN102280240B (en) | Method for preparing sintered NdFeB with low dysprosium content and high performance | |
| US10138564B2 (en) | Production method for rare earth permanent magnet | |
| KR20090074767A (en) | Process for producing sintered NdFeB MAGNET | |
| EP2919241B1 (en) | Electrodepositing apparatus and preparation of rare earth permanent magnet | |
| CN111341512B (en) | High-cost performance rare earth permanent magnet and preparation method thereof | |
| CN106920669B (en) | Preparation method of R-Fe-B sintered magnet | |
| CN111554502A (en) | Method for preparing high-coercivity sintered neodymium-iron-boron through pressurization diffusion heat treatment | |
| CN104575901A (en) | Neodymium iron boron magnet added with terbium powder and preparation method thereof | |
| JP2006228937A (en) | Manufacturing method of rare earth sintered magnet and device for molding in magnetic field | |
| CN108274009B (en) | Cr target material repairing method | |
| WO2023001189A1 (en) | High-performance sintered neodymium-iron-boron magnet and preparation method therefor | |
| CN108817405B (en) | W target repairing method | |
| CN105513733A (en) | Method for preparing sintered rare earth permanent magnetic material | |
| EP3291263B1 (en) | Method for producing rare-earth magnet | |
| CN110400669A (en) | A kind of high performance neodymium iron boron of low heavy rare earth and preparation method thereof | |
| CN113380528B (en) | Method for remolding sintered neodymium iron boron grain boundary | |
| CN109898051A (en) | A kind of wear-resistant corrosion resistant DLC/SiNxLaminated film and preparation method thereof | |
| CN108565088A (en) | A kind of band coating sintered NdFeB magnet and preparation method thereof | |
| CN118156015A (en) | Technology for regenerating neodymium-iron-boron permanent magnet material from neodymium-iron-boron waste |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |